Production of Acetaldehyde From Acetic Acid

Department of Chemical & Biomolecular Engineering

Senior Design Reports (CBE) University of Pennsylvania

Year 2002

Production of Acetaldehyde from Acetic Acid Calvin daRosa

Aurindam Ghatak

University of Pennsylvania


Claire Pinto University of Pennsylvania

This paper is posted at ScholarlyCommons. http://repository.upenn.edu/cbe sdr/45

PRODUCTION OF ACETALDEHYDE FROM ACETIC ACID

Authors:

Calvin daRosa

Aurindam Ghatak

Claire Pinto

Faculty Advisor

Dr. John V ohs

April 9, 2002

Department of Chemical Engineering


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09 April 2002 Dr. John Vohs Prof. Leonard Fabiano Department of Chemical Engineering University of Pennsylvania Philadelphia, P A 19104

Dear Dr. Vohs and Prof. Fabiano:

Enclosed in this report is the completed economic analysis of our proposed process. The process is designed to produce and recover acetaldehyde at high purity from acetic acid. This process design recovers 12,818 lblhr of acetaldehyde by extractive distillation at 99.6 % weight purity. A second commodity chemical, ethyl acetate, is produced as a byproduct in this process and is purified by a series of distillation columns. Ethyl acetate is produced at a rate of 1,139 lblhr and purity of 99.6 weight percent.

Capital cost estimations and profitability analysis have been completed for our process. Financial modeling of our process assuming the price of acetic acid to be 0.16/lb yielded an Investors Rate of Return (IRR) of 11.4 % and a Total Capital Investment (TCI) of $47,242,990. This scenario is not economically feasible. However, when the price of acetic acid is taken to be $0.12/lb, the IRR and TCI are 18.5 % and $47,224,990 respectively. In the light of that fact that the possible legislation ofMTBE out of gasoline might make this process more economically attractive, the group recommends further research into the feasibility of such a plant and the possible future construction of the facility given the realization of the second scenario.

Sincerely,

~0?d4--Calvin P. daRosa

~

Aurindam K. Ghatak

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Claire L. Pinto

TABLE OF CONTENTS

Abstract. ................... .......... . .................................. .. ........ ..... 5

Introduction.... . , .... . .................. .. ................................... , ........ 7

Process Flowsheet. .................. . ................................................ 13

Material Balance ...... ................... . ................................... . ....... 16

Process Description ................... . ......................................... . .... 23

Energy Balance and Utility Requirements ..... ............................ . ...... 35

Unit Descriptions ............ ..... . .................. . ................................ 39

Absorber . . .................... . .... ........ ................ 39

Compressor. .. . .............................. . ... .. . ....... 40

Condensers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

Decanter... . ... . .. ...... . ........ . ......................... . 44

Distillation Columns ..... . ......... ...................... 44

Fired Heater. ...... . ................. . .............. . .. . ... 49

Flash VesseL ......... . .................................... 50

Heat Exchangers ......... . ........... . .................... 50

Mixers ....... ............................................... 53

Pumps .. .. . ..... . .......................................... . 54

Reactor. ...... .. ............... ... .... . .. .. ............. . ... 59

Reboilers .. ....... . .................. . .... . .... .. ....... ... . 61

Reflux Accumulators ........... .. ......... . .............. 63

Refrigeration System .. . ..... .................. ...... .. ... 65

Splitters . . .. .... .. ..... .. ... ....... ........ .. ......... . ...... 65

Stripper ............ .. .... .. ... ............ " . ... .. .. .... . .. 66

Tanks . . .. . .................................................. 67

Valve ................. ...... ........... ... . ....... .......... .. 70

Unit Specification Sheets .................. ...... . ...... . ........... . ..... . .......... 71

Equipment Cost Summary......... . ..... . ..... ...... . .. . .. . ...... . .... . ... . ........ 135

Fixed-Capital Investment Summary.................... ...... . ..... ... ... .... . .... 137

Important Considerations ...... , .... . ... . .. . .... .. ... '" .... .. ..... . ..... . .. ........ .141

Operating Cost and Economic Analysis ................. ...... . ..... .......... .. . 145

Conclusions and Recommendations ........... . .......... . ....... .. ........... . ... 159

Acknowledgements ........... ...... ................... . ..... . ... . .. ................. 161

Bibliography.... ........ , .. .. ..... . ....... . .......... . , ...... . .... .. ... ....... . ....... 162

Appendix A: Unit Cost Calculations . . ........ ... ..... .. .... . ..... . ..... ...... . .. .163

Appendix B: Utility Cost Calculations ... .. .................... . ... .... .......... .201

Appendix C: Aspen Plus Results ... . ... . .... . . .. ........ .. ... . ... . ........ . ..... ...207

Appendix D: Problem Statement. ... . .......... . ........... .. ........... ....... .... 269

Appendix E: Patent. .... . ....................... .. ... . ..... . , ..... ............. , ..... .273

Abstract Our group has designed a process to manufacture 101,520,000 lb/yr of acetaldehyde by hydrogenation ofacetic acid over a 20% wt. palladium on iron oxide catalyst. The reaction conditions used are the optimum according to a patent filed by Eastman Chemical (Tustin, et.al., U.S . Patent No. 6,121,498): temperature is range is from 557-599 of at a pressure of254 psi. The conversion of acetic acid in the reactor is 46 %, with selectivity of 86% to acetaldehyde. Major by-products are ethanol, acetone, carbon dioxide, and the light hydrocarbons methane, ethane, and ethylene. Acetaldehyde is purified in a series of steps: it is first absorbed with an acetic-acid rich solvent, then distilled to separate acetaldehyde from heavier components. A refrigerated condenser is then used to recover additional acetaldehyde from the vapor distillate of the main separation. Acetic acid is purified and recycled to the reactor to limit the amount of feedstock required. Ethyl acetate is produced as a by-product in the acetaldehyde distillation column and is purified and sold. The economics of the process is strongly dependent on the price of acetic acid, and we examined scenarios under which acetic acid was available at either $0.16/Ib or $0.12/Ib. The total capital investment in either situation is approximately $47,000,000. If acetic acid is available at $0. 16/1b, we estimate an IRR of 11.3 %, but if acetic acid can be purchased for $0.12/Ib the IRR is 18.5% after 20 years. It is our recommendation to pursue more research into projecting both the cost of acetic acid and the market for acetaldehyde. If acetic acid will be available at the lower price, the company should pursue production of acetaldehyde.

5

6

Introduction The main product manufactured in this process is acetaldehyde. Acetaldehyde was chosen as the primary product because of its wide use in industry and the profitability of its sale as a chemical of given purity. In addition to acetaldehyde, ethyl acetate is produced as a side product. Table 1 below shows basic chemical information concerning the products.

Table 1: P

Synonym Molecular Formula Molecular Weight CAS No. Melting point Boiling point Density

f f duct Acetaldehyde (grimary product) Ethanal C 2H 4O 44.05 75-07-0 -190.3 OF 69.6 OF 0.6149 g/cm J -

Ethyl Acetate {side product) Acetic acid ethyl ester CH 3COOC 2H s 88.0 141-78-6 -117 OF 171°F 1.108 g/cm J

I. Uses Acetaldehyde is primarily used in industry as a chemical intermediate, principally for the production of pyridine and pyridine bases, peracetic acid, pentaerithritol, butylene glycol and chloral. It is used in the production of esters, particularly ethyl acetate and isobutyl acetate (lARC V.36 1985; Chern. Prod. Synopsis, 1985). It is also used in the synthesis of crotonaldehyde as well as flavor and fragrance acetals, acetaldehyde 1,1 dimethylhydrazone, acetaldehyde cyanohydrin, acetaldehyde oxime and various acetic esters, paraldehyde halogenated derivatives (lARC V.36, 1985). Acetaldehyde has been used in the manufacture of aniline dyes and synthetic rubber, to silver mirrors and to harden gelatin fibers (Merck, 1989). It has been used in the production of polyvinyl acetal

7

L

resins, in fuel compositions and to inhibit mold growth on leather (lARC V.36, 1985). Acetaldehyde is also used in the manufacture of disinfectants, drugs, perfumes, explosives, lacquers and varnishes, photographic chemicals, phenolic and urea resins, rubber accelerators and antioxidants, and room air deodorizers; acetaldehyde is a pesticide intermediate (Sittig, 1985; Gosselin, 1984). Acetaldehyde, an alcohol denaturant, is a GRAS (generally recognized as safe) compound for the intended use as a flavoring agent (Furia and Bellanca, 1975; HSDB, 1997). It is an important component of food flavorings added to milk products, baked goods, fruit juices, candy, desserts, and soft drinks. In 1976, approximately 19,000 Ib of acetaldehyde were used as food additives, primarily as fruit and fish preservatives and as a synthetic flavoring agent to impart orange, apple and butter flavors. Ethyl acetate, the side product of this process, is widely used in printing inks, paints and coatings, pesticides, pharmaceuticals, laminations and flexible packaging.

II. Production i.

Reasons for entering the market

Acetaldehyde was first produced commercially in the United States in 1916. U.S. Production of acetaldehyde reached its peak in 1969 at approximately 1.65 billion lb (lARC V.36, 1985). There has been an overall decline in the demand for acetaldehyde due to the use of more economical starting materials for principal derivatives and a lower demand for some acetal derivatives (Chern. Prod., 1985). However, in recent times due to a decline in the number of suppliers and an increase in potential U.S. acetaldehyde exports, there is a vast potential for profitability in manufacturing acetaldehyde. In 1985,

8

estimated U.S. exports of acetaldehyde were 1.2 billion lb (Chemical Products Synopsis, 1985).

ii.

Alternative processes and their disadvantages

Acetaldehyde can be made commercially via the Wacker process, the partial oxidation of ethylene. The major disadvantage of that process is that it is very corrosive requiring very expensive materials of construction. Another major disadvantage is that the reaction is prone to over-oxidation of the ingredient, the products of which are thermodynamically more stable than acetaldehyde which is the partial oxidation product. This over oxidation of the ingredient reduces the yield of acetaldehyde produced and converts expensive ethylene into carbon oxides (Tustin, et al.). Acetaldehyde is also manufactured by oxidizing ethanol using air. A mixture of air and ethanol vapor is fed into a multi-tubular reactor. Temperature is maintained between 750-932 of (400-500 °C), and the pressure at 29.4 psi. The catalyst used is chromium activated copper. Vapor coming out of the reactor is passed through a scrubber and unreacted ethanol is separated and recycled. However, this process gives a relatively poor yield of acetaldehyde The process investigated in this report converts acetic acid into acetaldehyde. Acetic acid is relatively inexpensive and is available at $0.12-$0.16/lb. It can be generated from inexpensive methanol. Due to the possible legislation ofMTBE out of gasoline, there may be a worldwide glut of methanol, so any chemicals that use methanol may become much more economically attractive. That is why acetic acid is our starting material of choice.

9

The catalyst used in this process is 20% palladium on an iron oxide support. This catalyst gives a selectivity of 86% to the desired reaction at 46% acetic acid conversion. Though this process can also be effectively catalyzed by mercury compounds, the toxic nature of mercury makes it unfeasible.

iii.

Discussion of Production Method

The reaction is carried out in a packed bed reactor at a temperature range between 557 and 599 of. The following reactions occur in the reactor: CH)COOH + H2 -> CH)CHO + H 20 (main reaction)

(1)

CH)COOH + 2H2 -> CH)CH 20H + H 20

(2)

2CH)COOH -> CH)COCH) + CO2 + H 20

(3)

3CH)COOH + 9H 2 -> 2CH4 + C 2H 6 + C2~ + 6H20

(4)

Under reaction conditions, the selectivity to reaction (1) is 86%. This facilitates a good yield of acetaldehyde and further justifies the cost of the reactor conditions. The product is then passed through an absorber and then separated as the distillate using a fractional distillation column. The following reaction occurs in the distillation column to produce ethyl acetate: CH)COOH + CH 3CH20H -> CH3COOCH2CH3 + H 20

(5)

This generation of ethyl acetate in situ is beneficial as it facilitates an ethyl acetate-water azeotrope in the acetic acid separation column, which makes it easier to separate the acetic acid. This acetic acid is then recycled back to the reactor. After being separated from the water, first in a decanter and then by distillation, the ethyl acetate is purified to 99.6 % wt, and can be sold.

10

The Gulf Coast is the location of choice for this plant. This is primarily due the region being an industrial belt. As a consequence, storage facilities as well as raw materials are readily available and cheap. As mentioned in the problem statement, due to this choice of location, it is assumed that hydrogen can be purchased over the plant fence for $0.50Ilb at 200 psig. Additionally, the prices of utilities are relatively inexpensive. Natural gas is available at $2.30IMMBTU, cooling water is purchased at $0.33IMGal and steam at 35 psi at $2.46IMLbs.

III. Environmental issues and potential safety problems EP A regulates acetaldehyde under several Acts such as the Clean Air Act (CAA) and the Clean Water Act (CWA). EPA has established water quality criteria, effluent guidelines, rules for regulating hazardous spills, general threshold amounts and requirements for the handling and disposal of acetaldehyde wastes. Process enclosures, local exhaust ventilation and other engineering controls must be used to maintain airborne levels below maximum exposure limits. Acetaldehyde is an extremely flammable liquid and vapor. Its vapor may cause flash fires. It forms explosive peroxides and polymerizes, resulting in hazardous conditions. Acetaldehyde is therefore sold in stainless steel tanks with a refrigerating system to ensure that the temperature of the product does not rise above 15°C. Acetaldehyde is also a potential cancer hazard. High vapor concentration may cause drowsiness or irritation of the eye and respiratory tract. For eye protection, safety glasses with side shields and a face shield need to be worn by people with risk of exposure. Additionally, chemical resistant gloves, boots and protective clothing appropriate for the

11

risk of exposure need to be worn. Decontamination facilities such as eye bath, washing facilities and safety shower must be provided. Ethyl acetate, on the other hand, is not subject to EPA emergency planning requirements under the Superfund Amendments and Reauthorization Act (SARA) (Title III) in 42 USC 11022. However, ethyl acetate is an irritant of the eyes and upper respiratory tract at concentrations above 400 ppm [NLM 1992]. Ethyl acetate occasionally causes sensitization, with inflammation of the mucous membranes and eczema of the skin [Hathaway et al. 1991]. As a consequence, ethyl acetate is stored in a cool, dry, well-ventilated area in tightly sealed containers. Splash-proof chemical safety goggles or face shields and coveralls should be worn during any operation involving potential exposure to ethyl acetate.

12

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MATERIAL BALANCE

Item Number:

S-101

Temperature (oF) Pressure (psia) Total Mass Flow (Ib/hr) Components (Ib/hr): HYDROGEN CO2 METHANE ETHYLENE ETHANE ACETALD ACETONE ETHYLACE ETHANOL WATER HOAC

77 14.7 21,447.80

S-102 263.2 20.1 438.03

S-103 369.9 98 .6 20,743.76 trace trace

21,447.80

trace trace 1.47 < 0.001 0.001 436.55

trace 0.006 0.016 < 0.001 366.13 20,377 .61

S-103b

S-104

369.9 238 98 .6 14.7 20,686 .08 42,571.91 trace trace

trace trace

trace trace 0.006 0.006 0.016 1.49 < 0.001 0.001 365.11 365.11 20,320.95 42,205.31

S-201 241 .9 263 .0 42,571 .91 trace trace

trace 0.006 1.49 0.001 365.11 42,205.31

*** VAPOR PHASE *** Density kg/cum Viscosity cP *** LIQUID PHASE *** Density kg/cum Viscosity cP Surface Ten dyne/cm

S-202

930.46 0.36 16.94

835.12 0.23 14.09

835 .12 0.23 14.09

947.66 0.40 19.33

960 .79 0.43 20.47

S-204

S-205

280.10 464.7 477.6 599 245 .9 255.0 254.8 252.0 20,783.29 42,571.91 20,402.42 62,974.33 2,339 .05 trace 1,790.54 trace 516.52 302.49 303 .96 4,445.69 trace 219.70 0.006 299.41 1.49 254 .71 0.001 2,376.36 365 .11 7,934.87 42,205 .31

6.35 0.02

1,073.48 1.12 27 .04

S-203

28.80 0.016

7,781.47 7,781.47 5,137.53 5,137 .53 1,495.12 1,495.12 855.34 855.34 855.42 855.42 621.46 621.46 285.40 285.40 906.51 908 .00 17.25 17.25 933.97 1,299.08 1,512.96 43,718 .26

2.10 0.015

726.98 0.17 6.81 -

Item Number:

..J

Temperature (oF) Pressure (psia) Total Mass Flow (Ib/hr) Components (Ib/hr): HYDROGEN CO2 METHANE ETHYLENE ETHANE ACETALD ACETONE ETHYLACE ETHANOL WATER HOAC *** VAPOR PHA5E *** Density kg/cum Viscosity cP *** LIQUID PHA5E *** Density kg/cum Viscosity cP 5urface Ten dyne/cm

5·206

5·206a

5·206b

5·207

5·208

5·301

5·302

5·303

5·304

5·305

556.8 556.8 250.9 250.9 62,977.88 42,195.18

556.8 250 .9 20,782 .70

202.6 268 262 .8 245.92 20,402.42 42,195.18

280.1 245.7 62,979.67

113 113 159.2 126.4 244.7 244.7 235.0 234 .9 62,979 .67 23,469.70 62,277.91 65,870.50

7,088 .04 4,748.99 5,425.89 3,635.35 1,565.20 1,048.68 916.61 614.13 921.10 617.13 13,468.60 9,023.96 665.97 446.20 908.03 608.38 771 .86 517 .15 7,201.54 4,825.03 24,045.05 16,110.18

2,339.05 1,790.54 516.52 302.48 303 .96 4,444.64 219.77 299.65 254.71 2,376.51 7,934 .86

7,781.47 4,748.99 5,137.53 3,635.35 1,495.12 1,048.68 855 .34 614.13 855.42 617.13 621.46 9,023.96 285.40 446 .20 906.51 608 .38 17.25 517.15 933.97 4,825.03 1,512.96 16,110.18

7,088.04 5,425.88 1,565.20 916.63 921.10 13,471 .78 665.76 907.31 771 .84 7,201 .08 24,045.05

7,088.04 5,425.88 1,565.20 916.63 921.10 13,471.78 665.76 907.31 771.84 7,201.08 24,045.05

6.34 0.015

6.34 0.015

4.69 0.02

4,685.00 0.02

4.69 0.02

2.83 0.012

5.90 0.015

869.51 0.28 26 .59

7,088.02 trace 0.02 5,328.15 trace 122.96 1,543.27 trace 28.45 893.76 trace 27.13 898.61 trace 31 .92 6,792.88 6.47 6,167.54 119.04 785.89 615.79 126.56 2,775.68 1,983.88 33.52 110.70 126.75 266.36 13,552.93 12,873.06 379.53 45,046.25 43,892.99

3.74 0.012

944.18 941.97 0.49 0.55 42.46 L...... 42.39

Item Number:

.g


5-306

5-401

159.4 113 244 .7 233.5 39,509.77 19,877.11 0.02 97.73 21.93 22.87 22.49 6,677.43 546.90 781 .38 738.33 6,935.17 23,665.52

*** VAPOR PHASE *** Density kg/cum Viscosity cP

7,088.00 5,205.19 1,514.82 866 .63 866.69 631.81 . 289.14 918 .35 17.47 946.23 1,532.78

2.85 0.012

5-401a

5-402

5-501

5-501 a

5-502

5-503

5-504

121 .8 101.8 77 152.3 120.9 214.7 43 .5 212.7 229.9 32.0 785.61 20,404.31 105,380.47 105,379.58 10,354.66

98.3 30.1 2,463.56

101.81 32 .0, 2,885.40

6,995.85 5,137 .53 1,495.13 855 .36 855.42 623.59 285.38 906.41 17.24 933 .93 1,512 .85

785.61

trace 1.30 0.54 1.88 1.09 2,455.29 trace

0.04 215.16 47 .99 41 .93 49 .63 2,527.19 trace trace trace 3.46 trace

2.85 0.012

1.19 0.009

159.4 233.0 19,618.71

5-403

7,781.46 5,137.53 1,495.13 855.36 855.42 623 .59 285.38 906.41 17.24 933.93 1,512.85

0.04 220.69 50.38 50 .01 54.41 12,846.44 1,162.51 2,764.63 865.07 19,807.78 67,558 .51

0.04 trace 220.69 5.53 50.38 2.39 50.00 8.07 54.41 4.78 12,843.29 10,306.52 1,162.71 trace 2,765.36 trace 865.08 trace 19,808.00 27.372 67,559.63 trace

2.48 0.012

3.48 0.012

2.48 0.013

936.37 0.56 41 .92

935.77 0.55 41.85

3.456

3.71 0.0098

**- LIQUID PHASE --

Density kg/cum Viscosity cP Surface Ten dyne/cm

926.34 0.56 41 .01

747.63 0.19 18.96

750.34 0.19 19.10

Item Number:

::0

Temperature (oF) Pressure (psia) Total Mass Flow (Ib/hr) Components (Ib/hr): HYDROGEN CO2 METHANE ETHYLENE ETHANE ACETALD ACETONE ETHYLACE ETHANOL WATER HOAC *** VAPOR PHASE *** Density kg/cum Viscosity cP *** LIQUID PHASE *** Density kg/cum Viscosity cP Surface Ten dyne/cm

5-505

5-506

10 262 .7 28.0 37.8 421 .84 92,139.53 0.041 213.86 47.45 40.05 48.54 71.90 trace

< 0.001

5 -506a

5 -507

5-601

5-602

5-603

5 -604

5 -701

5-702

262 .6 37 .8 62,277 .57

158 262 .7 31.8 37 .8 62,277 .91 29,861 .62

263.2 100.0 29,861.62

117.5 118.1 275.2 35.0 98 .0 95.0 22,326 .31 22,326.31 31,444 .17

182.5 40 .0 5,111 .13

trace trace trace trace trace 9.57 1,162.71 4,106.58 163.78 20,051.42 66,645.46

trace trace trace trace trace 4.87 785.95 2,775.97 110.71 13,553.36 45,046.71

trace trace trace trace trace trace trace trace trace trace 6.47 3.10 785.89 376.83 2,775.68 1,330.91 110.70 53 .08 13,552 .93 6,498.49 45,046.25 21,599 .21


< 0.001 trace

< 0.001 trace

868.23 0.27 34.14

868 .12 0 .27 34 .23

< 0.001 . trace

< 0.001 trace

17.83 17.83 20.93 1,598.79 1,598.79 1,975.61 17,200.99 17,200.99 18,531 .88 110.58 110.58 163.66 1,746.22 1,746.22 7,878.58 1,651.91 1,651.91 2,873 .51

4.82 487.45 4,044 .88 31.88 540 .20 1.90

3.05 0.011

945 .04 0.49 42 .56

868.23 0.27 34.14

867.80 0.27 34 .10

895.15 0.41 34 .16

894.70 0.41 34 .11

784 .92

834 .37 0.27 32.29

Item Number:

~


5-703

5-704

214 .1 113 36 .0 39 .0 36,555.16 36,555.16 < 0.001 trace

< 0.001 trace

5-705

5-706

182.3 24 .7 5,111.13

181.9 25.0 4,356.10

< 0.001 trace

< 0.001 trace

5-707

184.3 24 .9 755 .20 trace

5-801

5-802

5-803

5-804

117.5 35.5 8,295.16

259.4 35 .0 2,161 .83

234.1 27.4 9,262 .68

182.1 25.0 1,194.31

trace

trace

5-805

167.6 22 .0 439 .28 trace I

I

25.83 25.83 2,463 .10 2,463.10 22,576.48 22,576.48 195.55 195.55 8,418 .79 8,418.79 2,875.41 2,875.41

*** VAPOR PHASE *** Density kg/cum Viscosity cP

5.02 0.011

*** LIQUID PHASE *** Density kg/cum Viscosity cP Surface Tenjyne/cm_

834 .76 0.25 40.45

4.82 487.45 4,044.88 31.88 540.20 1.90

4.66 424 .01 3,434.98 29 .15 462.28 1.02

0.17 63 .50 610 .00 2.74 77.92 0.88

3.63 439 .38 803 .75 55 .58 6,208 .52 784 .29

2,161.83

0.32 145.94 19.51 50.45 8,263 .04 783.42

1.33 0.014

910 .22 0.50 48.51

834 .57 0.27 32 .31

834.49 0.27 32 .37

835.00 0.26 31 .98

943 .08 0.57 64 .57

891 .97 0.25 54.45

3.31 293.44 784 .24 5.13 107.31 0.88

3.16 229 .99 174.35 2.39 29.39 trace

3.56 0.01

3.08 0.0096

Item Number:

t:

Temperature (oF) Pressure (psia) Total Mass Flow (Ib/hr) Components (Ib/hr) : HYDROGEN CO2 METHANE ETHYLENE ETHANE ACETALD ACETONE ETHYLACE ETHANOL WATER HOAC *** VAPOR PHASE *** Density kg/cum Viscosity cP *** LIQUID PHASE *** Density kg/cum Viscosity cP Surface Ten dyne/cm

5-901

5-901a

5-902

117.5 35.0 5,933.43

221 28 .0 1,577.33

trace

< 0.001 trace

trace trace

3.16 229.99 174.35 2.39 29.39 trace

4.66 424.90 4,571.37 29.39 464.07 439.05

< 0.001 0.89 1,136.39 0.24 1.79 438.03

< 0.001 0 .89 1,134.92 0.24 1.79 1.48

895.16 0.41 34.16

853.48 0.26 16.21

838.96 0 .25 17.39

167.6 22 .0 439.28

5-903 175 16.0 1,139.31

3.08 0.0096

22

Process Description 1. Reaction Section

The feedstocks for the reaction of interest are acetic acid and hydrogen. Hydrogen gas is available at 200 psig, and the acetic is available as a liquid. We assumed both starting materials to be at 77 OF. These starting materials are each mixed with recycle streams composed primarily of the respective reactant before proceeding to the reactor. The pure acetic acid feed stream S-101 is combined with recycle streams S-102 and S-1 03, which originated at the ethyl acetate distillation column DC-91 0 and the acetic acid distillation column DC-61 0, respectively. In preparation for the high pressures required for reaction, the acetic acid feed is pumped to 263 psi by the acetic acid feed pump, P-110 (see Unit Description on p. 54). The pure hydrogen feed, S-402, is mixed with the mostly-hydrogen recycle stream S-40 1, and this combined stream is compressed from 213 psi to 263 psi in the compressor CP-410 (see Unit Description on p. 40). This is a very expensive part of the process because of the price of both the . compressor itself and the high electricity requirement. The combined acetic acid stream S-201 is passed through heat exchanger HX-200 (see Unit Description on p. 50), where hot reactor effluent in stream S-206b, heats the acetic acid from a liquid at 242 OF to a partial vapor at 465 OF. In the process, the reactor effluent is cooled to its dew point of280 OF. A different portion of the reactor effluent, stream S-206a, is used to heat the hydrogen feed S-207 from 203 OF to 478 OF in the heat exchanger HX-21 0 (see Unit Description on p. 51). The cooled reactor effluent S-208 exiting HX-21O is also at its dew point of280 OF and 246 psi, this was done for ease of mixing when two reactor effluent streams are reunited. The hot acetic acid and hydrogen

23

streams, S-203 and S-204 respectively, are both fed to the fired heater F-230 (see Unit Description on p. 49), which raises their temperature to 599°F. Optimal reaction conditions occur at approximately 570 of, but the reaction is endothermic, so heat would have to be supplied in order to maintain a constant temperature. Instead, we decided to heat the reactants to a higher temperature rather than attempt to insulate the reactor. The feed temperature of 599 of is well within the range of suggested temperatures for this reaction (Testin, et al.). F-230 is designed to operate on natural gas, but waste material streams OFFGAS and ACETONE WASTE are rich in hydrogen and hydrocarbons and are also burned in F-230. These streams are used to furnish 8,547,300 Btu/hr of the 15,291,600 Btu/hr required to operate the furnace . More energy could be taken from these streams as well as the purge streams, but limiting the amount of energy derived from waste streams to approximately 55% makes controlling the heating rate of the furnace more reliable. Any portion ofthese streams that is not used in the furnace is sent to the flare stack to be burned. The reactor RX-240 (see Unit Description on p. 59) is a cylindrical vessel containing a packed bed of20% wt. Pd- Fe203 catalyst pellets. In order to ensure the proper oxidation state for the desired conversion, the hydrogen and acetic acid are fed in a 5/1 molar ratio. Conversion of acetic acid is only 46 %; this is in order to improve the selectivity to acetaldehyde, which is 86 % under the given conditions. Side products formed in the reactor include ethanol, acetone, carbon dioxide, and light hydrocarbons. The reactor effluent S-206 is at 557°F, and contains, by mass, 11 % hydrogen, 21 % acetaldehyde, and 38 % acetic acid.

24

2. Acetaldehyde Purification

The reactor effluent S-206 is then split into two streams and used to preheat the acetic acid and hydrogen feeds. It is split instead of passing sequentially into the heat exchangers so that both the hydrogen and acetic acid feeds can be heated to higher temperatures. After passing through the heat exchangers, the temperature of the combined stream is 280 of, its dew point. This is hot enough to supply energy sequentially to the reboilers of the azeotropic distillation column (DC-900) and the acetone waste column (DC-81 0), but the amount of steam and cooling water utilities saved would not counteract the need to move the hot fluid over long distances and the associated control complications. After passing through the acetic acid heat exchanger HX-200 and the hydrogen heat exchanger HX -210, the separate reactor effluent streams are mixed together, forming stream S-301. This stream must be cooled further in order to achieve high recovery in the absorber column; cooling water is used to cool the stream to 113 of in HX-300 (see Unit Description on p. 51). This partially condenses the stream, and the cool effluent, S-302 is fed to the flash vessel FV -310 (see Unit Description on p. 50) to separate the liquid and vapor phases. Only the vapor stream S-303 exiting the flash vessel is sent to the absorber AB-320 (see Unit Description on p. 39), which it enters on the bottom stage. The solvent fed to the top stage of the absorber is the acetic acid-rich bottoms product from acetaldehyde distillation column DC-500 (see Unit Description on p. 44). Under the conditions of high pressure (the top stage operates at 233.5 psi), this solvent preferentially absorbs the acetaldehyde, allowing hydrogen, carbon dioxide, and other

25

light materials to escape: 85 % of the acetaldehyde is recovered, but only 3.5% of the ethane (the next-heaviest component) is recovered. The amount of material recycled to the absorber is an important variable in the economics of the process. As the recycle amount increases, the recovery of acetaldehyde increases, but at the expense of larger diameters for both the absorber and the distillation column, as well as a more difficult separation of the acetaldehyde from the water and acetic acid. The selected solvent recycle allows recovery of 95% of the acetaldehyde, while also leaving a feasible separation and relatively low column costs. The pressure of the absorber is also as high as possible in order to improve acetaldehyde recover and limit the amount of work the compressor CP-410 must do. The mainly-hydrogen vapor exiting AB-320 is recycled to the reactor, with a 1.3% purge taken to prevent excessive buildup of light components. This purge stream PURGE2 is burned in the flare stack. The bottoms product from the absorber, S-305, is combined with S-306, the liquid exiting the flash vessel FV-310. S-305 and S-306 contain 10% and 17% acetaldehyde by mass, respectively. At the time of mixing, the pressure is still high, 230 psi. The combined stream S-50 1 is passed through a valve to reduce the pressure to 43 psi before being fed to the acetaldehyde distillation column DC-500. Design of the distillation column to recover acetaldehyde was complicated by several factors. The boiling point of acetaldehyde at atmospheric pressure is 70 OF, so it is preferred to keep the pressure elevated to reduce the need for refrigerants to condense the vapor. However, acetaldehyde fonns an azeotrope with water at pressures higher than 30 psi, and this becomes more water-rich with increasing pressure. In addition, the presence oflight components such as carbon dioxide and methane require adjustments to

26

be made in the distillation. First, they lower the boiling point ofthe mixture further, making it more difficult to use cooling water to condense the distillate. Second, their concentration is high enough that even if the acetaldehyde is completely separated from the heavier components, its purity will still be only 97.2% wt., which is not high enough to be sold. Thus, this column requires a partial condenser with both liquid and vapor distillate: the liquid is taken as the acetaldehyde product, while the vapor distillate is fed to another column where additional acetaldehyde can be removed from the lighter components. Several alternatives were considered before choosing to operate the condenser at 32 psi. Since the liquid-liquid separation of acetaldehyde and water actually increases with temperature, one alternative examined carrying the high pressure from the absorber into the distillation column, then allowing the two liquid phases to separate in a decanter. This method did not produce acetaldehyde at the required purity, was difficult to control, and required very high reboiler temperatures. A second alternative involved using the main column as selected, but also adding an absorbing column, in which the acetic acid-rich bottoms product would be used to absorb acetaldehyde. This did not produce sufficient separation, and the added flow into the distillation column increased the column's cost. The selected design involves operating the condenser of the acetaldehyde distillation column at 32 psi. The distillate vapor fraction was varied to keep the temperature of the distillate at 102 OF, which can be cooled using cooling water. The liquid product, HAC PRODUCT, contains 10,355 Iblhr (82,012,000 Ib/yr) of99.5% wt acetaldehyde. The vapor distillate S-504 is 22 % by mole of the total distillate and contains 2,527 Iblhr of acetaldehyde. Since this is a significant portion of the product, it

27

was necessary to recover as much of this stream as possible. The vapor distillate is then sent to the bottom stage of a small secondary column, DC-51 0 (see Unit Description on p. 46), which has a refrigerated condenser at 10 of. A second product stream, HAC PRODUCT, exits the bottom stage ofDC-510 and contains 24641blhr (19,515,000 lb/yr) of99.7 wt% acetaldehyde. Sixty tons of refrigeration is required at the condenser, and because of the temperature of 10°F is fairly moderate, this can be provided by an ammonia absorption system RF-520 (see Unit Description on p. 64). Decreasing the temperature further would increase the yield of acetaldehyde, but at the expense of more expensive equipment and a larger heat duty. In this design, 71.9 Iblhr (569,000 lb/yr) of acetaldehyde is lost to the stream OFFGAS . This stream, with its high levels of methane, ethane, and ethylene is burned in the fired heater, F-230, to reduce natural gas costs. The acetaldehyde distillation column is also the location of an esterification reaction between ethanol and acetic acid, which forms ethyl acetate and water. Equilibrium for this reaction is achieved wherever acetic acid and ethanol are present together, but for the purposes of this design, it was assumed this reaction occurs only in the bottom stage ofDC-500, where the high temperatures and the presence of acetic acid and ethanol in the liquid phase especially favor this reaction. When equilibrium is reached, over 80% of the ethanol has been reacted. The presence of ethyl acetate is very important in the acetic acid separations section of the process, where ethyl-acetate forms an azeotrope with water, easing the separation of water from acetic acid. The bottoms product S-506 from the acetaldehyde distillation column is split, with part proceeding to the acetic acid separation sequence, and the remainder being cooled by cooling water in the heat exchanger HX-530 (see Unit Description on p. 52) and then recycled to the top

28

stage of the absorber AB-320, where it acts as the solvent to preferentially absorb acetaldehyde.

3.

Acetic Acid separation

The main goal of the acetic acid separation column DC-610 (see Unit Description on p. 46) is to obtain a pure stream of acetic acid, which can be recycled to the reactor feed. The reasons for this are twofold. The primary reason is that the high cost of acetic acid makes it economically feasible for us to reuse the unreacted acetic acid rather than dispose of it. This is particularly relevant because of the low conversion in the reactor, which results in a significant amount of unreacted acetic acid in the system. The second reason is that acetic acid is an impurity in water and its substantial presence in the wasteYv'ater stream will increase costs of wastewater treatment. There are two streams entering the acetic acid distillation column. The feed stream, S 602, is the bottoms from the acetaldehyde separation columns and enters DC-61 0 at the 1i

h

of 30 actual trays. It primarily consists of the unreacted acetic acid and the products

of side reactions such as water, ethyl acetate, acetone, and ethanol. The recycle stream S 603 fed to the second stage is rich in ethyl acetate and is used to facilitate the low boiling water - ethyl acetate azeotrope, which makes the separation of acetic acid in the bottoms easier. The feeds S-602 and S-603 are pumped to 100 psi and 98 psi, respectively, before entering the column. The condenser is operated at 95 psi because as pressure increases, the water-ethyl acetate azeotrope becomes more water-rich, easing the separation from acetic acid. This significantly increases the purity of acetic acid that is collected at the bottoms. lfthe same process were operated at 37.8 psi (the pressure of the feed stream), then the mass fraction is only .92-.93 as opposed to .982 at this pressure. Though the

29

higher pressure increases the cost, it is a cost that is well incurred since the acetic acid increase in the bottoms is critical as it lowers the acetic acid that is lost in the wastewater stream. Further increases in pressure beyond 95 psi cause very marginal increases in the acetic acid mole fraction and do not justify the additional costs. The nwnber of equilibrium stages calculated is 18. The increased separation with additional stages is minimal after 18 stages and does not justify the increasing cost. The calculated tray efficiency is 61 %, meaning 30 actual trays are required. We use a kettle reboiler in this process and a total condenser. A total condenser is used because the distillate must be fed to the decanter DE-720 (see Unit Description on p. 44) as a liquid. Before the distillate enters the decanter, it goes into a mixer, M-700. The mixer incorporates the distillate stream of the acetic acid separation colwnn with the distillate stream of the DC-900 col umn, whiCh primarily consists of ethyl acetate and water, and the bottoms of the acetone separation column, DC-81 0, which contains ethyl acetate that was contained in the water-rich stream coming out of the decanter and water and acetone impurities. The pressure across the mixer drops to 39 psi. This is done because operating the remaining distillation columns in the separation sequence at higher pressure does not produce results that are significantly favorable enough to account for incurring the higher cost when the separating columns were operated at a higher pressure. In addition, this places less of a load on the pump P-730 (see Unit Description on p. 56), which must increase the pressure of recycle stream S-705 to only 40 psi before sending it to the mIxer. The exit stream from the mixer has a temperature of214 of and is cooled to 113 of by passing it through the heat exchanger HX-71 0 (see Unit Description on p. 52). The

30

exit stream from this heat exchanger is fed to the decanter DE-720, which is used to separate the water from the ethyl acetate in the feed stream. The water rich stream S-801 contains 74.8% by mass of water and S-901 contains 77.0% ethyl acetate.

4. Ethyl Acetate Separation

The ethyl acetate-rich organic layer exiting the decanter in stream S-90 1 is sent to the ethyl acetate splitter, which recycles 78.9% of the stream to the acetic acid distillation column where it enhances the separation of water from acetic acid. The rest of the stream is fed into the distillation column DC-900 (see Unit Description on p. 48). Column DC-900 is used to separate water from the acetic acid and ethyl acetate in S-90 1. The low-boiling azeotrope of water and ethyl acetate is taken in the distillate along with acetone and acetaldehyde, leaving a bottoms product that is primarily ethyl acetate and acetic acid. The acetic acid is purified and recycled to the reactor, and the ethyl acetate is sold as a product. The distillate stream of this distillation, S-706, is recycled to the decanter DE-720. This is to separate the water from the ethyl acetate, which is then either recycled to the acetic acid distillation column, or purified for sale. The separation in DC-900 was achieved by using a condenser pressure of 30 psi and 12 equilibrium stages (20 actual trays). A total condenser and kettle reboiler are used in this process. The bottoms product of DC-900, S-902, is 72% ethyl acetate by mass, with acetic acid composing most of the balance. This stream enters the ethyl acetate distillation column, DC-91 0 (see Unit Description on p. 48), at stage 13 of23 (tray 25 of 43). The main purpose of this column is to separate the ethyl acetate from the acetic acid at a level

31

of purity whereby the ethyl acetate can be sold. This column is operated at a condenser pressure of 16 psi and the distillate contains 99.6% mass of ethyl acetate. The bottoms product contains 99.7% by mass of acetic acid and is recycled back to the reactor via the stream S-1 02. Ethyl acetate is stored in a cool, dry, well-ventilated area with a holding capacity of 7300 ft3 (enough capacity to hold 14 days worth of ethyl acetate production) in tightly sealed containers.

5. Acetone and Wastewater Disposal The water-rich stream S-SO 1 exiting the decanter is then sent to the stripper ST -SOO (see Unit Description on p. 66). The condenser is operated at a pressure of25 psi. The bottoms stream of this column is sent to a waste treatment plant for purification before it is disposed off. The distillate, S-S04, primarily contains acetone and ethyl acetate and is fed to the acetone separation column, DC-Sl 0 (see Unit Description on p. 47), at stage S of 11 (13 th of IS actual trays). A partial condenser is used for the stripper because utility costs are decreased by not condensing the vapor and feeding a dew point vapor to the acetone distillation column. The acetone distillation column, DC-S1 0, aims to remove all of the acetone from the feed stream as the distillate and remove it from the system. The acetone in the distillate cannot be made pure enough to be sold as a side product, unlike ethyl acetate. This column has IS actual trays and operates at a condenser pressure of 22 psi. The bottoms product S-707 mainly contains ethyl acetate and is mixed with S-706, the distillate stream of the DC-900 column, via the mixer M-740. The combined stream, S-705, is at 24 psi

32

and is pumped to 40 psi before being fed to the mixer M-700 where it is mixed with the acetic acid separator distillate to be fed into the decanter.

33

.

34

Energy Balance and UtiJity Requirements Because of the high temperatures required for the reactor and the many dis61lation columns, supplying energy for heating and cooling process streams is of paramount concern for the economics of the process. The largest heating and cooling requirements are found in the acetic acid distillation column, which requires 39,534,800 Btu/hr for the reboiler at 370 of and 36,586,600 Btulhr for the condenser. These requirements are satisfied with 300 psia stearn (dropped from its source at 600 psig) and cooling water, respectively. The reboilers and condensers for each of the other columns are handled similarly (using steam at the appropriate pressure), except for the low-temperature acetaldehyde condenser in DC-51 O. The refrigeration unit RF-520 utilizes ammonia absorption to cool a 40% ethylene glycol in water solution that circulates in the condenser. The glycol removes 612,900 Btulhr of heat by partially condensing the distillate ofDC-5IO at 10 OF. Because of heat leak to the surroundings and inefficiencies in heat transfer, we assumed that the ammonia absorption system must supply 900,000 Btu/hr of refrigeration. Assuming the ammonia system operates at -10 OF, 507 Btu/min/ton are required for steam in the generator and 5.4 gpm/ton of water are required for the conditioner (McKetta). The refrigeration load is 75 tons, requiring 2,497,500 Btulhr of steam at 300 OF (68 psi) and 24,000 gpm of cooling water. The acetic acid and hydrogen streams, S-20I and S-207 respectively, which are the reaction starting materials must be heated from 242 OF and 203 OF to 599 OF before entering the reactor. This is above the optimal reaction temperature of 572 OF, but still within the range of recommended temperatures (Tustin, et.a!.). It was heated to this temperature because the primary reaction is endothermic, and by heating above the

35

optimal temperature we allow the temperature in the reactor to decrease as the reaction progresses. This method was used because it was suggested that this would be more efficient than attempting to insulate the reactor at the high temperature required. The reaction consumes 2,677,000 Btu/hr, and the effluent is a total vapor at 557 OF. The hot reactor effluent is split and sent to separate heat exchangers to heat the hydrogen and acetic acid feed streams. The rate of energy transferred to the acetic acid in HX-200 is 4,305,300 Btu/hr, and 8,741,000 Btulhr is transferred to the hydrogen stream in HX-21 O. Following this, the hydrogen and acetic acid feed streams still require 12,692,000 Btu/hr to reach 599 OF; this is accomplished in the fired heater, F-230. Waste streams OFFGAS and ACETONE WASTE are burned to produce 8,547,300 Btulhr, and natural gas is required for the rest of the duty, which because of inefficient heat transfer is 15,291,600 Btulhr total. After being cooled to its dew point by the reactor feeds, the reaction product S-401 is cooled further, to 113 OF by transferring 20,300,000 Btulhr to cooling water in HX-300. The option of using heat from the reactor effluent stream S-401 at 280 OF to heat the reboilers ofDC-900 and DC-810 was examined, but ultimately rejected. There is sufficient energy in S-401 to maintain a 45 OF driving force with the bottoms, but substituting this method for steam heating did not justify the need to pump the hot fluid over long distances and the more complicated control aspects. Heat integration among the condensers and reboilers in the separation section was not attempted because the operating pressures needed to optimize product composition and column costs does not allow for productive stream matching.

36

The utility requirements are summarized in the table below.

Table 2: Heat Transfer Among Process Streams Cold Stream

S-201 S-207

Cold Stream Temperature Change 242°F to 465°F 203°F to 478°F

Hot Stream

Hot Stream Temperature Change 557°F to 280°F 557°F to 280°F

S-206b S-206a

Energy Transferred (BtU/hr) 4,305 ,300 8,741,000

Table 3: Cooling Water Requirements Process Stream or Condenser

Temperature

C-500 102 of C-610 275.2 of C-800 182°F C-810 184 of C-900 182°F C-910 175°F RF-520 S-301 280 of to 113 of S-506a 263°F to 158°F S-703 259 of to 113 of TOTAL REQUIREMENTS

Amount of Cost Cooling Water Duty Cooling Water ($/ru:) (Btu/hr) Required (Gallhr) 10,559,800 85,332 36,586,600 147,824 994,200 4,020 428,700 1,732 2,911,400 11,763 2,059 509,600 24,300 1,503,600 20,300,000 82,020 2,736,000 11,050 3,689,100 14,906 80,219,000 385 ,006 $127.06

28.16 48.78 1.33 0.57 3.88 0.68 8.02 27.07 3.65 4.92

Table 4: Steam Utility Requirements Reboiler

Temperature of Stream

R-500 262.7 of R-610 369.9 of R-810 184.2 of R-900 221.2 of R-910 262.9 of RF-520 300 of TOT AL REQUIREMENTS

Pressure of Purchased Steam (psig)

Steam Heat Duty (Btulhr)

75 16,892,000 600 39,534,800 35 252,312 3,150,280 35 75 486,919 75 2,497,500 \62,813,911

37

Amount of Steam Required (lblhr) 14,195 29,636 215 2,683 409 2,099 ~238

Cost ($Ihr)

35.49 82.98 0.53 6.60 1.02 5.25 $132.00

Table 5: Natural Gas Requirements TotaJD uty 0 fF Ire dB eater (BtU/hr)

15,291,600

Energy from Waste Streams (Btu/hr) OFFGAS

3,604,800

WASTE ACETONE

4,942,500

Natural Gas Required (Btulhr)

6,744,300

Table 6: Electricity Requi.·ements Process Unit CP-410 P-110 P-540 P-600 P-620 P-730 PB-500 PB-610 PB-810 PB-900 PB-910

Electrici ty Required (kW) 459.6 18.7 20.5 3.8 3.1 0.3

Cost ($/hr) 16.086 0.654 0.718 0.134 0.109 0.010 0.262 0.392 0.003 0.013 0.010

7.S

1l.2 0.1 0.4 0.3 l.5 0.2 5.6 0.3 0.1 1.1 0.1

PR-SOO

PR-SlO PR-610 PR-800 PR-810 PR-900 PR-9l0 Total Requirements

534.1

0.OS2

0.008 0.196 0.011 0.003 0.039 0.003 $18.69

The costs listed are what would be paid if these utilities were purchased from an outside source. This was not done for steam and cooling water, because it was determined that building allocated facilities would be more profitable (see Appendix, p.).

38

Unit Descriptions Absorber

AB-320 (see spec. sheet p. 72)

The absorber unit AB-320 is a trayed tower used to separate the acetaldehyde from light hydrocarbons, carbon dioxide, and the unreacted hydrogen that results from feeding that material in large excess. The primary objective of this unit is to recover as much acetaldehyde as possible because 1.3 % of the material leaving through the top of the column leaves the system as PURGE. 23,470 Iblhr of the vapor stream S-303 is fed to the bottom stage of the column, and 62,278 lb/hr of S-304, the solvent recycled from the bottoms of the acetaldehyde distillation column, is introduced on the top stage. This solvent level was chosen to balance the amount of acetaldehyde recovered in the absorber with the ease of separation of the acetaldehyde from the remaining liquid, which contains a lower fraction of acetaldehyde as solvent flow increases. The recovery stream S-305 exits as a liquid from the bottom stage, and has a total flow of 65,871 lb/hr with an acetaldehyde mass fraction of 0.094. S-401 exits the top of the column and contains mostly unreacted hydrogen and light gas side products; 98.7% of this stream is recycled to the reactor, the remainder is purged and burned in the flare stack. The top stage pressure in the absorber is 233.5 psi, with the intention of keeping the pressure as high as possible without resorting to compressing the reactor effluent. The absorber was designed to recover over 85 % of acetaldehyde fed to it, so that the resulting loss to purge would be only approximately 0.15 % of acetaldehyde. This design led to a column containing 15 theoretical trays; the O'Connell correlation was used to calculate the stage efficiency (Seader). This was found to be 51 %, requiring 30 actual

39

trays. Using equations and tables found in Seider, the calculated dimensions were 2.5 ft diameter and a height of 74 ft; the associated bare module cost of the tower and trays is $117,300. IPE calculated a 3 ft diameter, 76 ft. height, and an equipment cost of $120,000. The material used for both the column and the trays is stainless steel because of the concern of corrosion caused by acetic acid.

Compressor

CP-41O (see spec. sheet p. 73)

Compressor CP-41O is a major piece of equipment because of the large expense associated with compressing gases, especially hydrogen. A reciprocal compressor is used to compress 20,404 felhr of the mixed hydrogen stream S-207 from 212.7 psi to 262.8 psi. The temperature of the stream also increases, from 152.3 OF to 202.6 oF. The load required was limited as much as possible by maintaining high pressures throughout the reactor section of the process, while still ensuring that the feed to the compressor was above its dew point. The power is 330.9 kW, and the efficiency is estimated by Aspen to be 72%. This leads to an electricity requirement of 459.6 kW. The material used was stainless steel, and the bare module cost was calculated to be $2,628,000.

Condensers

C-500 (see spec. sheet p. 74)

Condenser C-SOO is a partial condenser that is used for the acetaldehyde distillation column, DC-500. A partial condenser with both liquid and vapor distillate is employed for two reasons. First, the significant concentration of light compounds such as carbon dioxide would cause the acetaldehyde purity in the product to be too low if a

40

single disti llate stream was taken. Second, condensing those light gases and all of the acetaldehyde would require very low temperatures and a large amount of refrigeration. Instead, the fraction of vapor distillate was set in order to have a distillate temperature of 102 of, which can be achieved with cooling water. To accomplish this, 22% of the distillate remains vapor; this stream (S-504) contains approximately 20% of the acetaldehyde produced, and this is recovered in the DC-51 0 column. The condenser is made of stainless steel, and has a heat duty of 10,559,800 Btulhr. Using a heat transfer coefficient of97.6 BtU/(hr-ft2-0F), B-JAC estimates a surface area of 13,109 ft2; because of this large size and the temperature crossover of the hot and cold stream temperatures, B-JAC split this exchanger into two in series. A 1-8 shell-and-tube heat exchanger was designed, with a length of 8 ft., and shell size of 70 in. The estimated installed cost from B-JAC is $209,960.

C-520 (see spec. sheet p. 75) C-520, a partial condenser with all vapor distillate, is used for DC-51 0, the refrigerated acetaldehyde recovery column. If a liquid distillate were condensed, the temperature requirement would be unreasonably low, and there is little processing benefit from having a liquid distillate. The heat duty of the condenser is only 612,900 Btu/hr at 10°F, making refrigerant cooling a practical solution for this process. A 40%-ethylene glycol in water solution is circulated in the condenser to cool the distillate. The heat transfer coefficient estimated by B-JAC is only 32 .2 Btu/(hr-ft2-0F), and the required surface area is 403.2 ft2. In order to limit the amount of glycol solution needed to cool the condenser, the solution is heated from -5 OF to 30 OF; because of the temperature

41

crossover, two condensers, both 1-2, are required in series. The length ofthe tube is 14 ft., and the shel1 width is 10.75 in. The material used was stainless steel. The estimated installed cost reported by B-JAC was $16,600.

C-610 (see spec. sheet p. 76) The condenser used for the acetic acid distillation column is a total condenser, because in the next step in the process the liquid distillate is fed to the decanter DE-720. Cooling water is used, and the exiting distillate has a temperature of275 of. The heat duty is 36,586,600 Btu/hr, and using an estimated heat transfer coefficient of 129 BtU/(hr ft 2 _OF), the required surface area is 2,494 ft2. A single 1-4 shell-and-tube heat exchanger is used for this process. The tube length is 10ft., and the shell diameter is 38 in. Using stainless steel as the material, B-JAC estimated the installed cost of this item to be $64,710.

C-800 (see spec. sheet p. 77) For the stripper, a partial condenser was used because sending S-804 to the acetone distillation column DC-81 0 as a vapor reduced the overall utility requirements without significantly altering the separation. The condenser C-800 is a 1-4 shell-and-tube heat exchanger, made of stainless steel. The required heat duty is 994,200 Btu/hr, and using a heat transfer coefficient of 112 Btu/(hr-ft2 -OF), the required surface area is 112.2 ft2. The shell diameter is 8.6 inches and the tube length is 16 ft. The installed cost is $7,570.

42

C-810 (see spec. sheet p. 78) The condenser for the acetone distillation column DC-81 0 is a 1-4 shell-and-tube heat exchanger made of stainless steel. The heat duty is 428,700 Btu/hr, with a distillate temperature of 168 of. A partial condenser with all vapor distillate was used because the distillate stream WASTE ACETONE is being burned in the fired furnace, so it is unnecessary to condense the stream. The heat transfer coefficient is 95 Btu/(hr-ft2 _OF), and the resulting area is 78 ft2. The tube length is 10ft., and the shell diameter is 8.6 in. The installed cost is $6,700.

C-900 (see spec. sheet p. 79) A total condenser is used for the near azeotrope distillation column DC-900. The heat exchanger is a 1-2 shell-and-tube heat exchanger made of stainless steel. This condenser subcools the product to 2 of below the saturation temperature so that when the disti llate is mixed and fed to the pump P-730, the feed stream is a total liquid. The distillate temperature is 18l.9 of, and the heat duty is 2,911,400 Btu/hr. Using a heat transfer coefficient of 105 Btu/(hr-ft2 _OF), B-JAC estimated the required surface area to be 275 ft2. The tube length is 14 ft., and the shell thickness of 12.75 in. The installed cost is $9,250.

C-910 (see spec. sheet p. 80) A total condenser is used for the ethyl acetate distillation column so that the liquid ethyl acetate can be recovered and stored. C-910 is a 1-8 shell-and-tube heat exchanger made of stainless steel. The distillate temperature is 175 of, and the heat duty is 509,600

43

Btulhr. The effective surface area based on an estimated heat transfer coefficient of72.6 Btul(hr-ft 2_OF) is 473 ft2. The tube length is 6 ft., and the shell diameter is 24 in. The installed cost is $18,470.

Decanter

DE-720 (see spec. sheet p. 81)

The purpose of the decanter is to separate water from the ethyl acetate in the inlet stream

S ~ 704.

It achieves this to an extent of getting a water-rich stream, S-80 1 with

74.8% by mass of water and an ethyl acetate rich stream, S-901 with 77 .0% by mass of ethyl acetate. The outlet temperature of the decanter is 117 .5°F and its outlet pressure is 35.5 psi . The capacity of the decanter is based on a 10 minute residence time at half full and equals 214 ft3. The decanter is a horizontal, stainless steel vessel, with a diameter of 4.5 ft. and length of 13.5 ft; using cost charts, we determined its bare module cost to be $63,000.

Distillation Columns

DC-500 (see spec. sheet p. 82)

DC-500 is the major unit for separating acetaldehyde from the heavier components in the reactor effluent: acetic acid, water, acetone, ethyl acetate, and ethanol. Even though acetone's boiling point is closest to acetaldehyde's, the key heavy component in this separation is water because of its high concentration. At pressures as low as 30 psi, water forms an azeotrope with acetaldehyde, which becomes richer in water as pressure increases. As a result of this, the pressure of the condenser was set at 32 psi to limit the recovery ofthis azeotrope. Acetaldehyde's relatively low boiling point

44

(10°F) makes this low pressure undesirable because of difficulties in condensing the material, but attempted higher pressure methods such as liquid-liquid separation from water could not produce acetaldehyde in the needed purity. Fenske-Underwood-Gilliland calculations provided the minimum number of stages as 20 and the minimum reflux ratio as 1.61. At 1.3 times the minimum reflux (LID = 2.09), the Gilliland correlation yields the estimated number of stages as 40. This actual conditions used in the simulation were a reflux ratio of 2.40, and 40 equilibrium stages. The tray efficiency is 56%, necessitating 71 actual trays. Stream S-501 enters above the 50 th stage to provide a larger rectifying section, allowing better purification of the acetaldehyde distillate. Using cost charts available in Seider, the distillation column dimensions are 4.5 ft in diameter, and 157 ft. taB; the estimated cost of the column and trays was $1,013,500. IPE estimated the column dimensions as a 4 ft. diameter and 171 ft. height. The material and labor cost using lPE was estimated as $1,087,000. The height was determined by taking a 2-f1. tray spacing, a 4-ft. disengagement height for the condenser, and a 10-ft. bottoms sump. DC-500 also has the esterification reaction in which acetic acid and ethanol react to form water and ethyl acetate (Reaction 5, p. 10). This reaction is very important to the process, and the patent describes adding sulfuric acid to catalyze this reaction if it does not occur in sufficient yield. Under the conditions of this column, that step was not necessary. This reaction is important because ethyl acetate is needed in the acetic acid separation section to form a low-boiling azeotrope with water in order to facilitate the separation of water from acetic acid. The ethyl acetate-water product is favored thermodynamically, and under the reaction conditions over 80% of the ethanol reacts.

45

The ethyl acetate can then be purified, and we are able to purify and sell 1,139 Ib/hr of ethyl acetate. HAC PRODUCT, the liquid distillate, contains 99.5 % acetaldehyde by mass at a flow of 10,355 Ib/hr. The bottoms product, S-506, contains 92,140 Iblhr of 72.4 %wt acetic acid, with water being the other major component. Only 9.6 Ib/hr of acetaldehyde is in this stream. S-506 is split, with part returning to the absorber AB-320 as the solvent, and the remainder proceeding to the acetic acid separations section, where pure acetic acid is recycled to the reactor and ethyl acetate is purified for sale.

DC-510 (see spec. sheet p. 83) The column DC-51 0 contains only a rectifying section and is intended to condense acetaldehyde from the vapor distillate of the main acetaldehyde distillation column. S-504 enters the column on the bottom stage, from which the second acetaldehyde product HAC PRODUCT is also taken. The temperature of the condenser is 10°F, and indirect refrigeration is provided via an ammonia absorption-ethylene glycol system. Theoretically, the number of stages required to recover pure acetaldehyde in good yield is only three, but low tray efficiency (26 %) caused by the large relative volatility of ethane to acetaldehyde leads to the need to for eight actual trays. The height of the column is 30 ft, and its diameter is 1.5 ft. Stainless steel is used for the tower and trays. The bare module cost of the column, using cost charts, is $62,500.

DC-610 (see spec. sheet p. 84) The acetic acid separation column was designed for 18 equilibrium stages. The efficiency is 61 %, and the actual number of trays is 30. Assuming a 2-ft. tray spacing, as

46

well as the sump and disengagement heights, the height ofthe column is 74 ft., and the diameter is 10.5 ft. The acetic acid-rich stream recovered as the bottoms of the acetaldehyde distillation column enters DC-610 at tray 17. The ethyl acetate-rich recycle stream S-603 enters the colurrm on the second tray and is used to form the ethyl acetate water azeotrope, which makes the separation of acetic acid from water simpler. The bottoms rate is 20,744 lblhr, the molar reflux ratio is 2.5 and the condenser pressure is 95 psi. On the recommendation of the industrial consultants, stainless steel was the material chosen for the tower and the trays. This is because acetic acid has a corrosive effect on carbon steel and stainless steel is sufficiently corrosion resistant. The bare module cost of this column with trays is calculated to be $1,491,200.

DC-810 (see spec. sheet p. 85) This acetone distillation colurrm is designed to remove the acetone from the system in the distillate to be used as fuel in the fumace. The distillate stream, ACETONE WASTE, primarily contains acetone, ethyl acetate and water with very small quantities of acetaldehyde and ethanol. The bottoms stream, S-707, contains 80.8 % ethyl acetate and 10.3 % water. Eleven equilibrium stages were designed for the column; the tray efficiency of 60.8 % implies the need for 19 actual trays. Using 2-ft. tray spacing, and 14

•

ft. total for the sump and disengagement heights, the column is 52 ft. tall, with a 1.5 ft.

diameter. Based on the flow rates a smaller diameter is necessary to avoid flooding, but the 1.5-ft. diameter produces an aspect ratio of 35, which is much more reasonable. The stripper distillate stream S-804 enters the column at tray 13. The distillate rate is 439 lblhr, the molar reflux ratio is 4 and the condenser pressure is 22 psi. Stainless steel was also the material of choice for this column. Its bare module cost is $103,600.

47

....

DC-900 (see spec. sheet p. 86) Th.is column is designed to remove the acetone, ethanol and the ethyl acetate-water azeotrope as the distillate and isolate the acetic acid and the remaining ethyl acetate in the bottoms. The ethyl-acetate rich stream S-901 from the decanter is fed at the 10th tray. Twelve equilibrium stages are needed for the separation, and the efficiency is 60%, requiring 20 actual trays. To that end, this separation column is 54 ft in height and has a diameter of 2 ft. The distillate rate is 4356 lblhr, the reflux ratio is 1.8 and the condenser pressure is 30 psi. Stainless steel was also the materiaJ of choice for this column. Its bare module cost is $150,532.

DC-910 (see spec. sheet p. 87) This ethyl acetate distillation column is designed to purify ethyl acetate as the distillate to a level at which it can be sold. The bottoms product is acetic acid, which is recycled to the reactor. Twenty-three equilibrium stages are needed for this separation; the tray efficiency is 41.5 %, and the actual number of trays is 45. This separation column is 104 ft in height and has a diameter of 3 ft. Stream S-S-804 enters the column at tray 25. The distillate rate is 1139 lblhr, the reflux ratio is 1.8 and the condenser pressure is 16 psi. Stainless steel was also the material of choice for this column. Its bare module cost is $433,400.

48

Fired Heater

F-230 (see spec. sheet p. 88) In order to completely heat the hydrogen and acetic acid feed streams, S-204 and S-203, to the desired reaction temperature, energy must be supplied by burning fuel in the fired heater F-230. F-230 is a vertical cylindrical fired heater. 20,402Ib/hr of the gaseous hydrogen feed S-204 at 478 of and 42,571 lblhr of the partial vapor S-203 at 465 OF are fed to F-230 separately because they are different phases. The heat duty required to raise the temperature of the streams to 599 OF to prepare for the reactor is 12,692,000 Btulhr. Assuming a stack temperature of 650 of, according to McKetta the efficiency is 83% and thus the required total heat duty is 15,291,600 Btulhr. This is furnished by burning natural gas, along with waste streams from the process: OFFGAS and ACTONE WASTE. The cost for this unit was estimated based on a design heat duty of 20,000,000 Btu/hr. This leads to an installed cost of $609,400 (Walas). The material used is stainless steel because it is able to handle the high temperatures and also will not corrode in the presence of acetic acid. Of the 15,291,600 Btulhr required to heat the process streams, 8,547,300 Btulhr (56 %) is supplied from burning the process streams. This amount was chosen in order to balance the cost of natural gas that must be bought with the control and safety concerns that would be associated with using waste streams for nearly all of the energy in the heater.

49

Flash Vessel

FV -310 (see spec. sheet p. 89)

The flash vessel FY -310 is used to separate the liquid and vapor portions of the reactor effluent leaving the heat exchanger HX-300. The volumetric flow rate into the flash vessel is 101,146 ft 3lhr. The required volume, determined by considering a 5 minute holdup time at half full, is 16,860 ft3. This is a large process vessel, and the diameter was set at 17 ft., so that it would not have to be fabricated on the site. The length height is 76.5 ft. This is made of stainless steel because of the corrosion caused by acetaldehyde and acetic acid. The bare module cost for the flash vessel is $1,832,000.

Heat Exchangers HX-200 (see spec. sheet p. 90) HX-200 is used to increase the temperature of the acetic acid feed stream S-20 1 from 242 OF to 465 OF, where it is a partial vapor. To do this, 20,783 lb/hr of reactor effluent S-206b is cooled from 557°F to 280°F, its dew point. The amount of heat transferred is 4,305,300 Btulhr, and the estimated heat transfer coefficient between the vapor and liquid was 10.8 BtU/(hr_ft2 _OF). This is relatively low for what is primarily liquid-vapor heat exchange. It is a 1-1 shell-and-tube heat exchanger made of stainless steel. The surface area is 8,343 fe, the tube length is 20 ft., and the shell diameter is 48 in. The cost estimated by B-JAC was $194,840.

so

HX-210 (see spec. sheet p. 91) In HX-210, 20,840 lb/hr of the hydrogen feed stream S-201 at 202.6 of 1S heated to 477.6 of by cooling 42,1961b/hr of the reactor effluent S-206a from 557 of to 280°F. This temperature is chosen because it is the dew point of S-206a at the operating pressure, and having only vapor will ease mixing with S-206b, which is also cooled to its dew point. This is a 1-1 shell-and-tube heat exchanger, which requires three exchangers in series because of the large surface area required . The amount of heat transferred is 8,741,000, and using B-JAC the heat transfer coefficient was estimated to be 16.7 Btu/(hr-ft2_OF). The total required surface area is 8920 ft2, and the dimensions are a 10ft. tube length and 60 in . shell diameter. HX-210 is composed of stainless steel to prevent corrosion. The installed cost estimated by B-JAC was $630,750 for the three in series.

HX-300 (s ee spec. sheet p . 92) HX-300 is used to decrease the temperature of 62,979 Iblhr of the cooled reactor effluent S-301 from 280°F to 113°F in order to increase the recovery of acetaldehyde in the absorber AB-320 . S-301 enters as a dew point vapor, and is partially condensed in the heat exchanger. Cooling water is used to transfer 20,300,000 Btulhr from S-301. The heat exchanger is a 1-8 shell-and-tube heat exchanger made of stainless steel. The estimated heat transfer coefficient used was 70.9 Btul(hr-fe-OF), requiring a size of6687 ft2. The tube length is 12 ft ., and shell diameter is 58 in. The estimated installed cost for HX-300 is $163,820.

51

HX-530 (see spec. sheet p. 93) Stream S-506a, the solvent for the absorber, flows at a rate of 62,278 Ib/hr and a temperature of 263 of into the heat exchanger HX-530. Cooling water is used to lower the temperature to 157 of because more acetaldehyde is absorbed when the feeds to the absorber are at lower temperatures. The required heat transfer rate is 2,736,000 Btulhr. The estimated heat transfer coefficient in B-JAC is 105 Btu/(hr-fe_OF), which appears to be reasonable for liquid-liquid heat transfer. The required area is 320 ft2, and the estimated price is $10,750. The material used for the heat exchanger is stainless steel, and it is a 1-2 shell-and-tube exchanger. The tube length is 20 ft., and the shell diameter is 10.8 in.

HX-710 (see spec. sheet p. 94) HX-710 employs cooling water to reduce the temperature ofthe S-703 from 260.3 OF to 113.0°F before it is fed to the decanter DE-720. The exchanger has a heat duty of 3,689,100 Btu/hr. A heat transfer area of 921 ft2 is calculated for HC-71 0 in B-JAC based on an overall heat transfer coefficient of95.4 Btu/(hr-ft2-0F). It is a 1-6 shell-and-tube heat exchanger with the following dimensions: tube length is 20 ft., shell diameter is 18 in. Stainless steel is the material of construction, and the installed cost is $15,940.

52

Mixers

M-220, M-310 Both M -220 and M-31 0 are used to mix reactor effluent, and a small pressure drop is assumed across each. M-220 mixes 20,783 lb/lrr ofS-202 and 42,196 lb/hr ofS 208, both at 280 OF and 246 psi, the dew point of the vapors. These streams had been used to heat the acetic acid and hydrogen feeds . These streams are mixed to allow a single heat exchanger, HX-300, to cool the streams before feeding the resulting vapor stream to the absorber AB-320. M-310 mixes 65,871 lblhr of the recovered absorber bottoms S-305 and 39,510 lblhr of the liquid stream S-306 exiting the flash vessel. There is a pressure drop of 5 psi across the mixer; this pressure drop can be almost arbitrarily large, because the mixed stream is then passed into the valve V-50 1 to decrease its pressure to 45 psi before entering the acetaldehyde distillation column DC-500.

M-400 Mixer M-400 combines the pure hydrogen gas feed at 215 psi a and 77 OF with the hydrogen-rich stream S-402a at 159 OF and 233 psi. The pressure of the combined stream is decreased to 213 psia. This pressure is low enough to ensure that the vapor is above its dew point and no liquid will be fed to the compressor. The outlet temperature is 152 OF.

M-700 M-700 combines the 31,444 Iblhr liquid distillate from the ace6c acid distillation column at 275.2°F and 95 psi with the recycle stream S-702 which is at 182.5 °F and 40

53

psi and has a flow rate of 5, 111 Ib/hr. It integrates the two streams to liquid stream S-703 and lowers the pressure to 39 psi, with the corresponding temperature of214.1 of.

M-740 M-740 combines the 43561blhr liquid stream S-706 (distillate from the near azeotrope distillation column) at 181.9 of and 25 psi with liquid stream S-707 (the bottoms from the acetone distillation column) which is at 184.3°F and 24.9 psi and has a flow rate of755 lb/hr. The combined stream is a liquid with a flow rate of 5,111 Ib/hr at 182.3 OF and 24.7 psi.

Pumps

P-I10(seespec. sheetp. 95)

Pump P-ll 0 is used to increase the pressure of the combined acetic acid feed stream S-1 04 to 263 psi, so that it will be at the proper pressure for reaction. The entering stream is at ambient pressure because it includes the pure acetic acid feedstock S-101, assumed to be at 14.7 psi. The net required power is 9.7 kW, but since the efficiency is only 0.52 the total power supplied is 18.6 kW. This result from the simulation agrees well with the hand-calculation for required power included in the appendix. This is a centrifugal pump made of stainless steel. The purchase cost, determined from cost charts, is $11,570 and the bare module cost is $57,860.

54

P-540 (see spec. sheet p . 96) Pump P-540 is used to increase the pressure of the absorber solvent stream S-507 from 31.8 psi to 235 psi so that it can be fed to the top stage of the absorber AB-320, which is at high pressure to maximize acetaldehyde recovery. The volumetric flow rate is 1149 ft3/hr. The power requirement is 9.7 kW, but the efficiency is 0.52, so the total power is 18.6 kW. This is a stainless steel centrifugal pump, and the bare module cost is $57,860.

P-600 (see spec. sheet p. 97) Pump P-600 is used to increase the pressure of the acetic acid distillation column feed from 37.8 psi to 100 psi. The power requirement is 1.86 kW, but because of the efficiency of only 0.485, 3.83 kW of electricity is necessary. This is a stainless steel centrifugal pump, and the bare module cost is $30,860.

P-620 (see spec. sheet p. 98) P-620 pumps the S-901 recycle stream from the stream splitter to the second stage of the acetic acid distillation column DC-61 O. It increases the pressure ofthe stream from 85 psi to 98 psi . The temperature of the stream is virtual1y unaffected by this change in pressure. An efficiency of 0.44 is used for the centrifugal pump. The electricity 3

requirement is 3.1 kW. The volumetric flow rate is 400 ft 1hr. The estimated bare module cost is $28,930.

55

P-730 (see spec. sheet p. 99) P-730 pumps the recycle stream S-705 from the mixer M-740 to the mixer M-700. It increases the pressure of the stream from 24.7 psi to 40 psi. The temperature of the stream is increased from 182.3°F to 183.4°F by this change in pressure. An efficiency of 0.27 is used for the centrifugal pump. The electricity requirement is 0.27 kW. This is a stainless steel centrifugal pump, and the flow rate is 98 ft 3l1rr. The estimated bare module cost is $12,860.

PB-500 (see spec. sheet p. 100) The reboiler pump for the acetaldehyde distillation column DC-500 is a centrifugal pump made of stainless steel, and used to pump the bottoms of DC-500. The capacity is 289 gpm, and its power requirement is 7.46 kW. The estimated bare module cost of the pump is $18,000. ·

PB-610 (see spec. sheetp. 101) The reboiler pump for the acetic acid distillation column is constructed from SS304. It has a design pressure of 93.65 psig, a design temperature of 408.30°F and a driver power of 11.2 kW. It is a centrifugal pump. The bare module cost is estimated to be $45,000.

56

PB-SI0 (see spec. sheet p. 102) The reboiler pump for the acetone distillation column DC-Sl 0 is constructed from SS304. It has a design pressure of 15.00 psig, a design temperature of215.97°F and a driver power of 0.1 kW. Based on cost charts for centrifugal pumps, the bare module cost is $10,930.

PB-900 (see spec. sheet p. 103) The reboiler pump for the near azeotrope column DC-900 is constructed from SS304.

It has a design pressure of 15.00 psig, a design temperature of 231.94°F and a driver power of 0.37 kW. It is a centrifugal pump, and the bare module cost for this pump is $14,410.

PB-910 (see spec. sheet p. 104) The reboiler pump for the ethyl acetate distillation column DC-91 0 is constructed from SS304. It has a design pressure of 15.00 psig, a design temperature of 312.94°F and a driver power of 0.3 kW. The bare module cost for this centrifugal pump is $13,540.

PR-500 (see spec. sheet p. 105) The reflux pump for the acetaldehyde distillation column DC-500 is a stainless steel centrifugal pump with a capacity of67.6 gpm. The work output is 1.49 kW, and the bare module cost is $21,210.

57

PR-510 (see spec. sheet p. 106) PR-510, the reflux pump for the refrigerated acetaldehyde recovery column, is a centrifugal pump made of stainless steel. Its capacity is 3.5 gpm at a driver power of 0.25 kW. The estimated bare module cost is $12,860.

PR-610 (see spec. sheet p. 107) PR-610 is the reflux pump for the acetic acid distillation column. The required power is 5.6 kW. It is a stainless steel centrifugal pump. The bare module cost is $35,360.

PR-800 (see spec. sheet p. 108) The reflux pump for the stripper S-800 is made of stainless steel. It is a centrifugal pump with required power of 0.25 kW. The bare module cost is $12,860.

PR-810 (see spec. sheet p. 109) The reflux pump for the acetone distillation column is a centrifugal pump and made of stainless steel. The power required is 0.1 kW, and the bare module cost is $10,290.

PR-900 (see spec. sheet p. 110) The power for the reflux pump for DC-900 is 1.1 kW. It is a centrifugal pump, and the material is stainless steel. The bare module cost is $19,930.

58

PR-910 (see spec. sheet p. 111) The reflux pump for the ethyl acetate distillation column is made of stainless steel. It is a centrifugal pump with driver power of 0.1 kW. The bare module cost is $10,290.

Since the purchase cost for each of the pumps listed above is relatively small compared to the total capital investment of this process, a spare for each pump was purchased to avoid long delays if a pump goes out of service.

Reactor

RX-240 (see spec. sheet p. 112)

The process unit RX-240 is a packed-bed reactor filled withPd-Fe203 catalyst pellets. The design ofthe reactor was limited somewhat by the reaction information available in the Eastman Chemicals patent regarding this process (Tustin et aL, U.S Pat. No.6, 121,498). The desired reaction (1) is the reduction of acetic acid to form acetaldehyde. CH 3 COOH + H2 -) CH 3CHO + H 20

(1)

In the hydrogen-rich environment of the reactor, acetaldehyde can be further reduced to ethanol (2). CH 3CHO + H2 -) CH J CH20H + H 2 0

(2)

In process simulations, reaction (2) was not modeled as a sequential reaction, but instead the following direct hydrogenation of acetic acid was used:

59

(2a) A major factor in the design of the catalyst for this process was to promote (1), while suppressing (2). This can also be accomplished by lowering the acetic acid conversion: at higher space velocity (low conversion) the selectivity to acetaldehyde is enhanced. Other side reactions that were considered in designing the reactor were the production of acetone from acetic acid (3), as well as the formation of light hydrocarbons (4).

Reaction (4) is used merely as a material balance to account for side products listed in the patent. Selectivity to methane and C2 hydrocarbons (ethylene and ethane) was presented as 2% total, so we assumed 1 % to methane and 0.5% for each ethylene and ethane. The reaction conditions allow 46% conversion of acetic with reaction selectivities listed in Table 7.

Table 7: Reaction Selectivity Reaction Number 1 2a 3 4

Reaction

CH 3 COOH + H2 ~ CH 3CHO + H 2O CH 3COOH + 2 H2 ~ CH 3 CH 20H + 2 H 2O 2 CH 3COOH ~ CH 3 COCH 3 + CO 2 + H 2O 3 CH 3 COOH + 9 Hz ~ 2 CH 4 + C2~ + C 2H 6 + 6 H 2O

Selectivity (Acetic Acid Conversion) 89% 5% 4% 2%

The gas hourly space velocity (GHSV) for volumes of gas per volume of catalyst was reported as 2600 hr- 1 under the reaction conditions. The catalyst consists of 20% palladium on iron oxide pellets. Based on a feed gas flow rate into the reactor of 224,307 ft 3/hr, this implies a catalyst bed volume 0[86.3 ft 3 (see Appendix for Calculations). The reactor diameter is 4 ft., and the height of the catalyst bed is 6.9 ft. In

60

addition, the reactor has a 6 ft. footer, O.S ft. distributor, O.S ft. catalyst support, and a 3 ft. header. The total height of the reactor is 17 ft. The bare module cost ofthe reactor, a vertical vessel, is $267,400. A catalyst density of 42 lb/ ft3 was assumed, producing 3623 lb of catalyst in the reactor. At a price of $1 ,6S0/lb (Dr. Rob Becker), the cost for a charge of catalyst is $S,979,000. The operating conditions for the reactor are based on the optimal conditions described in the patent: the feed enters at S99 of and 2S2 psia, with a hydrogen to acetic acid ratio of SI1 by mole. Under the conditions of the patent, the catalyst does not show significant degradation in perfonnance with time on stream, and because coking is not considered a risk, we assumed a catalyst replacement of20 % per year (Vrana), or complete replacement once every five years. The material of construction for the reactor is stainless steel. One benefit of the catalyst described in the patent for the process is the ability to use relatively inexpensive materials of construction compared to more corrosive methods employed earlier. It was suggested that carbon steel may be satisfactory for the material, since gaseous acetic acid is not expected to be corrosive. However, on the suggestion of Bruce Vrana to limit possible sources of corrosion throughout the process, we decided to use stainless steel for this vessel. Stainless steel is also stable at the reaction temperature; it is classified as suitable up to SOO °C (932 OF) (Perry).

Reboilers R-SOO (see spec. sheet p. 113) The reboiler for the acetaldehyde distillation column DC-SOO is a kettle reboiler constructed from stainless steel. The heat duty is 16,892,000 BtU/hr at a bottoms

61

temperature of262.7 of. Steam purchased at 75 psig is used to provide the energy. Two reboilers in parallel are used, and the effective heat transfer area is 8,108 ft2. The estimated heat transfer coefficient is 105 Btu/(hr-ft 2_OF). The installed cost calculated by B-JAC is $153,460.

R-610 (see spec. sheet p. 114) The reboiler for the acetic acid distillation column, constructed of stainless steel, employs 600 psig steam for the 39,534,800 BTUlhr heat duty. The process fluid is at a pressure of 98 .6 psi. The heat transfer area required is calculated to be 7,200 ft2 assuming a heat transfer coefficient of 112.5 BtU/(hr-ft2_OF). Its installed cost is $126,330.

R-8J 0 (see spec. sheet p. 115)

The reboiler for the acetone distillation column, constructed of stainless steel, employs 35 psig steam for the 252,310 Btu/hr heat duty. It is a kettle reboiler. The process fluid is at a pressure of 22 psi. The heat transfer area required is calculated to be 120.2 ft2 assuming a heat transfer coefficient ofl 02 BtU/(hr_ft2 _OF) . Its installed cost is $10,620.

R-900 (see spec. sheet p. 116) The reboiler for the distillation column DC-900, constructed of stainless steel, employs 35 psig steam for the 3,150,280 Btulhr heat duty. The process fluid is at a pressure of 30 psi. The heat transfer area required is calculated to be 626

62

ft? assuming a

heat transfer coefficient ofl 0 l.5 Btu/(hr-ft2 _OF). The installed cost for this kettle reboiler is $15,520.

R-910 (see spec. sheet p . J J 7) The reboiler for the ethyl acetate distillation column, constructed of stainless steel, employs 75 psig steam for the 486,920 Btu/hY heat duty. The process fluid is at a pressure of 20.1 psi . The heat transfer area required is calculated to be 109 ft2, based on an estimated heat transfer coefficient of 100 Btul(hr-ft2_OF). Its installed cost is $8,740.

Reflux Accumulators

D-500 (see spec. sheet p . J 18)

Liquid reflux from the top stage of the acetaldehyde distillation column DC-500 is returned to the reflux accumulator D-500. The vessel is stainless steel to prevent corrosion from acetic acid or acetaldehyde. It is a horizontal vessel with diameter equal to 3.5 ft. and a height of 10ft. The capacity of the accumulator is 852 gallons, and the estimated bare module cost is $41,600.

D-510 (see spec. sheet p. J J 9) The reflux accumulator for the refrigerated acetaldehyde recovery column DC 510 is made of stainless steel and has a capacity of 53 gal. Its diameter is 1.5 ft, and it's length is 5.5 ft. The material is stainless steel and the estimated bare module cost is $16,624.

63

D-61O (see spec. sheet p. 120) This reflux accumulator for the acetic acid distillation column is constructed of SS304 and has a capacity of 3000 gallons. The dimensions of the vessel are 5.0 ft in diameter and 20.0 ft in length. Its bare module cost is $93,510.

D-SOO (see spec. sheet p. 121)

This reflux accumulator for the stripper, constructed of SS304, has a capacity of 66 gallons. The dimensions of the vessel are 1.5 ft in diameter and 6.0 ft in length. Its bare module cost is $17,350.

D-810 (see spec. sheet p. 122) The reflux accumulator for the acetone distillation column has a capacity of 50 gal. It is a horizontal vessel with 1.5 ft diameter and 5.5 ft length. The material is stainless steel, and the bare module cost is $17,660.

D-900 (see spec. sheet p. 123) This reflux accumulator for this distillation column is constructed of SS304 and has a capacity of 187 gallons. The dimensions of the vessel are 2 ft in diameter and 8 ft in length. Its bare module cost is $21,820.

D-910 (see spec. sheet p. 124) This reflux accumulator for the ethyl acetate distillation column, constructed of SS304, has a capacity of 48 gallons. The dimensions of the vessel are 1.5 ft in diameter and 5.5 ft in length. Its bare module cost is $17,663.

64

Refrigeration System RF-520 (see spec. sheet p. 125) The refrigeration unit was not rigorously designed, but the estimated costs of purchasing and operating a packaged unit were analyzed. This refrigeration unit cools an ethylene glycol solution, which in turn is used to provide a heat duty of 612,900 Btu/hr to the condenser C-520 at 10°F. Assuming "heat leak" of 30% of refrigeration produced, the refrigeration unit was designed to operate at 900,000 Btu/hr (75 tons). Since heat would be transferred indirectly through a glycol solution, the refrigeration unit itself was designed to operate at -10°F. Lower temperature refrigeration could be achieved to recover a larger fraction of acetaldehyde, but at lower temperatures refrigeration becomes considerably more expensive and more heat loss is expected. According to costing estimates, a refrigeration unit this size costs $356,800 installed (Walas). Because of uncertainties regarding how complete this quoted system is, and factoring in costs for the glycol solution and holding tanks, we set the installed cost at $500,000 for this unit. Operating costs were estimated based on the amount of steam and cooling water required to generate and condense ammonia vapor (McKetta) .

Splitters SPLIT, SPLIT2, PRODSPL PRODSPL is used to split the reactor product S-206 into two separate streams to heat the acetic acid and hydrogen feeds. This is done rather than introduce S-206 to the heat exchangers sequentially because it allows the temperature of both S-201 and S-207

65

iIii

to be raised to nearly the same value. Because of the difference in the calculated heat duties in HX-210 and HX-200, one third of the S-206 is sent to HX-200, with the remainder passing to HX-21 O. SPLIT splits the hydrogen rich gas stream exiting the absorber AB-320 into a recycle to the reactor, and PURGE, which is flared. The flow rate into SPLIT is 19,877 Ib/hr, and 98.7 % is recycled to the reactor. This split fraction is as high as could be practically designed without causing excessive buildup of light components in the process. SPLIT2 splits 92,140 lblhr of S-506 into the solvent for the absorber AB-320 at 62,277 lb/hr and the balance to the acetic acid distillation column. SPLIT2's role is to recycle acetic-acid rich solvent back to AB-320 where it absorbs acetaldehyde. The split fraction was set by the interest of maximizing recover of acetaldehyde without causing undue difficulty in the resultant distillation.

Stream Splitter (ETACSPLIT) ETACSPLIT splits the 28181.37Ib/hr liquid stream S-901 at 117.5°F and 35.5 psi into two separate streams. 79.17% by mass gets diverted to the liquid stream that is returned to pump P-620; the remainder is fed to DC-900.

Stripper

ST -800 (see spec. sheet p . 126) This stripping is designed to remove the water from the system in the bottoms to be sent to a wastewater treatment plant with the objective of purifying it enough to be able to dispose of it. The bottoms stream, WASTE WATER, contains 89.2% by mass of water.

66

The main impurities in this stream are acetic acid (8.5%) and acetone (1.6%). The distillate stream, S-804, primarily contains ethyl acetate and acetone. The stripper was designed using 4 equilibrium stages; the tray efficiency is 34.8%, so the actual number of trays is 12. Since there is no reboiler in this column, there is not a bottoms sump, but there is a 4-ft. disengagement height for the condenser. To that end, this separation column is 28 ft. in height and has a diameter of 1 ft.; both the trays and the column itself are constructed out of stainless steel. The water-rich decanter product stream S-80 1 enters the column at tray 2. Steam is introduced into the stripper at 2161 lb/hr at the bottom tray. The distillate rate is 1194 lb/hr and the operating pressure is 22 psi. The bare module cost of this column is $287,800.

Tanks

T-1 (see spec. sheet p. J 2 7)

Storage tank T -1 is used to hold a one-day supply of acetic acid feed. It holds only this much because our facility is on the site of a major chemical company, so there is no need for us to maintain a large inventory. At steady state, the volumetric flow rate of pure acetic acid feed is 320 ft 31hr, which would imply the need for a 7,680 ft3 holding tank for the reactant. The tank is made from stainless steel to resist corrosion. The bare module cost estimate, from Ulrich, is $115,700.

T-2 (see spec. sheet p. 128) Tank T -2 holds a 12-hour supply of the bottoms product from the acetic acid distillation column, stream S-103. The volumettic flow rate is 402 ft31hr, and the

67

necessary volume for the holding tank is 4824 ft3. The material of construction is stainless steel, and the bare module cost is $52,100.

T-3 (see spec. sheet p. J29) Tank T -3 holds a 12-hour supply of the acetic acid bottoms product from the ethyl acetate distillation column. The volumetric flow rate of this stream is 7.5 ft 31hr, so the required tank volume is 90 ft3. This vessel is made of stainless steel and has a bare module cost of $6,940. Both T -3 and T -2 can be used to store additional acetic acid that will be necessary at start-up, when there are no recycle streams to augment the fresh feed.

T -4 (see spec. sheet p. J3 0)

Tank T -4 is used to hold a fourteen day supply of ethyl acetate product. The volumetric flowrate of the product stream is 21.8 ft3 1hr, so a tank with a volume of7,309 ft3

(207 m 3) is required. This is a stainless steel vessel, and the bare module cost is

$115,700.

T -5 (see spec. s heel p. J31) Holding tank T-5 holds the combined acetaldehyde product from the HAC PRODUCT streams. A fourteen-day inventory of acetaldehyde is required for T -5 . The combined volumetric flow rate is 275 felhr, and the required volume is 92,400 [e. The material of construction is stainless steel because high levels of acetaldehyde can corrode carbon steel. Because of acetaldehyde's low boiling point, there must be cooling facilities to keep the temperature below 60 OF, this is considered when calculating the

68

bare module cost, as the purchase cost was multiphed by a factor of two (in addition to the bare module factor) to account for refrigeration. The purchase cost is $66,860, and the bare module cost of the tank is $601)700.

T-6 (see spec. sheet p. 132) Storage tank T-6 is used to hold the intermediate S-501, before entering the acetaldehyde distillation column HC-500. It would be preferred to have a tank storing the reactor effluent S-206, but its high temperature and large volumetric flow rate because of the large presence of hydrogen and carbon dioxide gas make this impractical. In case of plant stoppages that stream must be flared. The volumetric flow rate of the distillation column feed is 1810 fe!hr, so a tank that can hold a 12-hour supply of this material must have a volume of 21,720 ft3 (615 m 3). This tank must be made out of stainless steel because of the corrosion risk from acetic acid. The bare module cost is $127,300.

T-7 (see spec. sheet p. 133) Tank T -7 holds the bottoms product S-506 from the acetaldehyde distillation column DC-500; this location is chosen because if there is a shutdown in the acetic acid separations section, the acetaldehyde reaction/purification section can still operate. The volumetric flow rate ofS-506 is 1700 ft3/hr, so a 12-hour hold of it will occupy 20,400 fe . This must be made of stainless steel because of the high acetic acid level, and its cost is $115,700.

69

Valve

V-SOl (see spec. sheet p. 134)

The valve V-SOl is used to decrease the pressure of the feed to the acetaldehyde distillation column from 230 psi to 43.5 psi. The flow rate of the stream is l05,380 lblhr. The pressure of this liquid stream is decreased because the acetaldehyde distillation column operates using a condenser pressure of 32 psi.

70

lL

Sl.33HS NOll.VJlilIJ3dS l.INn

ABSORBER Identification Item Item #

Absorber AB-320

Date:

4/9/02 cp

By:

No. Required Principal Function: To separate acetaldehyde from the side products and unreacted acetic acid. Operation: Continuous

Materials handled: Quantity (lblbr) Composition (lblbr) Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

OUTLET STREAMS INLET STREAMS S-305 S-401 S-303 S-304 62,277.9165,870.5019,877 .11 23,469.70 trace 0.02 trace 122.96 trace 28.45 trace 27.13 trace 3l.92 6.47 6,167.54 615 .79 785.89 2,775.68 1,983.88 110.70 126.75 13,552.9312,873.06 45,046.2543,892.99

7,088.02 5,328.15 1,543.27 893.76 898.61 6,792.88 119.04 126.56 33.52 266.36 379.53

159.2 235.0

113 244.7

126.4 234.9

7,088.00 5,205.19 1,514.82 866.63 866.69 63l.81 289.14 918 .35 ] 7.47 946.23 1,532.78 159.4 233.5

Tray Spacing (ft):

34 Average Pressure 2 (psia):

Diameter (ft): Height (ft):

3 Material of Stainless Steel 76 Construction:

Design Data: No. of Trays:

233.5

Comments & Drawings: See process flowsheet pg. 13 and Appendix A p. 177.

72

Compressor Identification

Item

Item #

Compressor CP-410

No. Required

4/8/02 akg

Date:

By:

1

Principal Function: To increase the pressure of the hydrogen feed into the furnace

Operation: Continuous

Materials handled:

Inlet Stream

Quantity (lblhr): Composition (lblhr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF): Pressure (psia):

Design Data:

Net work reqd (hp) Volume (ft\

Utilities:

S-403 20,404.31

Outlet Stream

S-207 20,402.42

7,781.46 5,137.53 1,495.13 855.36 855.42 623 .59 285 .38 906.41 17.24 933.93 1,512.85

7,781.47 5,137 .53 1,495.12 855.34 855.42 621.46 285.40 906.51 17.25 933 .97 1,512.96

152.3 212.7

202.6 262.8

-

385.06 Compressor Speed (rpm) 9335 Material of Stainless 2100 Construction: Steel

Motor driver

Comments and Drawings: See process flowsheet pg . 13 and Appendix A p. 165.

73

Heat Exchanger Specification Sheet -

1 ~c.>rT1P?E1Y:. 2 Location :

---

_._-'" Our Reference:

3 Service of Unit: C-500

4 Item No.: 5 Date:

6 Size 7 Surf/unitteff.)

Your Reference:

Rev No.:

4/3/02

Job No.: ir:J.._. _.~.!lor Shells/unit 2 ft2

69--96 13109.2

8 9 Fluid allocation

-

-_....._.._

.

f!~.i.s!.guantitY-,-Jotal

..

Vapor Un/Out)

13

Liquid

14

Noncondensable

Ib/h

15

.

__._-

21 Molecular wt , NC

749473 6897 42286

749473

749473

101.8

90

105

~ Latent .......•._...heat _-.... ~ _._ JElI~. ~. pre~sLJ.rE:!.(abs~l,!,~) ~

26 Velocity 27 Pressure dro p, allow./calc. 29 Heat exchanged

10530000

30 Transfer rate, Service

86.34

31

46.676 -_ ..

0 .009 43.84

0.186 43.83

0.783

. ..

44.01 0.9302

0.9432

BTU/{Wh~F)

0.008

0 .101

0.356

0.362

BTUllb

187.8

192.7

~i

32

80

ftls

9.8

2.96

2

1.412

[ '

20

0.003 97.6

9.3

psi

Sketch

~

Sizelrating

._-

Out Intermediate

39 in / 40 Tube No. 4378

00 0.75

41 Tube type 42 Shell

10

CS

Tubesheet-stationa~

46 Baffle-crossing

! i

I

oX=n=;.tl i

12/ 150 ANSI 12/ 150 AN~I 6 / 150 ANSI ....... 12/ 150 ANSI 4 / 150 ANSI / 150 ANSI .. Tks-avg 0.065 in Leng!b.. .§. ... Material CS ---..

I

-- . ~- .

Shell cover

in

Pitch 0.9375

ft

I Tube !2attem

in

3..0

-- _._-

_-

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...........

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Type

_ single seg

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Tl:!2 e Bundle .entrance 440 - _.

52 -Gaske . ls - Shell side ._... _ 53 ... Floating head

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p.?? ".".__ .. ._- in 23

.-.................

T~Re

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vert

--

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49 Bypass seal

55 WeighUShell 56 Remarks

0.0625

..

CS

48 Supports-tube

54 ...<:'9.ge requirements

0 .0625

0070

47 Baffle-long

50 Expansion ioint 51 RhoV2-lnlet nozzle

8

CS

45 Floating head cover

I Code 170

-.

1

C$

43 Channel or bonnet

751

180

in

In

37 Connections

Tube Side

- .- ! Code

75/

F

F BTu/(h*ft2*F)

Clean 276.49

.._-_. Shell Side

34 J)~..slg~ temperature r- 35 Numb_~e?!>?es per shell Corrosion allowance

4.987

0.003

MTD corrected

J3TU/h Dirty

.-

.-.

CONSTRUCTION OF ONE SHELL

~ ~2.gnfTesl pressure

0.664

0.6173

..

32

61 . 07~_ _

61.587

44.01

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. ..

28 Fouling resist. (min)

.- -

0.235

0.3206

BTUI(lb*F)

I~_~. f!11.?l.~.!:1.c:!lJctivity__

58

-r

115

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22 Specific heat

57

CW

..

110.55 --.-

F

20 Molecular wt, Vap

44

Tube Side

__

584

F

Dew / Bubble point

18 Density 19 Viscosity

---

ft2

..

16 Temperature (In/Out)

38

2series

6554.6

49767

_._. Ib/h Ib/h ._. 49183 Ib/h _...... -....

17

Surf/shell (eft.)

PERFORMANCE OF ONE UNIT .. Shell Side

10 Fluid name

r11 12

1 ~arallel

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Tube Side

9!oove/ex!2and -.- .- Bundle exit 22

in - - .- - -

- ..-..

.-

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ASME Code Sec VIII Div 1 .-... .32791 Filled with water 56885.6

TEMA class Bundle

..

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...

23728.2

Ib

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Heat Exchanger Specification Sheet 1 Com an 2 Location : ::-:-:---::-_ _ _ _ _ _ _-=----::::-:_ ___________ _ _ __ __ _________

3 _§~ic~.Qf. Unit: 4 Item No .: C-520 51 Date:

Our Reference:

Your Reference:

Rev No.:

61 Size

Job No.:

10--168

in ft2

403.2

71 Surf/unit(eft.)

Type BEM Shells/unit 2

hor

1 parallel

Connected in Surf/shell (eft.)

PERFORMANCE OF ONE UNIT

Shell Side

8 91 Fluid allocation 10 Fluid name !..!.~quantity. Total 12 Vapor (In/Out) 113 liquid____ Noncondensa_~__.__ ___ 14

Ib/h Ib/h Ib/h

2607

Ib/h

54

2series

201.6

ft2

Tube Side

_ '10 c/~ [i/, y/itl( ~ " ""

21775

2661 342 __ 2265

I

__ _ ___.l1?75,

21775

___ __ ______ _ _

I

303 0.108

0.8165 0.258

.....l06.6 ftls psi I

261 Velocity 27 Pressure drop, allow./calc. 281 Fouling resist. (min) 291 Heat exchanged 301 Transfer rate, Service

8 9.98

ft2*h*F/BTU BTu/h Dirty

612890 31.43

2

- -0.89 -

20

0.003 MTD corrected

-

-

-

32.18

1.156 0.003

48.37

-

Clean 40 .9


Shell Side 33 OesignlTest pressure psi 751 I Code 34 Design temperature F 160

311

Sketch

.;g

35 Number passes per shell 36 Corrosion allowance .______ _i!!

I In

37 Connections 38 Size/rating ___ in! 39 40 Tube No. 74

__ _ lOut I Intermediate OD 0.75

41 Tube !}:pe 42 Shell __ ~_S3Q~

ID

43 Channel or bonnet

~ TUb~~h~~t:;~uonarv

__ _

Tube Side 751 I Code _ 90

1

O.Q?'?~

3/ 150 ANSI _ ___?!:1.~.Q_~!'J_~1. 2/ 150 ANSI 2/1 50 ANSI 1/150ANSI I / 150 ANSI Tks-avg 0.065 in Leng~14_ __ _ Material CS in Shell cover Tubesheet-fioating

Baffle-=-crossiniL- SS304

Impingement j)rotection Type

47 Baffle:long

single seg

Seal !}:pe U-bend

Cut(%d)

_______

in •_ _ __

SS304

4~

ft Pitch 0.9375

J_ Tube pattern 30

._

Channel cover

Floating head cover

1 !

____ . .

CS

5?

o!t~

2

_ _ _ ___

OD 10.75

F BTu/(h*ft2*F)

42

vert

Plate on bundle Spacing : dc 21 .25

in

1 Inlet 9.625 in __TYRe,_ _ _ _ __ _ _ __ __

_ _ _ _ __ _ __ _ _________Il,l!J~:t!::l!:>~_s~ ~~_tj()i,rJl. _ _..gr.()'O'':!.~!~.>:P.<:l. ~ .d. _ _ _ __ _ _ _ _ _ _ _ __ _Typ_~___ ,_ _____ .:...:.:.:::..:..:..:=::..::...._ _1 .:...1:..:5:..::5_

52 1Gas~ets - Shell side 53 Floating head

Bundle en_t.r~ nce ..JJL Tube Side

Filled with water

4

IE __A M _c_I~S~s~~~ B _

ASME Code Sec VIII Div 1 1037.4

Buncj!~_~_)(it

1542.7

~~l Remarks

57 58

,,=

Bundle

591.7

Ib/(ft*s2) 1

_ __ _ __ Ib

Heat Exchanger Specification Sheet ~~Q~~a~ny~:

_____________________________________________________________ _____________

2 Location:.... -- --------- -------------------- -------------- - - - - - - 3 Service_. _......_ of Unit: _-=-=c.....:...:=.::::.:...::..:.:..=-'--________________._ Our Reference: _ _ _ _ _ _ _ _ _ _ _ _ .__ _ _ _ _ __ 4 Item No.:

C-610

Your Reference :

~~~~~----~~-..----~~~~~~--------------------------------

5 Date:

Rev No.:

Job No.:

1--=+ -==_ _ _-.-:3:..;7_-_-1:..:2:..:0'_ _ _ ___..:.:in-'--____...:T../..yp"'e=--=B:...:V..:.:M"----"h""o'-r---'CO:.=n"-'n.:;.ec;:.;t=-ed::....:.:.in' --_ __1.:...,~araliel ft2 Shells/unit 1 Surf/shell (eff.) 2494.3 2494.3

1series ft2

PERFORMANCE OF ONE UNIT Shell Side Side 1--=+-=:...=:.::..::.=-="-'- - -- - --------- --+--------=0:.:..:::..:....::=-=-----1-._ _•_ _Tube :"':::'::-=-':0=;=-_. _

_

_

, · je; CW ... ----------+-----~--'-'=-'---------+-------=-.:..::....--.- . -

46,3=-4:...::9.-:.4__ __..__ _......_________._-=-=-=-+_ ____1:....:1..:,7.:...79::.;8=--______t -______.-:.1....:.

_

308.23 270 88 f-'1-=6+-T;:.;emc..:1J::.p~e;:.;r-=a.:.:tu:.:r.e::....>.: (I'-" n/-=O:...::u"'t)'___ _ _._ ______ - ----=-+---=-=-=-=---1--=-'-~.-~--=-"---_+_-:....: 17 Dew / Bubble ~oint 308.23 235.31 18 Density 0.421 51.55 62.241 ..... _... 0.014 0.213 0.781 :~ Yiscosity 37.88 ._._ - 55.12 20 Molecular wt.!. ~,<.lc:.. ~ - - - - - --------.-----+-- ::.:..:.=-=----1 ,

21 Molecul?l:.~.!_'_N.:..;C"____________ __ _-+_ ______+ 22 Specific heat 23 Thermal conductivity

BTUI{lb*F) BTUI(ft*h*F)

0.4139 0.015

-~

____._________+_- - - - - 0.781_L __..:.:1.c: .O. : .OO:. ;_ 7 _-+____-'--____ 0.091

0.352 _ --+_--=--'=c-::_ _

24 Latent he ::::a::..:t_ _ _ ____________--....!B:::..T!..!U~/.!!lb~__-'-4"_84-'--__-"-__....:4!.>5!-"8"_.1'____+-- -_... ___-L-_ __ ___ 25 Inle~pressure _(absolute) psi 87 .023 26 Velocity

_

.

._ __

8.7

ftls

27 Pressure drop ~o_w_.I_ca _ lc_ . _ __ _ ____ --'psc.=iit-_ ----C4_ _-'-____Q}-=8_-i_ __-=2::.::0' --__ 28 Foulinq resist. (min) ft2*h*F/BTU 0.0005 0.003 2c9-::F H.:::; ea:::t-=e:.:.,:xc"'hc.::;a:.:,: n""ge::.:d=--____-=3:.:;:6598300 30 Transfer rate , Service 76.98 31 32

BTU/h Dirty

129.13

CONSTRUCTION OF ONE SHELL Shell Side

MTD corrected Clean 263.63

190.6 2 - - - - - . £ . . . BTUI{h*ft2*F) Sketch

Tube Side

Pls.,.i_ -= 80;:.;/_ _--'-I-=C..::o.:;.de=--f-----'7..::5-'-.1_ _-'I-=C:...:o..::d..::.e-l 33 Desi9nlT~3.!..~u=r..::.e___ _ .__ _ -= _-'F-+-_ _ __3=_7:...:0'--___-t-_ _ _ _....:.1.:;.80-'---_____ 35 Number passes per shell 1 4

li~esign tem~erature

I

I rr

L!

Q .. ~' :".:........o

(P ut ::: t

\..

i

!

h, J~jlnh ~I)J •

~3~6~C:.:::o::.:.rr-= os::::i.:::: on~ al:.:.:lo~w.:.::a::.;n:.::: c"e _r---------i.!l.-------------_I_------------1 37 Connections _I ,, n _____.._. _____..,;"18=1_1,;"":5:..:;0..,;"A..c..N,;,,,,:S'-I_t_-----'1-=.8:.... 1 -'-'15'-'0.-:.A..c.N,;,,,,:S'--1 1 Size/rating 8/'---'...15:...:0:...:A...::N..:.,:S=-I-t-___ _1""8:.<... F38-f-...o::.:::=-::=-"'--___ +-"O'-"u~t______-t--_...__ .......:::. / ...:.,; 15 =.,:0:...,:A ...::N,.:.:S"-'I-j in/ 39 Intermed:::ia::,:t"'-. e -'-____-"6'-'.1....:1""5_0:....:A...::Nc:.S"-'-1-'--____-"-1150 AN St 40 Tube No. 1296 1 ~+_'_~~~~~---0 == D'-=0~ .7~5'-- ~T~k~ s~ ..::c::. vg~-=0~.0~4~9----~i~n~L~e~n~gt~h~ 10 ~____-,rft~P~i ~ tc~ h~0~.9 ~3~7~5'--___ in 1-'-'-t--'-~:....:J..c.:::. M=aterial SS304 Tube pattern 30 41 Tube type __ _ _ _________ _ ________.:..: SS304 10 42 Shell 00 3c_8c'--__--'-in:..:.....___I_..::S"-'h~ e:.:.. l1 ..::. co=-v:...:e:.:..r-----------------..--. - - - - - - --

I

43 Channel or bonnet SS304 Channel cover 44 Tubesheet-stationarv S..:: F~==:=.:=~:::..L--= S.=. 30=-4:.-...------.------_t_T -'-'uo..::bc=e=sh-'-=e.e.~~.~ .g?!!.0.fl-. ___._______ ______ _ _ _ _____________ Impingement protection None 45 Floating head cover TYDe single seg Cut(%d) 46 vert_~~acing: clcl..Q._ _ _ _ __ in 46 Baffle-crossin ~ .. SS304 Inlet 11 in 47 Baffle-Ion _ Seal ty~e _____________________. 48 Supports-tube _ _••__ ~________= U_=·b:;,,;:e:.:..n;.:;;d_ _ _ ________________'Ty2e _ ______..._ ____ _

I

1________ ......._ __ _ _ _ _______T.:..:u::.:b~e:...;-t~u"_b::::es"'-h:.::e:.:::e-'Jtj'o.::. -" in:.:.. t ___ _groovefe."x,~""a:.::nc:: d _______ _ 49 .E3YP?::::ss'-'s""e""a::... ... _ ___________ _ _ -'-T:i2.=..e_____________..____ _......._. ___._______ _ __ _ 50 . ~~!1sion joint

__

51 RhoV2-lnlet nozzle 967 Bundle entrance -_._- - - - - - - _._.._.Bundle.. -- exit ..-- Ib/(ft*s2) Gaskets .. Shell side Tube Side .____ _______ ._._ .._............_ _ ______ 53 Floatin.9.he.a:::,:d"--_ __ _ ______________ _ _ ___.____ _______ ________ ...._ __

~

54 Code requireme!!ts _ _

~. ~E

55 WeighVShell

8955.7

TEMA class

Code Sec VIII Div 1 Filled with water

13282.5

Bundle

B -...... --- ....- -

6385.1

-Ib

56 Remarks 57 f--- -- -- -- - - - - - - -- - - -- - - - ------- ------------------- - ____________ ...... _____ 58

Heat Exchanger Specification Sheet 11 Companl: LocatiOn :

~

3 _~ervice of Unit:

4 Item No.:

Our Reference: Your Reference:

C-800

5 1Date:

Job No. :

Rev No.: 8--192

61 Size

TY2.e BEM

in 112.2

71 Surf/unit(elf.)

hor

~I' Fluid allocation

Shell Side

10 Fluid name 11 1Fluid quantity, Total

ft2

.. . _ .. !~'-I! Ib/h

_. Noncondensable - - - - ---.

C. W

10586

32660

4160 6427

•. j

.1

184.8

0.01

cp

~. _~olecular wt, Vap

BTU/(lb*F~ BTU/(ft*h*F

22 Specific heat 23 Therma.Lconductivity 24 Latent heat

I

psi I

26. Velocity 27 Pressure drop. ,?lIow.lcalc.

ftls_1

50~~~8 __ J.__~~;:24

--

29 I Heat exchanged

97 9980 111.78

397.7 27 38 42

I

3

2.855

0 .( ~

ft2*h*F/BTU

30 I Transfer rate , Service

MTD cc: .rrecled

BTU/h Dirty

112.22

Clean 438.22


31

Sketch

Shell Side

32 331 OesignlTest ,,,on pressur~ '''J J U'~

si

34 Design temperature

F

Tube Side

7?i ___ LQ{)de

75/

250

~~ ~~~~~~:

I'" lin

Size/rating

lOut

in/

~~

4

?

_ __.9,Q.§.?;,.:".5

in

..

37 Connections

/ Code 180

35 Number passes per shell 36 Corrosion allowance

t

--1

·· . ·t~~~-~~~:

Ilntermediale.J__ _ _/_1.5.QAr:i?:.;.I-L I _ _ _ _/'--.:..: 15"-'0:...:Ac..:N :...:.:::c S'-1L..._ _ __

~.9 Tube No. 36

._ 00 0.75 _

41 Tube t y p e .

Tks-avg _ ____ _...._

61 .864 0.561

60.93

391.5

psi


120

0.36.----.-- 0.6136 - 0.01 0.076

BTUllb

25 Inlet pressure (absolute)

90

183.65

62.27

211'0
32660

I

181.7

1QA Q FI Ib/ft3 1__ -- 0.238 - -""-_._

19 Viscosity

32660

'

F

17 ~~J3_ubble point ______ ..____ __._ _ _ 18 Densi

I

10586

Ib/h

16 Tem . erature (In/Out)

Tube Side

S- ~a.t Ib/h

f-=--I----,-",,,-=->.:.n/Out)

381 ] ~.

1 series

112.2

Surflshell (elf.)


8

14 1 15

1 garallel

Connected in

Shell s/unit 1

ft2

0 .065_

_

.!!!Length 16

ft

Male..r:ial .C:? __..

_ _ __

Pitch 0.9375

_

_

in

1 Tube pattern 30

E~ll_

SS304

10

~ g,~Cl.Qnel

or bonnet

CS

+-C,-,h-,-,acc..nC'ncoe.;".1c.=..o' - --v...:e"-r_ _ _ __ __ _ _ ________

SS304

+-T_u-'-b"'e'-'s'-hco e-= e-' t-f1_0o.:a;;.:u;.c. ·n""_ _ __ __ __ __ _ ___ 1

00 8.625

..:cin '-!.-_+--'S:o:h-'-'e'-"II--'c~ o:..: v::::.er:...._ __ __ _ _ _ _ _ _ _

_ __ 1

~ .I.ubesheet-stationary -4-~

.Floating head cover

.-4-6..l?alfle-crossing

.__

__ ~? 3 04

..... Typ.~ 2i.Qgle seg

47§.Cl!f!~-lon g

vert

Plate on bundle Spacing: d c 5. 5 11.5

in in

Type Tube-tll~_e~~E'::.~tj
1672 . ..

Bundle entran ce __ .2J].

152 Gaskets· Shell side

_ _ __. _~l:!...1l9.!~€!.~t_J..2_ _ _ _Jb/(ft*s2)

Tube Side

Floating head

54 1Code requirements 551 WeighUShell

ASME Code Sec VIII Oiv 1 777.9

Filled with water

156 1 Remarks 57 58

1 '1

a

41

[Inlet

U-bend

49 By~ass seal 50 Expansion joint

153

Cut(%d)

Seal type

~? Supports-tube

51 RhoV2·lnlet nozzle

IIl]J2ingemenl protection

TEMA class 1147.6

Bundle

366.2

B Ib

Heat Exchanger Specification Sheet

__.._._ ---_

1 Company: 2 Location: r ............. __ .. __ .of Unit: ---3.. Service 4 Item No.:

--_.

- - - -

5 Date: 6 Size 7 Surf/unit(eff.)

-----

C-810

Our Reference: Your Reference: Job No.:

----

Rev No.: 8 --120

-

Type BEM Shells/unit 1

in ft2

77.6

Connected in

hor

1

Ib/h Ib/h Ib/h

1714

F F Ib/ft3 cp

174 .5 170.2 0.185 0.042

BTU/(lb"F) BTU/(ft*h"F) BTU/lb psi ftls psi ft2*h*F/BTU BTu/h Dirty

0.3426 0.01 246.2

Liquid Noncondensable

15 16 Temperature (In/Out) 17 Dew / Bubble Q.oint 18 Density 19 Viscosity 20 MQIEi..~!ar wt, Va ~ ~J Molecular wt, NC 22 Specific heat ._ - - - --_.._._ .. _.. 23 Thermal conductivity

~ ~~ ntheat

25 Inlet pressure (absolute) 26 ~~L~ --_. 27 Pressure drop, allow./calc. 1 - - - 28 Fouling resist. (min) 428730 29 Heat exchang~_d 88.15 30 Transfer rate, Service

in / Tube No. 40 Tube type

14289

1714

14289

14289

-- - 167.6

.

49.348 - _ .". 0.261

0.567 1 0.099 22 9.66

2

._.....

90

120

62.224 0.762

61.864 0.561

1.0006

0.9998

247.9

~Q~~~~ I ~~~:==

.

...._--_.. _--_ ... _ -- --_._-- _......._--_80

2.76 0.363

15

0.003 MTD corrected ._-_._-_ .. _... _....• Clean 245.66

95.04 CONSTRUCTION OF ONE SHELL 31 SheIlSid~ __ '--__ I'=!Q~..§lcli!__ _ 32 psi 751 I Code 75i ! Code . ~~. ~g nlTest pressure 180 240 34 Design temperature F 4 1 35 Number ~ assesp_er shell Corrosion allowance Connections Size/ratinq

ft2

CW

r--

1714 - - - ---

Ib/h

1series

77.6 Tube Side

S-!/ll';

J1. 1-- VapQlj.ln/Outl.

36 37 38 39 40 41

~arallel

Surf/shell (eff.)

PERFORMANCE OF ONE UNIT Shell Side

8 9 Fluid allocation 10 Fluid name 11 Fluid quantiY. Total 13 14

.... _ - - - --

1.206

_.

0.003 62.71

F BTu/(h*ft2*F)

Sketch

• -;==t]D . .

f

, I

I

in In Out Intermediate 0.75 ....... ,-_. __aD ...• _-_.._

2/150 ANSI 2/150 ANSI / 150 ANSI / 150 ANSI 0.049 in Length 10 Material SS304 Shell cover in Channel cover Tubesheet-floating

3/ 150 ANSI 1/ 150ANSI Tks-avg

-- -

ft Pitch 0.9375 30

in

I Tube pattem

10 OD 8.625 .~ ~~~_$_3.94 or bonnet 43 .Channel SS304 ..... .. .. _._ ....... _.. ---.. 44 _::Ll! \) ~~~.~.t-stationary SS304 ---- -------_...._-_... Impingement protection Plate on bundle 45 Floating head CO,(.!'!f -. .. Type vert single seg S~acing: C/C 25.625 in Cut(%d) 41 46 Baffle-crossin ~ ~ §}.94 in Inlet 9.5 47 Baffle-long Seal ty~e .. . I -. _____.____. ________ ..Type 48 Supports-tube .. ._U-bend ....... _..... ......... ._._ .. _... .. .... 49 Bypass sei!.!._ __._..____._____..._._ _ Iy\)E!::tLJtJE!.~.tl.E!.E:)_tj.~ _ gr9
,

_

_

-

.~-.------. --. -

Heat Exchanger Specification Sheet 1 Company: 2 Location: --.3 Service of Unit: C-900 Item No.: c--- Rev No.: 5 Date:

-±

Size ....-- -~ ----_

"'''" . _,.

__ .___

Our Reference: Your Reference: Job No.:

12--168

in 275.2

7 Surf/unit(eff.)

8 9 Fluid allocation 10 Fluid name 11 Fluidquantitv, Total ~ _Vapor (In/Out) 13 Liquid Noncondensable 14

-

ft2

_

·__ ·_·_··___ ___M_.____ ··__·

. ----.-.- - - ~ . - -. - -.---

_._-_.-

- "- _ ....

__

Type BEM hor Connected in 1 parallel 1series -. .. _.,------ Surf/shell (eff.) Shells/unit 1 275.2 ft2 PERFORMANCE OF ONE UNIT Shell Side Tube Side .. _ .-._----- Ib/h Ib/h Ib/h Ib/h

15 16 Temperature (In~Out) Dew / Bubble point 17

F F Iblft3

,.:L~ ~J2§Q~!Y.

:) - 7<,.\

cw

24205

97030

I

_... _-

11501 12704

24205

97030

97030

215 215 0.225 0.071 56.19

183.9 210.56 51.137 0.266 60.08

90

120

62.224 0.762

61.862 0.561

-

cQ ..1~ '{iscosity 20 Molecular wi, Va~ ______ ... 21 Molecular wi, NC_. 0.3434 0.5658 22 §p.ecific heat 1.0096 0.9998 BTlJ£{lb*F) 1 0.352 BTUt(ft*h*F) 0.364 23 Thermal conductivity ._. _ .. OL. 24 Latent heat BTUflb 25 Inlet pressure (absolutel. psi 80 --_ .. _" - - - , ,25 43.03 26 Velocity 4.1 ftls _. -'1 . ~~8___ ._ _15 27 Pressure drop, allow./calc. psi 2 ._---._ I 1.634 0.003 28 Fouling resist. (mini ft2*h*F/BTU 0.003 2911400 MTD corrected 103.64 29 Heat exchanged BTUth .___ ..L 102.09 Clean 347.79 Dirty 105.21 30 Transfer rate , Service BTUl{h*ft2*F) CONSTRUCTION OF ONE SHELL 31 Sketch Shell Side Tube Side 32 --_ .. psi 751 I Code 33 ~gnlTestpressure 75L_ _ ~Qg~ . t ! 280 180 34 Design temperature F rr 11 1 -2 - -. f ! ~ ~_mber passes per shell in 0.0625 36 Corrosion allowance In 6/ 150ANSI 6/150 ANSI 37 Connections 3/150 ANSI 6 / 150 ANSI 38 Size/ratinL - - ._ ' Out Intermediate . /150 ANSI / 150ANSI 39 in! 00 0.75 ft Pitch 0.9375 in Length 14 40 Tube No. 101 Tks~ 0.065 in Material CS I Tube pattern 30 ~ _T_~_t?~_!Y.P.~. 10 00 12.75 Shell cover 42 Shell SS304 in Channel cover 43 Channel or bonn.§.L__ Q§____ _. -- - " - ' -""" 44 Tubesheet-statio~ _.~_§~.2.~,. Tubesheet-floatin~L _ Impinqement protection Plate on bundle .. _ .__._ . .. _r~ rE~Q.9~·n.R)l~Cl~ _c;over SS304 vert inl Cut(%d) 43 S29cin.9: clc 13 . __IY~__ _?l~gle seg -'±§. !3affle-c~~~?ing

_~~~1.~

"'

--C I

©tI; 4J---aL-~

__

~ ~Cl.!f~:!
50 _~.~p.Clrl~~()rl19i nt 51 ._RhoV2-lnlet ........._... ..-.... _ -_nozzle .. - 52 Gaskets - Shell sig.e.

____ .m. ".

~~Uype

U-bend

Type

--.- Tube-tubesheet joint

-

Ilnle!_ 14

groove/e~_~_

._._l)~

2596

Bundle entrance 640 Tube Side

.TI. r---._

_ ._£JQ.a_t:.rlg head 54 Code requi!~f'!:I.~!1Js______~§ME Code Sec VIII Div 1 1434.1 Filled with water 2197.3 55 WeiqhVShel1 Remarks 56 -_._ .. __ .... _._ . 57 58

1'1

__

.

Bundle exit 32 ......

-- -

inl

_

..

TEMA class B Bundle 827.7

-

Ib/(ft*s2) I

'--1 Ib I

- .•..---

Heat Exchanger Specification Sheet 1 Company:

-.-

2 Location: 3 Service of Unit:

•...

C-910

4 Item No.:

Rev No.:

5 Date: 6 Size 7 Surf/unit(eff.)

Type BEM

in 473

14

-

F F Ib/ft3 cp

-- ...

Tube Side ........

BTU/(lb*F)

16983

16983

181.6 175.4

175

90

120

0.203 0.091

51.497

62.224

0.255

0.762

61.864 0.561

0.3126 0.009

BTUJ(ft*h*F)

28 Fouling resist. (min) 29 Heat exchanged 30 Transfer rate, Service

.

15.59

157.1 16

ftls

9.9

35 Number passes per shell 36 Corrosion allowance In 37 Connections Out Size/rating 38 --- ._-_._ in/ .... _.. _. __ . Tube No. 410 40 -.------_._- 41 Tube type SS304 42 Shell

ID

50 Expansion joint 51 RhoV2-lnlet nozzle 52 Gaskets - Shell side

751

ICode 1

8 0.0625

BTUJ(h*ft2*F)

e

?

i

!

!

~

..

,

'

2/150 ANSI 2/150ANSI /150 ANSI ft Pitch 0.9375 Tube pattern 30

in

I .. -

--- -

Channel cover Tub~~heet-floating Impinqem~PE()t~ction

_single seg Seal type

Cut(%d}

43

-~ - .

vert

Plate on bundle Spacing: dc 30

I

U-bend

Inlet

__. _ -in in

.

20.25

--

lYJ:>e__. _.gr()ove/~_x"pand

Tube-tubesheet joint Type Bundle entrance 99 Tube Side

----.. _-,...... _.

.~ . -- - .

Bundle exit 36 .. - .. _--_ ...... ...

Floating head

54 Code requirements 55 Weight/Shell

_....E...

69.13

0.065 in Length 6 Material CS Shell cover in

Type

757

0.22

0.003

ICode 180

CS 1-- 44 Tubesheet-.~tationa£l.. SS304 __. 1-._. 45 Floating head cover _

48 Supports-tube 49 Bypass seal

..___J

Sketch

250

Channel 43 -_.. _--or bonnet

SS304

15

Tube Side

1/150 ANSI

OD 24

----

80 0.71

Clean 139.86

72.57

6/150 ANSI 6/150 ANSI Tks-avg

_._-_ ... _

0.315

in

Intermediate OD 0.75

~~

751

F

0.9998 0.364

-----_.... _-_.

0.003 MTD corrected

CONSTRUCTION OF ONE SHELL Shell Side psi

.. ..

5

psi

1.0006 .__ .. 0.352

0.074

psi

ft2*h*F/BTU BTu/h Dirty

509570

0.505

..

156

BTUlib

26 Velocity 27 Pressure drop, allow.lcalc.

31

5634 3129

..

24 Latent heat 25 Inlet pressure (absolute)

32 33 DesiqnlTestEessure 34 Design temp_erature

8763

- - -

21 Molecular wt, NC 22 Specific heat 23 Thermal conductivity

58

ft2

16983

Ib/h Ib/h

15

57

1series ._--_._ --

473

8763

Ib/h

16 Temperature (In~Q.l!!) 17 Dew / Bubble J!9J.rlL Density 18 ._--.- . . - - . 19 Viscosity 20 Molecular wt, Vap

56 Remarks

1 parallel

C. W

Noncondensable

53

Connected in Surf/shell (eff.)

Ib/h

Vapor (In/OutL-.._.. Liquid

46 Baffle-crossing 47 Baffle-long

hor

Shells/unit 1

ft2


11 Fluid quanti!!', To!?1 13 -_.

.. .....

Job No.:

23--72

8 9 Fluid allocation 10 Fluid name 12

_

Our Reference: ---_.. Your Reference:

Ib/(ft*s21

_-_. .".-,--- _ ..

ASME Code Sec VIII Div 1 2571.3 .

_----.

Filled with water

TEMA class 4020.3

Bundle ..

B

-~,, -

..-

1640.9

Ib

__ .. _

-- ..

.

---"

DECANTER Identification

Item

Decanter

Date:

Item #

DE-nO

By:

No. Required

4/9/02 akg

1

Principal Function: Separating out all of the water from the ethyl acetate

Operation: Continuous Materials handled:

Inlet Stream

Quantity (lbmollhr): Composition (lbmollhr): Hydrogen Carbon Dioxide Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

Outlet Streams

I

I

S-704 36,555.16

S-801 8,295.16

S-901 439.28

< 0.001 trace

trace 0 3.63 439.38 803.75 55.58 6,208 .52 784.29

trace 0 3.16 229.99 174.35 2.39 29.39 trace

I

25.83 2,463.10 22,576.48 195.55 8,418.79 2,875.41

I

I

I

I

I

Temperature (oF): Pressure (psia):

113 36.0

Diameter (ft): Volume (ft\ Heat Duty (MMBtulhr):

Design Data:

117.5 35.5

167.6 22.0

Stainless Steel 14.5 Material of 12165.78 Constmction: 0.00288

Comments and Drawings: See process flowsheet pg . 15 and Appendix A p. 179. -

81

Distillation Column

Identification Item Item #

Distillation Column DC-500

No. Required

4/1/02 cp

Date: By:

1

Principal Function: Separating the Acetaldehyde Operation: Continuous

Materials handled: S-501a Quantity (lb/hr): 105,379.58 Composition (lblhr): Hydrogen 0.04 220.69 Carbon Dioxide Methane 50.38 Ethylene 50.00 Ethane 54.41 Acetaldehyde 12,843.29 Acetone 1,162.71 Ethyl Acetate 2,765.36 Ethanol 865.08 Water 19,808.00 Acetic Acid 67,559.63

Temperature (oF): Pressure (psi): Design Data: No. of Trays: Feed Tray:

Tray Spacing (ft): Diameter (ft): Height eft): UtiJities:

S-504 2,885.40

S-506 92,139.53

trace

0.04 215.16 47.99 41.93 49.63 2,527.19 trace trace trace 0.19 trace

trace trace trace trace trace 9.57 1,162.71 4,106.58 163.78 20,051.42 66,645.46

101.8 32

262.7 37.8

5.53 2.39 8.07 4.78 10,306.52 trace trace trace 27.372 trace

121.8 43.5 71 28 2 4.5 156

S-502 10,354.66

101.8 32

Average Pressure (psia): 32 Molar Reflux Ratio: 2.4 Material of Construction: Stainless Steel

Condenser (C-500) and Reboiler (R-500)

Comments and Drawings: See process flowsheet pg. 14 and Appendix A p. 165

82

Identification

CONDENSER COLUMN Item Condenser column Item # DC-510 No. Required 1

Date: By:

4/9/02 cp

Principal Function:

Separates the Acetaldehyde from the offgas outlet stream from the main acetaldehyde column

Operation:

Continuous

Materials handled:

Outlet Streams S-503

Inlet Stream

S-504 Quantity (lbmol/hr): Composition (Ibmol/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

62,277.57

Design Data:

Utilities: ~

-

1.30 0.54 1.88 1.09 2,455.29 trace

3.456

-

0.041 213.86 47.45 40.05 48.54 71.90 trace

< 0.001

98.3 30.1

8 Average Pressure (psia): 8 Material of Construction : Stainless 2 Steel 1.5 Molar Reflux Ratio: 53.1

Condenser (C-520) with a Refrigeration unit (RF-520) -

421.84

trace

101.80 32

No. of Trays: Feed Tray: Tray Spacing (ft): Diameter (ft): Volume (ft3):

S-505

2,463.56

trace trace trace trace trace 4.87 785 .95 2,775.97 110.71 13,553.36 45,046 .71


I

-

-

83

-

10 28

28

3.79

Distillation Column Identification

Item

Distillation Column

Date:

Item # No. Required

DC-610

By:

4/9/02 cp

1

Principal Function:

Purifying acetic acid by utilizing ethyl acetate-water azeotrope

Operation:

Continuous

Materials handled:

S-602

Quantity (Ib/hr): Composition (Ib/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF): Pressure (psia):

S-603

29,861.62

22,326.31

20,743.76


< 0.001 trace 0 0 0 17.83 1,598.79 17,200.99 110.58 1,746.22 1,651.91

trace trace 0 0 0 trace 0.006 0.016 < 0.001 366.13 20,377.61

117.9 98

263.2 100

Design Data:

No. of Trays : Feed Tray: Ethyl Acetate Tray: Tray Spacing (ft): Diameter (ft): Height (ft):

Utilities:


30 17 2 2 10.5 74

84

S-103

369.9 98.6

Average Pressure (psia): Molar Reflux Ratio: Material of Construction:

S-801 8,295.16 trace 0 0 0 0 3.63 439 .38 803 .75 55 .58 6,208.52 784.29 117.5 35.5

95 2.5 Stainless Steel

DISTILLA TION COLUMN Identification

Item Item # No . Required

Principal Function:

Waste Acetone separation column

Operation:

Continuous

Distillation Column DC-8l0 1

Date: By:

4/9/02 cp

S-804

S-805

S-707

Quantity (lb/hr): Composition (lb/hr): Hydrogen Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

1,194.31

439.28

755.2

trace

trace


18l.7 25

Materials handled:

trace 3.31

3.16

0.17

293.44

229.99

63 .50

784.24

174.35

610.00

5.13

2.39

2.74

29 .39

77 .92

107.31 0.88

trace

167.6 22

Design Data:

No. of Trays: Feed Tray: Tray Spacing (ft): Diameter (ft): Height (ft):

Utilities:


19 14 2 1.5 52

0.88

18l.9 25

A verage Pressure (psia): 22 Molar Reflux Ratio: 4 Material of Construction Stainless Steel

-

85

--"

DISTILLATION COLUMN Identification

Item Item # No. Required

Principal Function:

Water 1 Acetic Acid - Ethyl Acetate separation column

Operation:

Continuous

Distillation Column DC-900 1

Materials handled: Quantity (lblhr): Composition (lb/hr): Hydrogen Carbon Dioxide Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

S-901

S-902

5,933.43

1,577.33

< 0.001

trace trace

trace 4 .66


< 0.001

4/1/02 cp

S-706 4,356.10 < 0.001

trace 4.66

424.90

0.89

424.01

4,571.37

1,136.39

3,434.98

29.39

0.24

29.15

464.07

1.79

462.28

439 .05

438.03

1.02

117.5 35

221 28

Design Data:


Utilities:


20 10 2 2 54.5

86

Date: By:

181.9 25

Average Pressure (psia): 25 Molar Reflux Ratio: 1.8 Material of Construction Stainless Steel

DISTILLATION COLUMN Identification


Distillation Column DC-910 1

Principal Function:

Ethyl Acetate separation column

411102 cp

Date: By:

I

Continuous

Operation:

I

I

Materials handled:

Quantity (lblhr): Composition (lb/hr): Hydrogen Carbon Dioxide Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

S-902

S-903

S-102

1,577.33

1,139.31

438.03

trace trace

0 0

0 0

< 0.001


< 0.001

trace

0.89

1,136.39

1,134.92

0.24

0.24

1.79

1.79

0.001

438.03

1.48

436.55

221 28

175 16


Utilities:

Condenser (C-91 0) and Reboiler (R-91 0)

-

I I

0.89

Design Data:

-

trace

I

1.47 < 0.001

I

263.2 20.1

45 Average Pressure (psia): 16 26 Molar Reflux Ratio: 1.8 2 Material of Construction Stainless Steel 3 104

-

- - -

87

- -

-

.......

FIRED HEATER Identification Item

Item #

Furnace F-230

No. Required Principal Function: conditions

4/8/02

Date:

akg

By:

1

To increase the temperature of the reactant streams to optimum reaction

Operation: Continuous

Materials handled:

Quantity (lb/hr): Composition (lblhr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF): Pressure (psia): Design Data:

Heat Duty (MMBTU/hr)

Inlet Streams

S-203 42,57l.91

trace trace

Outlet Stream

S-204 20,402.42

S-205 62,974.33

trace 0.006 1.49 0.001 365.11 42,205.31

7,781.47 5,137.53 1,495.12 855.34 855.42 621.46 285.40 906.51 17.25 933.97 1,512.96

7,781.47 5,137.53 1,495.12 855.34 855.42 621.46 285.40 908.00 17.25 1,299.08 43,718.26

464.7 255 .0

477.6 254.8

599 252

15.29 Average Pressure (psia): 253 Material of Construction: Stainless Steel

Comments and Drawings: See process flowsheet pg. 13 and Appendix A p. 180.

88

FLASH VESSEL Identification Item

Item #

4/9102 cp

Flash Vessel Date: FV-310 By:

No. Required

1

Principal Function: Separates the S-302 stream into a vapor and liquid Operation: Continuous

Materials handled:

Inlet Stream

S-302 Quantity (lblhr): Composition (Iblhr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF): Pressure (psia):

Outlet Streams S-303

-

S-306 39,509.77 23,469.70

62,979.67

7,088.04

7,088 .02

5,425.88

5,328 .15

1,565.20

1,543.27

916 .63

893.76

921.10

898.61

13,471 .78

6,792 .88

665.76

119.04

907.31

126.56

771 .84

33.52

7,201 .08

266.36

24,045.05

379.53

0.02 97.73 21.93 22.87 22.49 6,677.43 546.90 78l.38 738.33 6,935.17 23,665.52

113

113 244.7

113 244.7

244.7

I

Design Data:

Vapor Fraction: Diameter (ft): Volume([t'"'3):

0.8 Material of Construction: Stainless Steel 17 Heat Duty (MMBtulhr): 20.3 16,860

Drawings and Comments: See flowsheet p. 13 and Appendix A p. 182. -

-

89

~ - ----.-

Heat Exchanger Specification Sheet 1~9rnJl~an:.o.Y,-,-:_ __

2 Locauon :

_ _ _ _ __ __ __._ __ _ _ _ _ __ __ __ _ ______ ____ ___._

- --

- - - - - - - - - - - - - - - - - - - - - _._ - - - - Our Reference: - - -=-=::.....:... = .::.:.=.="---- - - - - - - - - - - - - -._._ - - -

3 Service of Unit:

HX-200

4 Item No .:

Your Reference:

Rev No.:

5 Date:

Job No.:

47 --240

6 Size

Type BEM

in

7 Surf/unit{eff.)

8343.1

vert

Connected in

Shells/unit 1

ft2

8

1 parallel

Surf/shell (eff.)

1 series

8343.1

tt2


Fluid allocation 9 --==-=:.::..::;::..::..::.:..:.....f-=+ _ 10 Fluid name 1--'

---

-

Shell Side - + - ----=.:..;.::.:c....::;=.::;-

---

-

_ __ __ _ _ ___--+-_ _ _. . . .:<:...;) -_20 · b

=-_ _ __ 11 Fluid quantity. Total

12

_

Tube Side -..----'--'=-=-==-=--

_+

_______._--=I.=.b/'-'..h+-_ _ _--=:c2Q; g L_____l -_

-"-_ __ _ _ __ __ _-"I b/h Vapo~_ln/Qut)

20322

- -

,, - .261

_

-=27:..r6:..::5:.::2e-_

_

_

-.-

20322

3733 --27652 23919 -,~----+-~~~-~-~~~

Liquid

13 ~+-~~~--------------~I~b/~h _ _ _ __

14 Noncondensable _ __ _ ___ __ ---'-''lb''''/h'_'+_-.--- - -_ t _ - - --_t_ l--"-'-i_--'-'-'''-====~ .- - 15

241.9 16 Temperature (In/Out) ~+__'_'=:J"--e.:.;=c:::..l"-"-'::.=L---------------'-F+_-~55"-'6"".9~--I- -~~-+--..::..:....:..:= - 17 Dew / Bubble point F ~

0.406=--__+ Density_ __ _ __ __ _ _ _ _ _~lb~/~tt=_3~-~~-_+-~~ 0.294

19 Viscosity

0.017

cp

~2c:c0-t-'-'-Mc:cO-,-,le",c.=. ul:.:: a.;.... r "'-'-". wt.-'-'V a-'p_ ___.. .___ _ _ __

_ _ _ _--t_ _ _ _ ___t_-

~2c.:. 1-t-'-'-Mc:co-'-'le'-=c.=. ul:.:: a.;...."'-'-". r wt . _--=~ N C __ _._..__ . _ __ ____

22 Specific heat

0.013

+-_ _____t_.I

_ _

BTUI(lb'F)

0.7755

........

-

-.-

...

463.45

58_042

1.925

0.375

0.015

---

--

464.7

~-.

0.7328

0.5679

0.4608

0 .073 0.085 _-+_ - -0'.02 0.089 23 I~ermal conductivity_ _ _ _ _ _---=B=-T:....:U""/->.:(tt.=..·..:..:h'-'·FC..l=)+ -_ -===_-+_ -=-:..::..:.-=---_+_ _ -=-:"::= = .... _-- 182.3 141 .5 ..... 24 Latent heat _.... _ __ __ _ _ _ --=B=-T-'--U::.:/c.:..:lb=-t-_ _ _ _--<~----+---"-==~-----'-_'_"_'-'-"

I

25 ~~p!essure (absolute)

2si

250.915

_

263

_.. _._--

___ ._ _ _ _ _--'.ftI=-s=-t-_ __ _ _9.::..:.r0..:..8_ _ __ _I_ _ _ _ _....:..;...~ 0.14 __ __ _

26 Velocity

27 Pressure drop . allow.lcal<;:..... _.... __ _

_ _ __


_ _<=_ p~si=-t __ _ =--_--'_--=2"-' 5 .0:..::83 "'_ _ t--

ft2'h'F/BTU

31

10.11

Dirty

10.8

BTU/(h·ft2'FJ Sketch

Shell Side

33 DesignlTest pressure ..

psi

260/

. _ _T:....:u:.::b..::.e...=S:..:.:id:..:e:...-._

/ Code

280/

/ Code

-+-___-=5~Q. __ _ _

62..:..0_ __

F

34 ..!?esign temperature

._-----L

51.03

Clean 11.61


32

0.138

0.003

=2.:::.9FH :..:.e"-'a::..:t-"e:.:.:xcha:.:.n=qled "'.::: :::..-_ __-"3 4 ::..:0~o5:..:1.=.2...:..4_ _ __.__ .J~I:::c/h,-U,-,_ _ _ _.:.:. MTD corrected 30 Transfer rate . Service

I

8 -=-

0 .003

35.!':J.LJmber passes per s~'_=_ eII _ __ ___t_----L---+_-----' 1. -~ 36 Corrosion allowance --'i"'nt----------... _._.-t-_ _ _ _ _ _ _-1 8/300 AN§L.t---_

_

f-"'-"'+-...::=:.::::..:.:=-"'-_ _ ~=..:..---+----=.:8/ -'3--'0:...:0-AN---'S"-I-t- . f-"'-"'-l-_ _""-"-___ _ _--'-.:..:..:..:c="'-==........L_ ._ _....:/_ 3 ::.;;0.0 ANSI

--'3::..:,/....::3::::.0-"-0.:...:A::...:N=-S,-I 3 / 300 ANSI / 30Q1\NSI. . __

_ _ _.._

~:.t_:_=~~~'-.:.....---=~.:.:....:::--T.!...!k.!::s:..:: -a::..!v;;L. g ....:0::.;..0~-~='----i:!.Cn~L~e::!.n~g~th:....=.2c~0 49 __ ..__.._ _ . _ tt

r

OD 48

,~=

_ in

Material SS304 .. Tube pattern. ..:::.=-30 _ _ _ 1 Shell co'-"v.:;:: er:..........._ __ _ __ .._... .... _ _ __ ____ in

_ _ ________+_-"C'"'-h::::nn a.:..::..::e::..:I=cov.e:.:... .c: r - --

- -- - --

- - - - -- - -.. . ____ _ __.. ___

.= ==-'--..:....:.-"-_ __ _ _ _ __ _-j----'Tu :::.:b::..:e~s::..: h=-ee=..:t=~_<:J.Cl!i!1g r---:-o:+--=~L:..:.:='-'=...:..::.:

_ __

Pitch 0 .9375

_ _ _________ __...L.:I.:..:m.:r:..:.:piin"g;<=e.:..:m.:.::e::..:n.:..tr::pr-=o..:ote~cc=tio!1

None

._______

_ _~t..= Type'___=s::..:.ln:.;;gc..: le:...:s::..:e:;;g'___...::C:..:u'""t(...:.od °i<::..::.L)_.::.25 =___ J:!.()f__§pacing: clc 9, ? ._ _

f-'-'--r=.::.:..::.:::....::= '--_ _ _ __ _ _ _ _---'S:..:e:.::a::..1:.l.ty.r:.pe=___ _ .._ __ _ __ _._ 1-'4-=8+-"'S~ up r::.=::.:.. p,0 rt;.:: s-'ub -t=::..:e"--_ __

49 ..~..1'P.ilss seal

_ ._ _ _ ---=::....::.en U -b= c.:.:d=___ _ _____ __

891

_

_ _ .. .._._ __

F'loati!1_9...b.~_~...._.______

54 Code !eqlJ!!~'I!.~~._ .__ 55 WeiqhUShell

- - - - -- - _ _

_ __

_

__ __ __ _.-=B~~d.le_. e .>.
Tube Side

......;..:;;..;;;..::.-.::..:.=__ _ _

Filled with water ..

- ......

_ __ ._ _ __ _

_

_

46721.4

Ib/(ft*s2) _ __

_

.._

-

-

_....____

Ib

23819.6

_ - - - - - - ----- - - - -- _._-

_ _._____ .............- - - -- --

_

..__

_ _ _ __ T :_:E"'M"'-'-'A:....:c:.:.: la:::s::;:s_.:: B_ _.._ ___ __ Bundle

_

_ __

_ __ __ _ _ __ ._ _ _ _ __ ____ __ _ __ _ __

ASME Code Sec VIII Div 1._ _ __

32081.7

_

. _.________._

Bundle entrance 830

52 Gaskets - Shell side ...................... .........._...... ......::c.=;.;...=.---'-'_ _ __ _ __ _ _ _._....._

571-._ ____ 58

___--"T.LJy~~__ _._

Type

r?.1 RhoV2-lnlet nozzle

~r-Remarks

in

_ llnlet_..11:l:Q§~ _ _Ln

_ _ _ _ _ __ _ _ _ _ __ ~Tu =::..;:....tuc= b e -;.:: b.=. es=hc.;:..:: e e:.:..tL:joint "'""'_ _---'g<.:....::roQy.!'!le~p~ . __ . __

50 Expansion jOint

53

_

-

- _

...

_---

- -- - - - -- -- --- - -- ... "_

_

_

I

Heat Exchanger Specification Sheet .:L 2 3 4

_Company: Location: Our Reference: Service of Unit: HX-210 Your Reference: Item No.: Job No.: Rev No.: 51 Date: 58--120 in Type BEM hor Connected in 6 Size 19261.5 ft2 Shells/unit 3 Surflshell (eft.) 7 Surf/unit eft. PERFORMANCE OF ONE UNIT 8 9 Fluid allocatio~ "'v~..v" Shell Side )-1~u. 10 Ib/h 41237 11 Ib/h 41237 41237 12 13 Nonconde~c~hlo 14 V' 'VV'

I

.~

VV'.~__

1" 16 TemR~@_~re (In/Out) 17 _Dew I By'p_ble point 18 Densi _ ____ !Q. Viscosi

556.8

280.1

.___ __._.___... _.___.__._._ _ _!2!~-0.293 _ _ .._ _ _ ____ .c;p.. 0.017

0.405 0.013

BTU/(lb·F~ BTU/(ft*h*F BTUllb

24 Latent heat

- -

Tube Side

:)-107 20402 20402

20402

I

202.6

475.51

--._-= E-

20 Molecular w1, Vap 211 Molecular w1. NC 22 S ecific heat

ft2

b:-; /h~I===='±1----~---==+===~~= F F

f}_ Thermal co.Q.ductivity

3series

==I~:h!1===il ------t--=-==~== -+1- - - - +------+-----+-----

._ _ _ _ _ _

- - - - -.

1 parallel 6420.5

0.7339 0.073

0.7766 0.09

I I

25 8.

f2ll!,-et pressure (absolute) 26 Veloci 27 Pressure drop. allow.lcalc.

I

0.386 psi 5 3.16 8 281 Fouling resist. (min) ft2*h*F/BTU 0.003 0.003 29 Heat exchanged 8740987 BTu/h MTD - cc-Irrected - 30 Transfer rate , Service 5.72 Dirty 16.7 Clean 18.72 31 1 CONSTRUCTION OF ONE SHELL Sketch 32 Shell Side Tube Side 331 DesignlTest pressure psi 260/ ! Code 280/ / Code 620 34 Design temperature F 540 35 Number passes per shell I I 36 1Corrosion allowance .____.. _i.~!. ____.__ 37 Connections In 10 / 300 ANSI 81300 ANSI .I ~_~_J3ize/rating Out 10 / 300 A_~SI 10 / 300 ANSI I 39 inl Intermediate / 300 ANSI ___ 1 300 ANSI I 40 Tube No. 3427 _ 00 0.75 Tks-avg 0.049 in LenRth 10 _ ______ ft Pitch 0.9375 41 Tube type __._...________ Material SS304 [ Tube pattern 30 42 Shell SS304 10 00 60 in . ._ Shell cover .-.:::. -'

w-~

~ 'yJl_
~l.l!~E!§he.E!!:~tationary

45 46 47 48 49 50 51

Impingeme..f!!J~ rotec!Q_ n _ . _~one

_

Type single seg Seal type _ _ .. _

1506

-:~~.. _~~s_k_e_ts-~:~~,-,d;.:.::e",a""d__ ~ 9.o.cJ!'!J.equirements

55 WeiqhUShell 561 Remarks 57 1 1 58

.. ~hannel cover ___ _Iu_be.sheet-f1oating

SS304 SS304

Floating head cover Baffle-crossing SS304 Baftle-Iong Supports-tube _.__ B ass seal Expansion jOint RhoV2-lnlet nozzle

in

Cut(%d) ~_'2.
Spacing: clc 24.75 . 1 Inlet 20.125

in in

U-bend .... ._ _._....

__.._.--.!YP.e _ _ __ Tube-tubesheet joint groove/expand_ Type __ _._.___._.____...__ Bundle entrance 1732 Bundle exit b/tf!':~~ •.•.-- . ....•.. _ ._-_._-.......... __ . 1256 .._ _I_ Tube Side

ASME Code Sec VIII Div 1 32687 Filled with water 49210.8

TEMA class B Bundle 22316.9

Ib

Heat Exchanger Specification Sheet Company: - - -- - -- - - - - - - -- - -1---'1-t-=:.::::.:.:=:c.:.L' -- - -. -- - - - - - - -.."...- - - - - - - - 2 Loca tion: f--=+-===;;.;.:,..- - - - - -- - - - - - - -- - . - - -- --"--.-- - - - - - - -".- - - - - - - - Our Reference: 3 Service of Unit: - - - - - _::::..::.:....:....:.::..:..::.:..=.:-=-=.:'--------_._- - - -- _.. _ - -- -- HX-300 Item No.: . : ='__--'-..c..:....::.::.=-_ __ _ _ ....:....::=-:c..:.::.;c::.:...::=.::..:.... Your Reference: _ __ _ __ _ _ __ _ ._ _ _ _ _ _ _ _ ___________ --~ Rev No.: Job No.: 5 Date: 57 --144 1 series Type 8EM hor Connected in 1 parallel 6 Size in Shells/unit 1 Surf/shell (eff.) 6687.1 7 Surf/unit(eff.) ft2 6687.1 ft2 8 9 Fluid allocation _____ f~+-'-=::"'O:::==~ 10 Fluid name


________I ----'--S7h..:.:e:::,":_:S::.::ide "'=---- -_j-------'Tc.::u:.:::bc::e_S,,,,,id,,,,,eoC-.__ .____ .

S -301

C Wo.

11 Fluid quantity. Total ~~~~~~~~---------~ lb~/h~----~6-=3r03~1'-----+_----~71~7r3~7~7____._. Vapor (in/Out) 12 ~_j__~='-'-'-'.::.==-<----------.---'I.::cb/"-'h+_---'5::.:.7..:::6""05"--_+--1.:.::8:.:::0~78 "---I_---- ____j__--- ~_ _'=i.9.':l.lL. ____ _ ____._ _ _ _ _ _ _ _-'-'lb<,/"'h 1_ _ •_ _ _ •_ _!_'--3:::.:9::.::5:.::2~7-_t_-7 '-1-'-'-" 7 3"-7 7'---_!_--'-7-'-1.:..:73:::.:7-'-7-~j_____ _ "'!Qn_~!!__ de n?a __ bl ~. Ibtl! __ . 5427 - .--t. -- - -

1~ - - - - -- - -- , - . - -- -- - - - +- -16 Temperature (In/Out) 17

Dew / Bubble point

~ Q~..!l~_

-

---1--- - - - - 1 - --

-

- ,,

r---_-'-"-"___ +-_---=90=--_-+_ _ 1..?Q.__._

. -...- - - - - - - - ' - t--=-'-'- "'-"-- - 1 -- - -- + _ - - -- -1-- - - - - 61.587 60.566

_ _ _ __ _ _ _ _ _ _ _.__'~,.

19 Vis~~l'_ __ _ __ _ _ _ _ __ _ _...::=.I-----":.:.=...=--

+_-...::.:.::.='---t- _ ::.: 0 ."-.:::: 78 3 =----1_---"°..:.: .5::.:.7...:.1_ _ 1

!-"2:.-:0_f-'-' Mo:.:,::.: .:.:: lec:..::"" ula:.;,.r..:.;"". wt ' -V:...:a:;< IP'___ _ _ _ _ _ __ _ __ -t-_....:.::..:.:::.:._ __._f-- .:.=.:.:...::...--t----- - -t----.- - I-c2:. :1--1-'-' M.:.::o:.:,:le:..:c:..::u.:..: la:.;,.r..:.; wt c;J.""N .;:..C =--_ _ __ _ _ _____ _-+_--..:4c.:4..:.:.0::.:1_.._ _".._..:.44..:.;.'-=-0..:...1_-+_ ____ --1_ _ _ __ _ 1 1-"'2=2+-=,-pe S",::.;c""ifi.:.:; lc:..oh.:.::ec=t a.:..._ _ _ _ _ _ _ _ _-=B::.:T:..::U:..;./(>.::lb::-_*r:l_-=-0.'-'..7..:..::.. 184-=----1-_-=0.c=.91 5.::..-=-----1f-_=_0:.:: .9..::.30=-:2=----1-_ __ 0.9567 ~2~3+"T::.:.~~~~-=~n he rma l co c:.:d::.::u:..::c:::.-'-' tiv i~tty_ _ _ _ _ _____'B::<.T.:..:U~""'(1ft"-·-'-h'-*F'__":)4-_...:0 :::.:.-=7 0'__ _+-.......::0:.:.: .0::.::9::.::9'--_+-_.0.0.:._30.5.::..6=--_ 1--_0..::..::..8

::.:36 =--_1 ~2:.::'4+=-~te-,-, La ~ n.:..: th c:.:e::.::::,_ at __ __ _ _ _ _ _ _.......::B""'Tc.::U<'-/"' lb'-l____ _---+_ _ _ _ _+_- -""".----"'-- -____ I

25 Inlet pressure (absolute) psi 245.4 80 ~-J-!.:..=~=~~==:::eL.--------......J::O~-------'=-~-'-----_+--,,·-----'=------1 ~2~6~V-=lo e::.::-=iity c~L -_ __

_ __ _ _ __

_ _ _--'-'W:..::s'-l-_

~2~7+_re:::=-u P:...: ss=-:r-=e-=d::..=-' ro p~.-=a-'.:.. "0w-'.-/ca ':..:...;lc:.:.. --------=psii'-l-_ 28 Foulinq resist (min)

ft2*h*F/BTU

29 Heat exchan9..ed 30 Transfer rate. Service

_ _ _.:.::~:::.: 9 . 6 7----_+------~ 4 .2~7-·----- 1 J 0.837 20 ___-'1_ ........;6:..;..1-'-'9c.::2=--_1

0.003 0.003

_ 2 ==--_

203072=-9:eoO'___ ---'B:e..T:..:U:e.,:/"""h=--_ _ _ _....:Mc:..:.:.T""D.:.::::::.:..:e:::: co rr_=ct""'d e"'_ __..._ _.:::.6-'.1:.: .2.: :.6_ _______._ F 49.57 Dirty 70.92 Clean 133.83 BTUI(h*ft2*F)

31 CONSTRUCTION OF ONE SHELL 32 Shell Side 33 DesiqnlTest pressure psi 2601 ICode 34 Desiqn temperature 35 Number passes per shell

F

Sketch

Tube Side

751 I Code

.._....::.34-'-'0= --_ _ _ +___...:1:.::8:.::0_ _ --1 1 S

. .

~ ;

~

36 ,forrosion allo~ance .,--_ _ _.....:.: in-'j-_______ .__.__-I-_ __ O::.:.""0.::.62=.:5:::....._--I 37 Conne~!ions _ _ _ -1--'-'ln 12 / 300 ANSI 12 / 150 ANSI f.'3.._8+-_ :::.;.: Siz.:::;"'::..: e/ra tc:.:. inO>Z..g _ _ -+-=0'-"u:..:.t__ .._....,,_ I - ------="" SI -3-0_0_A_N_S_I_ ____..;.;~_ 12f/1:..=5'-"0'-'...:; A N..;.;S ::.;'-I I f.'3___9+-_ _-'i.:..:n.:...I_ _ _ __'_""ln.;..:te::..:r..:..;me-=.:;dc..:ia:..:,te=--'---_. ___41 300 ANSI .. 1 150 ANSI f.=4~0~T.::: u:::be~N~o"-=:29 . ~1:...4:-_ __-.-;:: 0:.:0:........::0:..:.:'--'~_-'.75 T!.:;"ks-a~v'-'g,_:::: Oc.Q65

41 42 --43 44

Tube type Shell SS304 Channel or bonnet Tubesheet-stationary

in Length 12 ._ _ _ _.,..:-:ftc.......:.P""'it:.::.ch:.:....::O..:..;.9c.::3'-'..7..::.5_ __ ..:.:..:.1 in Material CS I Tube pattern 30 0058 10 Shell cover in - - - - - - _.. CS___ _ ___________-t--=C""'h.=nnel a= coy~'_'_r_ __ _ ___.________._ _ _ _ floalic-."'--_ __ _ _______ _ _ __ SS304 Tubesheet.: .c..""""ng

f.=4":'5~F-~ lo::.::a:.::ti:.:J ng:L:.:. he~a""'d::....c :::;o:o.:vc::: e'-r_ _ _ _ __ __

46 8affle-crossino

SS304

Type

Impingem~.n!.pr();~ction

___ __ single=-~se-"'g"--_

_C =_u=-t"-'-(o/~d)

44

vert

Plate on b.LJQ_d_le__ __ __

Spacing: clc 30

in

4:::7:...~B~aff ~c:.:le:.-::.:: . lo~n.:;z.g----------.-;::S-=al e"-'-~Q.e=--_._ _ ___._ _ _......"..... _ _ ___'_I""lnc:.:leL_?B.125 4.~8~S.::: u ~~"' pP(O rts:..: -t:.:: u.:::::::_.. be _ _ _ __ __

,±~~)'P.ass

____'U ::<.-_"b_= e::.:.:::_.._ nd ... _

_. _ _i_n

__ _ _ ______T.Y~_._ ____. ___"._._..._ ._ _ _

__ Iu.Q.~..::!.':l.besheet joint_.. .. . __grQ.ove/expand _ _ ._ _ _ _ _ _ __ _ __T:.ry,pEe_ '-= _ _ _ __ _ _ __ _ _ _ ____ .......".......__ 51 RhoV2-I nlet nozzle 1257 Bu nd Ie en tran ce "-354 =-=--_ _ _ __ _~-= B u'_'_=~ nd l e..::e..:..; x'_'_it......:..11,-1_ . _ _ Ig/m:'l@ 5~2~G :::;a~s::.: k_=ts_' e =_ -.:.::::.:. S h::.:: e::.:. II .:::.id_= s:.:: e_ __ _ _ _______ _......:. T_=be u.::."---"""___ Side'--_ __ __ ,, __ ._. "_____ . __ _ _ _ ._ _

seal

5~0_+=-~~~~ Ex p a n s::.:: io::.: n..J;joi :::;::.:. nt:..-_

. ~5::!..3j---......:.F..:.:=o lo a'-"ti.:..: n-"g--'-'h-=ad e=:::.....-.-------- . - - - . - _._...........__.__ _ __ ___. . _-- -- - - - 54 Code reg uiremen~.._ ._ _-'A..:cS=M~E....:C""'od=e....:S""'e::.::c:...V:..:I.:.:".:::.D~iv:....:...1_ ___ ._ _ . TEMA class .=B_ _ _ _ _ _ __ 55 WeighVSheil 33610.4 Filled with water 52103.5 Bundle 24991 .7 Ib

56 Remarks

~5~7+------------ ..- - - - - -- - - --- -- - - -58

-,,---- - -- -- .-.._""..""___.......... _.

Heat Exchanger Specification Sheet 1 Company: 2 Location: 4 Item No.:

Reference: _._--_._-----_._..__Your ...• .._---.-.----- _ - --- - _

HX-530 ... _--_..

..

Job No.:

19--=~5.9______


..

"

Rev No.:

5 Date: 6 Size 7 Surf/unit(eft.)

320

_ ~D .._ _ __J:xRe BEM tt2 Shells/unit 1

Connected in 1 Rarallel Surf/shell (eft.) 320

hor


_._-----_._---_._.

---

10 Fluid name 11 Fluid guanti~, Total E . VaRor (In/Out) 13 14

._---_._ ---_._--_.._ - -...__.._ -_._ - - -- -_._-----------_._ ._ ._-_ .. -- -

Our Reference:

3 Service of Unit:

Li9.lJi.cL......

Ib/h Ib/h

Noncondensable

Ib/h

tt2

Tube Side

)-5Ob~

Ib/h

1series

CW

44655

100948

44655

44655

100948

100948

262.7

158

90

120

56.556 0.273

60.619 0.498

62.224 0.762

61 .861

0.6681 0.149

0.6283 0.15

1.0006 0.352

0.9998 0.364

15

~ ~mRerature (In/Out) ~ Dew / Bubble point

F F Iblft3 cp

18 Density

19 Viscosi~ 20 Molecular wt, VaR 21 Molecular wt, NC 22 Specific heat 23 Thermal conductivity

BTUI(lb~F) BTUI(ft*h~F)

24 Latent heat 25 Inlet pressure (absolute)

BTUllb

26 Velocity 27 Pressure drop, allowJcalc. 28 Fouling resist. (min)

psi

37 .8

ftls

1.45 ---.--- -

psi

34 Design temRerature 35 Number Rasses per shell

F

36 Corrosion allowance 37 Connections

in In

~ _Si?e/rating in / ;39 40 Tube No. 82

Out Intermediate 00 0.75 ID

OD 10.75

44 Tubesheet-statio~'§~Q~ .5~ Floating head cover 46 Baffle-crossing_ SS304 47 Baffle-Ionq 48 Supports-tube

F BTUI(h·tt2~F)

Sketch Tube Side

751

I Code 180

1

2 0.0625

~

I

~ .

~

,

I

6/ 150 ANSI 6/ 150 ANSI / 150 ANSI

/ 150 ANSI 0.065

in Length 20 Material CS Shell cover in

tt Pitch 0.9375

I Tube Rattern

Channel cover

in

30

._.

Impinqement protection T~e

single seg Seal type

Cut(%d)

27

Tube-tubesheet joint Type

.

58 -

C'1.

10.5625

Bundle exit 120

Tube Side

2- f--.

Inlet

in in

qroove/expand

Bundle entrance 129

~ rB·~f!1arks

SRacing: dc 4.625

Type

U-bend

-'-

None

hor

1

54 Code reQl!irements___. ... _._._~SME_~.Q1?_9~.c;.Y"1 Div 1 1538.1 Filled with water 2250.1 55 WeiqhUShell

.

95.18

Tubesheet-floating

49 Bypass seal 50 Expansion joint 1130 51 RhoV2·lnlet nozzle 52 Gaskets - Shell side Floating h~§l.g_ .._ 53

3.453

0.003

Clean 344.11

330

CS

I

20

0.003 MTD corrected

3/ 150 ANSI 3/ 150 ANSI Tks-avg

80 5.25

- - _._----_...

4.707 ._- -

5

tt2*h*F/BTU BTUlh Dirty

3029000 29 Heat exchanged 99.44 104.88 30 Transfer rate, Service CONSTRUCTION OF ONE SHELL 31 Shell Side 32 psi 751 ICode 33 Desiqn/Test pressure

41 Tube type . SS304 42 Shell 43 Channel or bonnet

0.561

Ib/(ft*s2)

__

._.. _...._..•. _- - -----_._-- ---_. B ... _--_.-.-_.. _..._ ----------_._..TEMAciass "--- _.... __...__ ._-_..... _-_ - ._ .._-_.

-_...._--- - _.

Bundle

935

Ib

Heat Exchanger Specification Sheet 1 Comf2 an t Location: Service of Unit: Item No.: Date:

2 3 4 5

6 Size 7 Surf/unit(eft.)

. .. .

-_._.-- . .....HX-710

_

Rev No.:

Our Reference: Your Reference: --, .. _---_.__._-_.. Job No.:

17 --240 921

in ft2

Typ-e BEM Shells/unit 1

hor



8 9 Fluid allocation 10 Fluid name

Ib/h Ib/h Ib/h Ib/h

ft2

Tube Side

S-70;

Cw

11 Fluid Quanl!.!Y, Total E _._Yi3.por (In/Out) Liquid 13 Noncondensable 14

1 series

1 f2arallel 921

122949

40674 122949

40674

40674

120

257

113

62.224 0.762

61 .862 0.561

49.737 0.212

55.839 0.49

1.0006 0.352

0.9998 0.364

0.6598 0.141

0.6038 0.146

122949

15 16 17 18 19 20 21 22

Temperature (In/Out)

F F Iblft3 cp

Dew / ~ubble point Density Viscosity Molecular wt, Vap Molecular wt, NC Specific heat Thermal conduclivi!):' ~ 24. Latent heat .--- r1-~let f2ressure (abs.olute) 26 Velocity 27 Pressure drop, allow.lcalc.

E

BTu/llb*F) BTUI(ft*h*Fl. BTUllb psi

_.

90

._-

80 2.57

ftls psi ft2*h*F/BTU BTU/h Dirty

20 ... 28 Foulinq resist. (min) 3689136 29 Heat ex~hanged 86.31 95.47 30 Transfer rate, Service CONSTRUCTION OF ONE SHELL 31 Shell Side 32 -_. psi 751 ICode 33 g~~gnfTest ~ressure 180 F r-!2-~_~lgn temf2erature ~ 1 ~~ ~.r:nber f2asses f2er shell 0.0625 in 36 Corrosion allowance In 6/ 150 ANSI 37 Connections 6/ 150 ANSI Out Size/raUnq 38 39 40 41 42 43 44

in / Tube No. 236 Tube type Shell CS Channel or bo~net Tubesheet-stational}'

45 Fl oa lin~Lh.~ad cover CS 46 Baftle-c!ossing 47 Baffle- lo.r:!9

..

19.818 0.003 MTD corrected Clean 260.06 Tube Side I Code 320 6 -.- ...------.- -.

751

- . - ~ -.-----

3 / 150 ANSI 3/ 150ANSI Intermediate / 150 ANSI / 150 ANSI 00 0.75 Tks-avg 0.065 in Length 20 Material CS 10._. 0018 Shell cover in Channel cover SS304 SS304 Tubesheet-floatinq Type

single seg Seal type U-bend

..

39 2.6

'_.

.lD:lJ>.irJ.gement f2rotection hor Cut(%d) 27

3

2.503 0.003 BTu/(h*ft2*F) Sketch

3

t

~ , ,

ft Pitch 0.9375

I Tube f2attern

57 58

.•... ........

Ot

l

in

30

None

- in in

Sf2acing: dc 3.625 15.9375 Iiniet

_•....._-_.

._ --_.

,

I

._.._.....J.Y2e .._--_.. ~ ~u.QQorts-tube Tube-tubesheet joint 49 Bypass seal groovelexf2and ._.. __ . e 50 Exf2ansion joint T:tf2 .---_. 487 Bundle entrance 403 -_._-_._-_._- 51 RhoV2-lnlet nozzle -Bundle --_._- exit 405 Tube Side 52 Gaskets - Shell side --_.._ F!oating head 53 ASME Code Sec VIII Div 1 TEMA class B 54 Code reQuir~r:nen\s 4306 Filled with water 6250.3 Bundle 2730.5 55 WeiqhUShell 2§. Remarks

_----.L

46.41

Ib/(ft*s2)

Ib . -

_---

._---

-

-..-

PUMP

Identification


Date: By:

Pump P-110 1

4/1/02

akg

Principal Function: Increase the pressure of the S-104 Stream from M-100

Operation:

Continuous

Materials handled: Quantity (lblhr):

Inlet Stream (S-l 04) 42571.91

Outlet Stream (S-20l) 42571.91

trace trace

trace trace

trace 0.006 1.49 0.001 365.11 42,205.31

trace 0.006 1.49 0.001 365.11 42,205.31

238 14.7

241.9 263

Composition (lb/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF): Pressure (psia):

Design Data: Type: Centrifugal Efficiency: Pressure Change (psia): 248.3 Electricity Required (KW) Volumetric Flow Rate (ft31hr): 720.2 Material of Construction: Net Work (hp): 24.9

0.52 18.6 Stainless Steel

Comments and Drawings: See process flow sheet pg.13 and pricing info on Appendix A pg.184

95

PUMP

Identification


Pump P-540 1

4/1/02 akg

Date: By:

Principal Function: To increase the pressure of the S-507 stream from HX-530

Operation:

Continuous

I

Materials handled: Quantity (lb/hr):

Inlet Stream (S-507} 62,277.91

Outlet Stream (S-304} 62,277.91


trace

6.47 785.89 2,775.68 110.70 13,552.93 45,046.25

158 31.8

159.2 235


Design Data: Type: Centrifugal Efficiency: Pressure Change (psia): 203.2 Electricity Required (KW~ Volumetric Flow Rate (ft3Ihr): 95307 Material of Construction: Net Work (hp): 25 .3

trace trace .trace trace


Comments and Drawings: See process flowsheet pg.14 and pricing info on Appendix A pg.185

96

PUMP

Identification


Pump P-600 1

4/1/02

Date: By:

akg

Principal Function: Increase the pressure of the S-601 Stream

Operation:

Continuous


Inlet Stream (S-60l) 29,861.62

Outlet Stream (S-602) 29,861.62



262.7 37.8

263.2 100


Design Data: Type: Centrifugal Efficiency: Pressure Change (psia): 62.2 Electricity Required (KW~ Volumetric Flow Rate (ft31hr): 551.7 Material of Construction: Net Work (hp): 5.14



97

PUMP

Iden tification


Pump P-620

4/1/02

Date: By:

akg

I

Principal Function: Increase the pressure of the S-604 stream from DE-720

Operation:

Continuous


I I I

I


Outlet Stream (S-603}

22,326.31

< 0.001

< 0.001

trace

trace

17.83 1,598.79 17,200.99 110.58 1,746.22 1,651.91

17.83 1,598.79 17,200.99 110.58 1,746.22 1,651.91

Composition (lblhr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF): Pressure (psia):

117.9 35

Design Data: Centrifugal Efficiency: Type: Pressure Change (psia): Electricity Required (KW~ 9 Volumetric Flow Rate (ft3 /hr): 399.2 Material of Construction: Net Work (hp): 0.6

118.1

98



98

PUMP

Identification


Pump P-730 1

Date: By:

4/1/02 akg

Principal Function: Increase the pressure of the S-705 stream

I

Continuous

Operation:



Outlet Stream (S-702} 5,111.13

< 0.001 trace

< 0.001 trace

4.82 487.45 4,044.88 31.88 540.20 1.90

4.82 487.45 4,044.88 31.88 540.20 1.90

182.3 24.7

182.5 40

Composition (lblhr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF): Pressure (psia):

Design Data: Type: Centrifugal Efficiency: Pressure Change (psia): 703 Electricity Required (KW; Volumetric Flow Rate (ft3/hr): 97 Material of Construction : Net Work (hp): 1.68


Comments and Drawings: See process flowsheet pg.15 and pricing info on Appendix A pg.187 -

-

-

-

99

-

PUMP

Identification


Pump PB-500

Date: By:

411102

akg

1

Principal Function:

Increase pressure at the reboiler

Operation:

Continuous

Inlet Stream 92130.05


Outlet Stream 92130.05

Composition (lb/hr): Hydrogen

trace

trace

Carbon Dioxide

trace

trace

Methane

trace

trace

Ethylene

trace

trace

Ethane

trace

trace

Acetaldehyde

7.21

7.21

Acetone

1,162.69

1,162.69

Ethyl Acetate

4,106.62

4,106.62

163.78

163.78

Water

20,050.10

20,050.10

Acetic Acid

66,639.65

66,639.65

114.97 34

262.7 37.8

Ethanol


Design Data: Centrifugal Type: Pressure Change (psia) 2 289.23 Volumetric Flow Rate 4.18 Net Work (hp): I

100

Efficiency: 0.56 7.46 Electricity Required (K" Material of Construction Stainless Steel

PUMP

Identification


Pump PB-6l0 1

Date: By:

Principal Function:

Pump bottoms of acetic acid distilIation column

Operation:

Continuous



4/ 1/02

akg



trace

trace

Carbon Dioxide

trace

trace

Methane

O.OOE+OO

O.OOE+OO

Ethylene

O.OOE+OO

O.OOE+OO

Ethane

O.OOE+OO

O.OOE+OO

Acetaldehyde

0.00

0.00

Acetone

0.01

0.01

Ethyl Acetate

0.02

0.02

Ethanol

0.00

0.00

366.31

366 .31

20,371.87

20,371 .87

297 .32 98.5

272.5 98.6

Water Acetic Acid

Temperature (oF): Pressure (psia) :

Design Data: Type: Pressure Change (psia) Volumetric Flow Rate Net Work (hp):

Centrifugal

I

0.1 493.46 4.68

101

Efficiency: 0.56 Electricity Required (KVI 11.2 Material of Construction Stainless Steel

PUMP

Identification


Pump PB-810 1

Date: , By:

Principal Function:

Increase pressure of bottoms of acetone distillation column.

Operation:

Continuous

Inlet Stream 755.20


4/1/02

akg



220E-27

2.20E-27

Carbon Dioxide

0,00

0.00

Methane

0.00

0.00

Ethylene

0.00

0,00

Ethane

0,00

0.00

Acetaldehyde

0.17

0,17

63.50

63.50

610.00

610.00

2.74

2.74

77.92

77.92

0.88

0,88

183.14 24.8

184.33

Acetone Ethyl Acetate Ethanol Water Acetic Acid


Design Data: Centrifugal Type: 0.1 Pressure Change (psia) Flow Rate (gpm): 4.24 0.04 Net Work (hp):

102

24.9


PUMP I

Date: By:

4/ 1/02 1 akg

Iden tifica tion


Principal Function:

Increase pressure of bottoms of near azeotrope distillation column

Operation:

Continuous

Pump PB-900 1



Composition (lblhr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

trace trace


Design Data: Type: Centrifugal Pressure Change (psia) 0.1 Flow Rate (gpm): 44.5 9 Net Work (hp): 0.17

103


trace trace 0.00

0.00

0.00

0.00

0.00

0.00

0.00

0.00

0.89

0.89

1,137.03

1,137.03

0.24

0.24

1.78

1.78

438.03

438 .03

212.64 27.9

221.03 28

0.6 Efficiency: Electricity Required (K\\ 0.37 Material of Construction Stainless Steel

PUMP 4/1/02 akg

Date: By:

Identification


Pump PB-910 1

Principal Function:

Increase pressure of bottoms of ethyl aceteate distillation column.

Operation:

Continuous

Materials bandied: Quantity (lblhr):

Inlet Stream 438.03


Composition (1blhr): Hydrogen

0.00

0.00

Carbon Dioxide

0.00

0.00 0.00

Methane

0.00

Ethylene

0.00

0.00

Ethane

0.00

0.00

Acetaldehyde

0.00

0.00

Acetone

0.00

0.00

Ethyl Acetate

1.48

1.48

Ethanol

0.00

0.00

Water

0.00

0.00

436 .56

436.56

261 .71 20

262.93 20.1

Acetic Acid


Design Data: Centrifugal Type: Pressure Change (psia) 0.1 Flow Rate (gpm): 2200.93 Net Work (hp): 0.125

104

Efficiency: 0.56 Electricity Required (K~ 0.3 Material of Construction Stainless Steel

PUMP Identification


Principal Function:

Return reflux to acetaldehyde distillation column.

Operation:

Continuous

Date: By:

Pump PR-500 1



Composition (lb/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

4/1/02 akg


0.041

0.041

220.678

220.678

50.39

50.39

49.998

49.998

54.4

54.4

12,833.82

12,833.82

trace trace trace

trace trace trace 30.79

trace


114.97 34

Design Data: Centrifugal Type: 2 Pressure Change (psia) Flow rate (gpm) 67.57 Net Work (hp): 0.62 -

105

30.79

trace 101.8

32

Efficiency: 0.6 Electricity Required (K'VI 1.49 Material of Construction Stainless Steel

PUMP

Identification


Date: By:

Pump PR-510 1

4/1/02 akg

Principal Function:

Operation:

Continuous

Inlet Stream 2070


Outlet Stream 2070

Composition (lb/hr): Hydrogen Carbon Dioxide

37.26

37.26

Methane

2.836 13.04

2.836

9.23

9.23 2,007 .65

Ethylene Ethane

13.04

2,007.65

Acetaldehyde Acetone

trace

trace

Ethyl Acetate

trace

trace

Ethanol

trace

trace

Water

trace

trace

Acetic Acid

trace

trace


94 30

Design Data: Centrifugal Type: Pressure Change (psia) 2 Flow Rate (gpm) 3.5 0.2 Net Work (hp):

106

10 28

Efficiency: 0.6 0.25 Electricity Required (K'" Material of Construction Stainless Steel

PUMP

Date: By:

Identification


Principal Function:

Return reflux to acetic acid distillation column.

Operation:

Continuous

Pump PR-610 1

4/1/02 1 akg

I




Design Data: Centrifugal Type: 2 Pressure Change (psia) Flow Rate (gpm): 241.8 Net Work (hp): 2.34

107


8.00E-05 1.71 E-08 0.00 0.00 0.00 22 .03 1,974.66 18,527.79 163.64 7,876 .99 2,872.85

8.00E-05 1.71 E-08 0.00 0.00 0.00 22.03 1,974.66 18,527.79 163.64 7,876.99 2,872.85

297 .32 95

272.5 97

Efficiency: 0.6 Electricity Required (K~ 5.6 Material of Construction Stainless Steel

PUMP

'Identification


Principal Function:

Return reflux to stripper column

Operation:

Continuous

Date: By:

Pump PR-800 1



4/ 1102 akg


Composition (lblhr): Hydrogen

trace

trace

Carbon Dioxide

0.00

0.00

Methane

0.00

0.00

Ethylene

0.00

0.00

Ethane

0.00

0.00

Acetaldehyde

3.52

3.52

Acetone

293.40

293.40

Ethyl Acetate

784 .07

784.07

Ethanol Water Acetic Acid


Design Data: Type: Centrifugal Pressure Change (psia) 2 Flow Rate (gpm): 9.46 Net Work (hp): 0.11

108

5.13

5.13

107.27

107.27

0.88

0.88

181.81 25

182.04 27

Efficiency: 0.6 0.25 Electricity Required (K'-' Material of Construction Stainless Steel

PUMP

Identification


Date: By:

Principal Function:

Return reflux to acetone distillation column

Operation:

Continuous

Pump PR-810 1


Inlet Stream 439.06

4/1102 akg



2.00E-08

2.00E-08

Carbon Dioxide

0.00

0.00

Methane

0.00

0.00

Ethylene

0.00

0.00

Ethane

0.00

0.00

Acetaldehyde

3.35

3.35

Acetone

229.90

229.90

Ethyl Acetate

174.07

174.07

2.39

2.39

29.35

29.35

0.00

0.00

167.98 22

174.97 24

Ethanol Water Acetic Acid


Design Data: Centrifugal Type: Pressure Change (psia) 2 Flow Rate (gpm): 4.09 0.043 Net Work (hp):

Efficiency: 0.6 0.097 Electricity Required (K'" Material of Construction Stainless Steel I

109

PUMP Identification


Date: By:

Pump PR-900 1

Principal Function:

Return reflux to near azeotrope column.

Operation:

Continuous

Materials handled:


Quantity (lblhr):

I

Composition (lb/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF) : Pressure (psia) :

4/1 /02 akg


2.13E-05 4.48E-09 O.OOE+OO O.OOE+OO O.OOE+OO 4.95 423 .97 3,435.12 29.16 462.42 1.02

2.13E-05 4.48E-09 O.OOE+OO O.OOE+OO O.OOE+OO 4.95 423.97 3,435.12 29 .16 462.42 1.02

181.9 25

189.94 27

Design Data: Centrifugal Type : 2 Pressure Change (psia) Flow Rate (gpm): 10.425 Net Work (hp) : 0.5

110

Efficiency: 0.6 1.12 Electricity Required (K" Material of Construction Stainless Steel

PUMP

Identification


Principal Function:

Return reflux to ethyl acetate distillation column.

Operation:

Continuous

Pump PR-910 1

Date: By:



4/1/02 akg



0.00

0.00

Carbon Dioxide

0.00

0.00

Methane

0.00

0.00

Ethylene

0.00

0.00

Ethane

0.00

0.00

Acetaldehyde

0.00

0.00

Acetone

0.89

0.89

1,135.56

1,135.56

Ethanol

0.24

0.24

Water

1.78

1.78

Acetic Acid

1.48

1.48

174.96 16

182.05 18

Ethyl Acetate


Design Data: Centrifugal Type: Pressure Change (psia) 2 Flow Rate (gpm): 4.43 Net Work (hp): 0.043

111


REACTOR

Reactor RX-240 1

Item Item No. No. Required

Function:

Hydrogenation of Acetic Acid to produce Acetaldehyde

Operation:

Continuous

Feed (S-205)

Materials handled: Quantity (Ib/hr): Composition (lb/hr):

Product CS-206)

62,974.33

62,977 .88

Hydrogen

7,781.47

7,088.04

Carbon Dioxide

5,137 .53

5,425.89

Methane

1,495.12

1,565.20

Ethylene

855.34

916.61

Ethane

855.42

921 .10

Acetaldehyde

621.46

13,468.60

Acetone

285.40

665.97

Ethyl Acetate

908 .00

908 .03

17.25

771.86

1,299.08

7,201 .54

43,718.26

24,045 .05

599

556.8

252 .0

250 .9

Ethanol Water Acetic Acid Temperature (oF): Pressure (psia) :

Design Data:

4/9/02 cp

Date: Bye:

Identification:

Height (ft): Diameter (ft): Volume (ft3):

17 Pressure (psia): 250 .92 4 Catalyst: 86 .27ft3 of Pd on iron-oxide 213 .63 Material of Construction : Stainless Steel

112

Heat Exchanger Specification Sheet 1 2 3 4 r-- 5

Company: -' Location: ...... Service of Unit: R-500 Item No.: -- - ,. Rev No.: Date: ~

Our Reference: Your Reference: --._---- Job No.:

55 / 7.?_ ____:.:tj6 ~ Size 8107.7 7 Surf/unit(eft.) 8 ..J!. Fluid allocation 10 Fluid name 11 Fluid quantity, Total Vapor (In/Out) 12 13 Liqu.!Q._ Noncondensable 14

in ft2

Ty~e BKU Shells/unit 2

hor


PERFORMANCE OF ONE UNIT Shell Side -

-~ .- -

----- -

:>TEAn

126836

18288 41530 85307

126836

18288 18288 ...

1..:'2 --- 16 17 18 19 20 21

ft2

Tube Side

:, -"fe'

Ib/h Ib/h Ib/h Ib/h

1series

212arallel 4053.8

r- -

Tem~rature

(In/Out) Dew / Bubble ~oint Density Viscosity_ Molecular W!, Vap

- .•.--.--... -----.

F F Ib/ft3 cp

255.5

262.66 255.5

53.886 0.268 38.49

0.18 0_013

280.95 280.95 0.115 0_014

__ .

- - 280.95 280.95 57 .874 0.212

-~ .-- . -

36.06

Molecular w1._NC _.. _ __ ____....I FUf.(lb*Ft ---.'_._-_. 0.3781 j?pecific heat 0.5292 __... ~ 23 Thermal condu(~.tivity BTU/(ft*h*F) 0.089 0.013 24 Latent heat BTUlib 574 536.2 . 25 Inlet pressure (absolute) psi 37.7 26 Veloci!y . ftls 27 Pre ssur~_9.~c:>p_, . allow./calc. psi 28 Fouling resist. (min) ft2*h*F/BTU 0.003 16837400 29 Heat exchanged BTUth MTD corrected 97.8 Dirty 105.34 Clean 349.16 30 Transfer rate, Service 31 CONSTRUCTION OF ONE SHELL ._ _ _~hell Side 32 Tube Side .. _-_ .. .. 33 DesignfTest Pt~ssure 751 ICode ICode 751 P~! 330 34 Design teml2er~_ture F 350 35 Number passes_per shell 1 2 - 0.0625 0.0625 in ~~~()sion allowance ~ In 4/ 150 ANSI 37 Connections 10/ 150 ANSI 8/ 150 ANSI 38 Size/rating Out 2/ 150 ANSI Intermediate 4/150 ANSI / 150 ANSI 39 in ! 00 0.75 40 Tube No. 11 04Us Tks..avg . 0.065 in Leflg!h 8 41 Tube type Material CS -10 42 Shell CS 0056 in Shell cover CS 43 Channel or bonnet Channel coveL . _ _.._._ CS 44 Tubesheet-stationary CS Tubesheet-f1~'l..~ .flg.._ __

_-

0.5457 0.016 920.7

1.0099 0.3~

920.7 50 9.51

- - 0.097

5 0.003 21.23

F BTU/(h*ft2*F) Sketch

~

1n.:!P.l!!g!,!_rrJ~_Q..~~rotection

§ rBCJ?t!flQ head cover CS § ~Ie- c::!:..()ssing

Ty~e

.iL ~Ie-Iong .. 48 - - §~Pl2orts-tube 49 50 51 52 53 54

-

Bypass seal Expansion jOint .... .. .". 757 . . .. . .- ... -RhoV2-lnlet nozzle Gaskets - Shell side

__

_

single seg

Cut('Z'o.d.)

Seal tYl2e U-bend _ .......................

45

vert

I

I

ft Pitch 1

I Tube ~attem

in 90 .-

None S~acing:

dc 22.875

I Inlet

22.875

in in

_--

Type .. _ Tube-tubesheet joint _g!()olJ~!~)(P?n.P _ ... _lype _ . .. .. _'- ---_.-.Bundle exit IbLltr.!@ _.. ....Bundle _ - entrance -_.- ----_...._---- Tube Side

_

. Floating head

Code r~ql:'~em~nts 55 WeighVShell 56 Remarks 57 58

ASME Code Sec VIII Div 1 21266.1 Filled with water 46399.7 ._._

;; "t

TEMAciass B Bundle 12624.8

Ib

Heat Exchanger Specification Sheet 1 Company: 2 Location: 3 Service of Unit: 4 Item No.: R-610

-

Our Reference:

Rev No.:

5 Date: 49/63 6 Size 7 Surf/unit(eff.)

7200

in

TY12e BKU Shells/unit 1

ft2

13


15 16 17

t--

Tem~erature

-

Connected in Surf/shell (eff.)

1 [!arallel 7200

Ib/h Ib/h · Ib/h

ft2

STEAfI?

210358

48604 191005

210358

1 series

Tube Side

S -iO)

r1-! £!!!.lQ_guantity, Total 14

hor


9 Fluid allocation - ' . . __ ..name c-!Q. - Fluid Vapor (In/Out)

---

Job No.:

--240

8

12

.

Your Reference:

48604

19353

48604

Ib/h

(In/Out)

F

Dew / Bubble point

F

18 Densi!Y 19 Viscosity 20 Molecular wt, Vap

Iblft3 cp

358.3

369.9

415.6 415.6

415.6

53.128 0.174

358.35 0.647 0.014

415.6

0.606 0.017

53.281 0.137

0.7365

1.0511 0.375

54 - r-___54 ---.-

21 Molecular wt, NC 22 Specific heat 23 Thermal conductivity 24 Latent heat

~_TUl(lb*F)

BTU/(ft*h*F)

0.6376

0.3969 0.015

0.09

BTUlib

25 Inlet pressure (absolute) 26 Velocity - 27 Pressure drop, allow.lcalc.

0.022 813.4

193.3

psi

98.6

_ _ 1i13.4_ 293

12.18 ftls 2 0.262 psi 28 Fouling resist. ' (min) ft2*h*F/BTU 0.003 0.003 MTD corrected 39535070 29 Jieat exchanged BTu/h 50.33 F Dirty 112.49 109.1 Clean 442.42 BTu/(h*ft2*F) 30 Transfer rate, Service 31 CONSTRUCTION OF ONE SHELL Sketch Shell Side Tube Side ~ ' -_. i 9 9 t 100/ ICode 33 DesiqnlTest pressure 310/ / Code ---p'si 430 480 F 34 Design temperature 1 2 35 Number passes per shell ! i 9 9 9 in 0.0625 36 Corrosion allowance 37 Connections In 4 / 150ANSI 10/ 300 ANSI 10/ 150ANSI Out Size/rating 3/ 300 ANSI 38 Intermediate 3/ 150ANSI / 300 ANSI 39 in/ 0.75 Tks-ilvg 0.065 Tube No. 872Us OD in Length 20 ft Pitch 1 in ~.o Material CS 41 Tube type I Tube pattern 90 10 0050 Shell cover 42 Shell SS304 in SS304 - - - _ .__._---_.. ----------43 Channel or bonnet Channel cover CS .-- 44 Tubesheet-slationary SS304 Tubesheet-floating _._--- _. r- Impingement protection Floating head cover None _._- ' -_. ~ single seg 44 SS304 Cut(%d) vert S[!acing : dc 23.375 Baffle-crossing in IY[!e ~ in _Baffle-long I Inlet 23.375 . ---_ ..... ._--_._ .._ ..... Seal type

~

r1Z Supports-tube

__

48 49 Bypass seal ... -. 50 ExPansion ioiQ~ 51 RhoV2-lnlet nozzle

U-bend TY12e Bundle entrance

528

55 WeighVShell

56 J~emarks 57 58

groove/ex[!and

._--

-- ---. Ib/(ft*s~

Bundle exit

Tube Side

52 Gaskets - Shell side Floating head 53

~ ~c:!.ereguirements

T.YQe Tube-tubeshe~~j!Jint

ASME Code Sec VIII Div 1 31395.9

Filled with water

TEMA class 64245.4

Bundle

B

21981 .2

Ib

Heat Exchanger Specification Sheet 2 Location: '~.

"'~"

----_._--_._--

----

1---3. .~e-",ice of Unit: 4 Item No.:

Our Reference:

R-810

51 Date: 6 Size

_ .

Your Reference: Job No.:

Rev No.: 15 I 20

-48

7 Surf/unit(eff.)

in

120.2

Type BKU

hor

Connected in

Shells/unit 1

ft2


1 parallel

Surflshell (eff.)


11 Fluid Q.U?Cl.!!.!Y., Total ~ __'{9.~Out) 113 Liquid 14 Noncondensable

Ib/h Ib/h Ib/h Ib/h

1764 1

~1GArn

1039 755._

I

1764

ft2

Tube Side

S- iDj

10 Fluid name

1series

120.2

265 1

265

I

265

___

- -·_·+1- -- - - - j f - -

15

10., -11:;; 1 AA ~.1 ____~ F,I---~~~--+---~~--_+

16 Temperature (In/Ol''' ~I Dew I Bubble pn;n. 171 uuvv, .... e,",,11 n 18 Oensi 19 Viscosi 20 Molecular wt, Vap__ ,.~.!.

235 235 183.37 235 235 F+I--------t---'-=-=~-__j---.-::='----'I_--'='---51.07 0.211 0.056 Ib/ft3 59.228 _.....__ ...__ .•...• .. ··· -·· ---·· · r-~ cp 0.266 0.063 0.013 0.256

· · ····-·-..

Molecular wt, NC

22 S ecific heat u, "'I'U , ' I -:=n:.::d:.::u:.:: c.::.'_'i_"''-tiv ty _ __ _ _ _ ___=~ 23 l}:1~Lf!lal .co 24 Latent hea:..;:t_ _ __

25 !il!~tprt3.~sure (absolute 1 26 Velocity

"'~' I

?7..l!:ressure drop, allow./calc. 281 Fouling resist. (min) 29 Heat exctJaflged 252310 30 Transfer rate, Service 41.04 31 I

ft2*h*F/BTU BTUlh Dirty

102.16

0.003 MTO corrected Clean 299.63

l.3.p~~JgnlTest pressure

psi

li.~?igl).

temperature l.§..~r:T.l~er passes per shell 35 Corrosion allowance 37 Connections In 38 Size/rating Out 39 in l 40 Tube No. 70Us

75/

75/

1

Tks-avg

1 150 ANSI

1/ 150 ANSI 0.049

00 16

44 Tubesheet-station?_ry__ ~~30':.. 45 Floating. head C()ver 47 Baffle-long

single seg

Cut(%d)

46

8 ~P2orts-tuQe ..

~

"

)

I in

None

ve.~Spacing :

dc 15

I Inlet

Seal type

in

15

in

Typ~

U-bend

49 ~~?EO.aL 50 rE-X2~!l.~!On jOint 51 RhoV2-lnletn()zzle

'f 0 -'-

... f!._~itch_ 1

in Length 4

Impingement protection Type

!

I

Material SS304 ...... __ ._. J.IlJ~ep.a..~~~rn 90 ._~I)__._ .....§.b.f:3.ll..~v~r SS304 Channel cover Tubesheet-floating

...9 hannel or bOI)~~S .. SS304

~ ~

/ Code 2 0.0.51? .. ,,___ .

2/-_.1_50ANSI ..................... - _ .

1/ 150 ANSI 1

1/ 150ANSI 2/ 150 ANSI

41 Tube type

10

/ Code

in

Intermediate 00 0.75

42 ~ . SS304

Tube Side

250~0

F

F BTU/(h*ft2*F)

Sketch

Shell Side

46 Baffle-crossing .

0.003 51.14


32

~:3

_____ _ _

Tub.~::!lJ!>~ sheetjoil1t. ___g~.<2.ove~!.p'§!:l.d

158

Tipe Bundle entrance

.._

Bundle....._exit ..... _.. _--_.-

Shell side . Tube. ~id_e___._ _ _. 53 _... Floating head 54 ..Code reql,lirernel!~ _ _... ASME_<;:ode ~ec VIII Oiv 1 TEMA class B 55 Weight/Shell 847 Filled with water 2000.5 Bundle 318.9

Iblm=!i.~)

~? _Q§?~~t~:

56 1 Remarks._ __ _ 57 1

.

1

58

, 'C

Ib

Heat Exchanger Specification Sheet 1 Company: 2 Location :

,

3 Service of Unit: 4 Item No.:

Our Reference : Your Reference:

R-900

Rev No.: Job No.: 5 Date: 17/ 22 --192 in 6 Size -..•. 7 Surf/unit(eff.) 626.3 ft2 9 Fluid allocation r!-0_ Fluid name f luid quantity, Tolal

rlj 12 13 14

--.

Type BKU

hor

Connected in

Shells/unit 1

1 parallel

Surf/shell (eff.)

-

Ib/h

Liquid

Ib/h Ib/h

Noncondensable

Ib/h

.<.rC'A m

211522

3393 14872 196650

211522

3393

- - --- -- - - .3393 ... _._

15

".

16 Temperature (In/Out) Dew / Bubble point 17

F

BTu/{lb*F) BTU/(Wh*Fl BTUllb

0.5362 0.016

1.0082 0.398

149.2

928.4

Out Intermediate 00 0.75 10 _.... ...•

101 .53

50.38

Sketch

751

I

I Code

I

I

oX1n~::n

330 2 0.0625

I

I

I

I

4/150 ANSI 1/ 150-------_ ANSI .. / 150ANSI

0.065 __ ~~_Jen9Ih 16 Material CS

ft Pitch 1

I J-)Jbe pattern

Shell cover

in 90

SS304

Channel cover

CS SS304

_~~~b.eet-floating

Impingement protection Ty~Single

seg

Cut(%d)

44

None Spacing: dc 23 .625 Inlet 23 .625

vert

I

Seal type U-bend

in in

Ty'pe Tube-tubesheet joint

groove/expand

Ty'pe Bundle entrance

995

F BTu/(h*ft2*Fl

Tube Side

8/ 150 ANSI

in

0.28

0.003

Clean 310 .51

4 / 150ANSI 4 / 150 ANSI

0018

I

2

290 1

Tks-avg

928.4 42 47.99

0.003 MTD corrected

in

48 Supports-tube 49 Bypass seal ". __ __

Bundle exit

---- Ib/{Ws2)

Tube Side

52 Gaskets - Shell sige Floating head 53

57

0.3262 0.01

I Code

F

_Ba ffle-Iong

50 Expansion iQii}t 51 RhoV2-lnlet nozzle

751

psi

45 Floating head cover SS304 .46 Baffle-crossing

58

0.5242 0.069

CONSTRUCTION OF ONE SHELL Shell Side

41 Tubejype SS304 42 Shell Channel or ~ - - -- bonnet 44 Tubesh~et-stationa!:y

55 Weight/Shell Remarks 56.. .. _.

58.206 0.221

28

ft2*h*F/BTU BTU/h Dirty

3150000 99.82

-

54 Code requirements

0.097 0.013

86.57

0.331 0.093 86.48

I

tUs psi

35 Number passes per shell 36 Corrosion allowance In 37 Connections Size/rating 38 39 in / 40 Tube No. 97Us

269.99 269.99

psi

26 Velocity 27 Pressure d_rop, allow.lcalc.

31

269 .99 269.99

50.663 0.242

CD

24 Latent heat 25 Inlet pressure -
32 33 DesiqnfTest pressure 34 Desiqn temperature

221 220.61

Iblft3

22 Specific heat 23 Thermal conductivi!,y

28 Fouling resisl (min) 29 Heatexchanqed 30 Transfer rate . Service

212.6

F

--, .. __..

18 Density 19 Viscosity 20 Molecular wt, Vap __ __ __ 21 Molecular wt, NC ._-_... _--.- - ..

~

ft2

Tube Side

<;-~1

Vapor (In/Oul)

1 series

626.3

PERFORMANCE OF ONE UNIT Sheil Side

8

-

..__.. _._ - -----

.. ASME Code Sec VIII Div 1 2748.9

Filled with water

TEMA class 6062

Bundle

. ...

B

1733.6

Ib

Heat Exchanger Specification Sheet 1 Company: 2 Location: 3 Service of Unit: Item No.: 4 .. _-_ .._--- 5 Date:

-_._--.-- ---

.__...

Our Reference: Your Reference:

R-910 Rev No.:

12 / 17 ~ Size 7 Surf/uniteeff.)

--_._."- _. __ ._._-_._ .. _------_._--_._ ..

Job No.: in_~lJeBKU

--72

108.7

hor

Connected in

Shells/unit 1

ft2

--- ,

11 Fluid quantity, Total 12 Vapor (In/Out)

108.7


C;TE"Ah'J

3899

. ..

Iblh Ib/h

ft2

Tube Side

5 - 162

-- Iblh

-- --_.

1 series

1 (2arallel

Surf/shell (eff.)


8 9 Fluid allocation 10 Fluid name

13 14

- _.....

.

541 3378

3899

521

F F

261 .7

262.9

Ib/ft3

48.051 0.1 88

0.218 0 .092

0.5501

0.3407 0.011

541 541

Ib/h

15 16 TemRerature (In/Out) 17 Dew / Bubble point 18 Density 19 Viscosity 20 Molecular wt, Vap 21 Molecular wt, NC 22 . Specific heat 23 Thermal conductivity 24 Latent heat .. - - --_..• 25 Inlet pressure (absolut~L. 26 Veloci!X 27 Pressure drop,allow.lcalc. 28 Foulinq resist. (min) 486920 29 Heat exchanqed 93.11 30 Transfer rate, Service 31

~. .

BTU/(ft*h*F) BTU/lb

-

-

100.36

Out Intermediate

",

43 Channel or bonnet 44 Tubesheet-stationary

SS304 SS304

48.09

.

~

__ ._--- ---

__ ..._ -_..

380

...

_ - 2---- - 2 / 150 ANSI 1/ 150 ANSI

1/ 150 ANSI

/ 150 ANSI in Length 6

0.065

ft Pitch 1

_

-_ .. _-- None

Im(2ingement (2rotection vert Cut(%d) 45

S(2acing: dc 23

I Inlet

in in ..

23

T:tee

.--

Ty~e-tubesheet

. TYQe .-.. -.. Bundle entrance 51 _RhoV2-lnlet nozzl~._..... ~22. __ ... _. Tube Side 52 Gaskets - Shell .side 53 _..£ ~()ating head •..__ .. ASME Code Sec VIII Div 1 54 Code re ~ments Filled with water 1818.9 803 .9 55 Weight/Shell

._---'.

in

Tube pattem 90

SS304

-

-- -~ -

t

I

I

Material CS in ._§hell cover Channel cover

Single seg T:te e Seal t}I(2e _ U-bend

F BTUI(h*ft2*F)

t

S.L. .__/~()<:l..~

Tubesheet-floati~

._._

_

7

1/150ANSI 4 / 150ANSI

00 12.75

45 Floating..head cover SS304 46 Baffle-crossing

56 Remarks 57

0.023

0.003

Tube Side

330

Tks-avg

__.

0.398 ....

_.899.3 - ..-... 7_L _~ __ . _ 9.34

Sketch

in

Size/ratinq 38 39 in / 40 Tube No. 44Us 41 Tube type 42 Shell SS304

1.0157

2

1

10

0.19

0.018 899.3

0.003 MTD corrected Clean 299.8

_ She~§l<:!~ . 751 ( Code

F

00 0 .75

56.952

0.5746

0.063 --"- -"--. -....... 1 4~., ? __._ .. H~.. 4. 20.1 ...... _..... _ -_._

psi ftls psi ft2*h*F/BTU BTU/h Dirty

psi

35 Number passes_2er shell Corrosion allowance lQ. r--· In E. Connections

310.54 310.54

I ~JJJillb*F)


32 33 DesignlTest pressure 34 Design temperature

47 Baffle~.lg.f1g 48 .!3.l!P(2orts-tube 49 B:t(2ass seal 50 Expa,:,sion joint

310 .54 310.54 0 .175 0.014

262

joint

-

groove/exeand Bundle exit

__

........

- -...- ..

-- --- ~

Ibl(ft*s2) ...

~.

-

-

-

"-"

..

TEMA --_... _... _class .. _---_ ._.......B.... Bundle

323.4

Ib

I

58

I II

REFLUX ACCUMULATOR Identification


Reflux Accumulator D-500 1

Date:

By:

Principal Function: Accumulate condensed liquid from DC-500

Continuous

Operation:

DC-500 Stage 1 flow

Materials handled:

Quantity (lb/hr): Composition (lblhr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

13,679.77 0.41 220.68 50.38 50.00 54.40 12,833.82 trace trace trace 30.79 trace


Design Data:

Diameter (ft): Volume (ft"'3): Length (ft)

101.8 32.0

3.5 Material of Construction: 12,165.78 Stainless Steel 10

Comments: Pricing and sizing info on Appendix A pg. 171

118

4/9/02 akg


Item

Item # No. Required Principal Function:

Operation:

Reflux Ac Date: RA-5l0 By: 1

4/9/02 akg

Accumulate condensed liquid from DC-51 0

Continuous

DC-510 Stage 1 flow

Materials handled:

Quantity (lb/hr): Composition (lb/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

861.13 0.04 213.85 47.45 40.05 48.53 71.92 0.00 0.00 0.00 0.00 0.00

Temperature (oF): Pressure (psia): Design Data:

Diameter (ft): Volume (ft"' 3): Length (ft)

10.0 28.0 1.5 Material of 7.07 Construction: 5.5

Stainless Steel

Comments: Pricing and sizing info on Appendix A page 171 -

-

-

-

- - - - -- - - - - - - - - - -

119

-

-

-

-



Reflux Accumulator D-61O 1

Principal Function:

Accumulate condensed liquid from DC-61 0

Operation :

Continuous

By:

DC-610 Stage 1 flow

Materials handled:


31 ,877 .24 0.00 0.00 0.00 0.00 0.00 22.03 1,974.66 18,527.79 163.64 7,876.99 2,872.85

Temperature (oF) : Pressure (psia):

Design Data:

Date:

Diameter (ft): Volume (ft/\3): Length (ft)

275 .2 95 .0

5 Material of Construction: 373.83 Stainless Steel 20

Comments: Pricing and sizing info on Appendix A pg . 172

120

4/9/02 akg




Date: By:

4/9/02 akg

Principal Function: Accumulate condensed liquid from ST-800

Continuous

Operation:

Materials handled:

I

ST -800 Stage 1 flow


1,633.55 trace 0.00 0.00 0.00 0.00 3.52 293.40 784.07 5.13 107.27 0.88


Design Data:

Diameter (ft): Volume (ft"3) : Length (ft)

182.0 25.0

1.5 Material of Construction: 8.83 Stainless Steel 6 I

Comments: Pricing and sizing info on Appendix A pg . 176

121



Reflux Accumulator D-810

Date: By:

1


Continuous

Operation:

DC-810 Stage 1 flow

Materials handled:

878.35


trace 0.00 0.00 0.00 0.00 3.35 229.90 174.07 2.39 29.35 0.00 167.6 22.0


Design Data:

Diameter (ft): Volume (ft A 3): Length (ft)

1.5 Material of Construction: 6.66 Stainless Steel 5.5


122

4/9/02 akg




Date:

By:

4/9/02 akg


Continuous

Operation:

Materials handled:

DC·900 Stage 1 flow


4,795.92 ,

0.00 0.00 0.00 0.00 0.00 4.95 423.97 3,435.12 29.16 462.42 1.02


Design Data:

181.9 25.0

Diameter (ft): Volume (ftA 3): Length (ft)

2 Material of Construction: 25 Stainless Steel 8

Comments: Pricing and sizing info on Appendix A pg. 174 -

123




Date:

By:


Continuous

Operation:

DC-910 Stage 1 flow

Materials handled:

Quantity (lblhr): Composition (lb/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

1,579.23 0.00 0.00 0.00 0.00 0.00 0.00 0.89 1,135.56 0.24 1.78 1.48


Design Data:

Diameter (ft): Volume (ftI\3): Length (ft)

182.0 25.0

1.5 Material of Construction: 6.33 Stainless Steel 5.5


124

4/9/02 akg

Refrigeration Unit Identification


Refrigeration unit RF-520 1

Date: By:

Principal Function:

Cool offgas using glycol-ammonia absorption system

Operation:

Continuous

4/8/02 1 akg

Materials handled:

Quantity (Ib/hr): Composition (Ib/hr): Ethylene Glycol

Temperature (oF):

Design Data:

21,775.00 21775

-10

Heat Duty: 900,000 Btu/hr I I

Utilities:

I I

125

STRIPPER Identification

Stripper ST-800


4/9/02 cp

Date: By: 1

Principal Function:

Separate out the wastewater from the aqueous outlet stream of the decanter

Operation:

Continuous

I I I

Inlet Streams

Materials handled:

S-801

2,161.83

9,262 .68

1,194.31

0.32 145.94 19.51 50.45 8,263 .04 783.42

3.31 293.44 784 .24 5.13 107.31 0.88

234.1 27.4

182.1 25.0

trace 3.63 439 .38 803.75 55.58 6,208.52 784.29 117.5 35.5


Design Data:

S-802

8,295.16

Quantity (Ib/hr): Composition (Ib/hr): Hydrogen Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

Outlet streams S-804 S-803

No. of Trays : Feed Tray: Tray Spacing (ft) : Diameter (ft) : Volume (ft3):

2,161.83

259.4 35.0

12 Average Pressure (psia): 25 2 Material of Construction : Stainless Steel 2 Molar Reflux Ratio: 3.5 1 28

126

STORAGE TANKS


Identification

Storage Tank T-1 1

Date: By:

4/9/02 cp

Principal Function: Holding tank for Acetic Acid feed

Continuous

Operation:

Inlet Stream (S-l 0 1)

Materials handled:

Quantity (lblhr): Composition (lblhr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

21,447.80

21,447.80 I

I


77 14.7

Volume (gal): Retention Time:

Design Data:

357,450.29 Material of Construction: Stainless Steel 1 day


-

-

-

127

4

STORAGE TANKS

Identification


Storage Tank: T-2

Date: By:

4/9/02 cp

1

Principal Function: Holding tank: for Acetic Acid recycle stream (S-l 03)

Operation:

Continuous

Inlet Stream (S-103)

Materials handled: Quantity (lblhr): Composition (lb/hr):

Hydrogen Carbon Dioxide Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

20,743.76 trace

trace

trace

0.006

0.016

< 0.001

366.13 20,377.61


Design Data:


369 .9

98.6

36,032.28 Material of Construction: Stainless Steel 0.5 days


128

,

STORAGE TANKS Identification


Date: By:

Storage Tank T-3 I

4/9/02 cp

Principal Function: Holding tank for Acetic Acid recycle stream (S-1 02)

Operation:

Continuous

Inlet Stream (S-l 02)

Materials handled:

Quantity (lblhr): Composition (lblhr): Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

438.03 trace trace 1.47 < 0.001

0.001 436.55


Design Data:


263.2 20.1

677.07 Material of Construction: Stainless Steel 0.5 days


129



Storage Tank T-4 1

Date: By:

4/9/02 cp

Principal Function: Holding tank for Ethyl Acetate distillate (S-903)

Operation:

Continuous

Materials handled:


Quantity (lblhr): Composition (lblhr): Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid

1.139.31 < 0.001

0.89 1.134.92 0.24 1.79 1.48


Design Data:


175 16.0

54,675.16 Material of Construction: Stainless Steel 14 days


130



Date: By:

Storage Tank T-5 1

4/9/02 cp I I

Principal Function: Holding tank for both Acetaldehyde product streams

Operation:

Continuous

I

Inlet Streams

Materials bandied: Quantity (lblhr): Composition (lb/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid


S-503

10,354.66

2,463.56

trace

trace

5.53

1.30

2.39

0.54

8.07

1.88

4.78

1.09

10,306.52

2,455.29

trace trace trace 27.372

trace

3.456

trace


Design Data:

S-502

101.8

98.3

32.0

30.1

689,753.23 Material of Construction: Stainless Steel 14 days


131



Storage Tank T-6 1

Date: By:

4/9/02 cp

Principal Function: Holding tank for feed to the Acetaldehyde distillation column (DC-500)

Operation:

Continuous

Inlet Stream (S-501 a)

Materials bandied:


105,379.58 0.04 220.69 50 .38 50.00 54.41 12,843.29 1,162.71 2,765.36 865.08 19,808.00 67,559.63

Temperature (oF) : Pressure (psia):

Design Data:


121.8 43.5

162,514.68 Material of Construction: Stainless Steel 0.5 day


132



Storage Tank T-7

Date: By:

4/9/02 cp

1

Principal Function: Holding tank for bottoms stream of distillation column (DC-500)

Operation:

Continuous


Materials bandIed:


92,139.53 trace trace trace trace trace 9.57 1,162.71 4,106.58 163.78 20,051.42 66,645.46


Design Data:


262.7 37.8

152,598.99 Material of Construction: Stainless Steel 0.5 day

Comments: Pricing info on Appendix pg. 199

..

133

r

Pressure valve Identification


Valve V-501

Date: By:

4/8/02 akg

1

Principal Function:

To decrease the pressure of the feed stream to the acetaldehyde separation column

Operation:

Continuous

Inlet Streams

Materials handled:

S-501 Quantity (Ibmol/hr): Composition (Ibmol/hr): Hydrogen Carbon Dioxide Methane Ethylene Ethane Acetaldehyde Acetone Ethyl Acetate Ethanol Water Acetic Acid Temperature (oF): Pressure (psia):

Design Data:

Tray Spacing (ft): Diameter (ft): Volume (ft3):

Outlet Stream

S-501a

105,380.47

105,379.59

0.04 220.69 50 .38 50.01 54.41 12,846.44 1,162.51 2,764.63 865.07 19,807.78 67,558.51

0.04 220.69 50.38 50.00 54.41 12,843.29 1,162.71 2,765 .36 865.08 19,808.00 67,559 .63

120.9 229.9

121.8 43.9

Average Pressure (psia): Material of Construction: Stainless Steel Molar Reflux Ratio:

Utilities:

134

EQUIPMENT COST SUMMARY

EguiQment name

Purchase Cost

DescriQtion

Source

AB-320

Absorber

CP-410

Compressor

C-500 C-520 C-610 C-800 C-810 C-900 C-910

Condenser Condenser Condenser Condenser Condenser Condenser Condenser

DE-720

Decanter

DC-500 DC-510 DC-610 DC-810 DC-900 DC-910

Acetaldehyde Distillation Column Acetaldehyde Recovery Column Acetic Acid Distillation Column Acetone Distillation Column Azeotropic Distillation Column Ethyl Acetate Distillation Column

$986,529 $6,331 $146,510 $10,050 $14,670 $42,210

Cost Cost Cost Cost Cost Cost

F-230

Fired Heater

$260,897

Walas

FV-310

Flash Vessel

$192,900

Cost Charts

HX-200 HX-210 HX-300 HX-530 HX-710

Heat Heat Heat Heat Heat

$83,265 $269,551 $70,009 $4,594 $6,812

BJAC BJAC BJAC BJAC BJAC

P-110 P-540 P-600 P-620 P-730

Pump Pump Pump Pump Pump

$11,570 $11,570 $6 ,171 $5,786 $2,571

Ulrich Ulrich Ulrich Ulrich Ulrich

PB-500 PB-610 PB-810 PB-900 PB-910

Reboiler Reboiler Reboiler Reboiler Reboiler

$3,600 $9,000 $2,186 $2,829 $2,700

Cost Cost Cost Cost Cost

$26,740

Cost Charts

$386,000

Cost Charts

$89,726 $7,094 $27,654 $3,235 $2,863 $3,953 $7,893 $9,000

Exchanger Exchanger Exchanger Exchanger Exchanger

Pump Pump Pump Pump Pump

135

BJAC BJAC BJAC BJAC BJAC BJAC BJAC Cost Charts Charts Charts Charts Charts Charts Charts

Charts Charts Charts Charts Charts

EguiQment name

Purchase Cost

Description

$4,243 $2,571 $7,071 $2,571 $2,057 $3,986 $2,057

Pump Pump Pump Pump Pump Pump Pump

Source Cost Cost Cost Cost Cost Cost Cost

Charts Charts Charts Charts Charts Charts Charts

PR-500 PR-510 PR-610 PR-800 PR-810 PR-900 PR-910

Reflux Reflux Reflux Reflux Reflux Reflux Reflux

RX-240

Reactor

$16,710

Cost Charts

R-500 R-610 R-810 R-900 R-910

Reboiler Reboiler Reboiler Reboiler Reboiler

$65,581 $53,987 $4,538 $6,632 $3 ,735

BJAC BJAC BJAC BJAC BJAC

0-500 0-510 0-610 0-800 0-810 0-900 0-910

Reflux Reflux Reflux Reflux Reflux Reflux Reflux

$5,190 $2,080 $11,680 $2,340 $2,210 $2,725 $2,210

Cost Cost Cost Cost Cost Cost Cost

RF-520

Refrigeration System

ST-800

Stripper

T-1 T-2 T-3 T-4 T-5 T-6 T-7

Storage Storage Storage Storage Storage Storage Storage

Accumulator Accumulator Accumulator Accumulator Accumulator Accumulator Accumulator

$213,675

Tank Tank Tank Tank Tank Tank Tank

136

Walas

$11,670

Cost Charts

$25,710 $11,570 $1,543 $25,710 $66,860 $28,290 $25,710

Cost Cost Cost Cost Cost Cost Cost

$3,331,384

Total Purchase Cost



Fixed Capital Investment Summary The bare module cost of equipment was determined using cost charts that can be found in Ulrich. The purchased cost of each piece of equipment was determined by the charts. Then, each piece of equipment was multiplied by the appropriate bare module factor based on operating pressure and materials of construction to find the bare module cost for each piece of equipment individually. The total bare module cost was determined by summing the individual bare module costs. Nearly all of the equipment was available in charts from which the purchase cost could be read, and then mUltiplied by the appropriate factor to find the bare module cost. The exceptions to this were the heat exchangers, the fired heater, and the refrigeration unit. We used B-lAC to design the heat exchangers, including the condensers and reboi1ers . B-lAC rigorously designed the heat exchangers and also returned an estimated cost of material and labor. For heat exchangers, Ulrich estimates that this cost is 2.34C p , and the bare module cost is 3.18 Cpo Assuming similar escalation in prices for our equipment, the ratio of bare module cost to installed cost equals 3.1812.34 = 1.36. The cost of the heat exchangers designed using B-lAC was multiplied by 1.36 to estimate the bare module cost. The costs for the refrigeration unit and fired heater were estimated using equations found in Walas. These equations calculated the installed costs for these pieces of equipment. Assuming similar ratios for the installed costs of these pieces of equipment as Ulrich provides for heat exchangers, the ratio of bare module cost to installed cost for this equipment is also 1.36. Estimates for pump costs were determined from cost charts provided by Ulrich. The pump power was taken from the Aspen Plus output for stand-alone pumps, and from IPE equipment sizing for reflux and reboiler pumps. The output this program provides for individual equipment is its installed cost. The large storage tanks were also cos ted llsing cost charts

137

available in Ulrich. Using the factors provided, the bare module cost could be determined directly. By using this method to determine the equipment bare module costs, and adding $5,979,000 for the catalyst (see Appendix for calculations), the total bare module cost, CTBM , was calculated to be $20,047,306. Table 8 on p. 139 summarizes the calculations involved in determining the total permanent investment. It was estimated that 5% of the total bare module cost should be set aside for each site preparation and service facilities. Allocated utility faci lities for cooling water and steam were build, at a total cost of$4,387,000 (see Appendix B, p. 203). These additional costs are added to the bare module cost to produce the direct permanent investment, which equals $26,439,037. An estimate of 15% of the direct permanent investment is set aside for contingencies. Adding this to the direct permanent investment yields the total depreciable capital, $30,404,892. Two percent of the total depreciable capital is then set aside for land costs, and 12 % for startup costs. This allotment for startup is slightly higher than normally suggested, but we believe it is warranted because of the complexities of our process and the many recycle streams that must be accounted for. Adding the startup and land costs to the total depreciable capital produces the total permanent investment, $34,661,557.

138

Table 8. Total Permanent Investment Total Bare Module Cost, C_TBM

$20,047,306

Cost of Site Preparation, C_Site Cost of Service Facilities, C_serv Allocated costs for utilities, C alloc

$1 ,002,365 $1,002,365 $4 ,387,000

Direct Permanent Investment, C_DPI

$26,439,037

Cost of Contingencies, C_cont

$3,965,855

Total Depreciable Capital, C_TDC

15% of C_DPI

$30,404,892

Cost of Land, C_land

Cost of Royalties, C_royal

Cost of Start-up, C_start

$608 ,098 $0 $3,648,587

Total Permanent Investment, C_TPI

$34,661,577

139

Ii

5% ofC TBM 5% ofC_TBM

2% ofC TDC 12%ofC_TDC

140

Important Considerations Acetaldehyde is an extremely flammable liquid and vapor. Its vapor may cause flash fires. It fonns explosive peroxides and polymerizes, resulting in hazardous conditions. Acetaldehyde is therefore stored in stainless steel tanks with a refrigerating system to ensure that the temperature of the product does not rise above 60 OF. This is why is important to have a refrigerated storage tank for the combined acetaldehyde product. Acetaldehyde is also a potential cancer hazard. High vapor concentration may cause drowsiness or irritation of the eye and respiratory tract. For eye protection, safety glasses with side shields and a face shield need to be worn by the workers at this plant with risk of exposure. Additionally, chemical resistant gloves, boots and protective clothing appropriate for the risk of exposure need to be worn. Decontamination facilities such as eye bath, washing facilities and safety shower must be provided. Acetic acid is strongly corrosive and causes serious bums. At temperatures above 102 OF explosive acetic acid vapor/air mixtures may be fonned. In order to prevent such hazards, there should be no open flames, no sparks and no smoking in the premises. Also, above 102°F, a closed system needs to be used as does ventilation, and explosion-proof electrical equipment. Although there is no evidence of acetic acid having carcinogenic, mutagenic or teratogenic effects, acetic acid is a lachrymator. Prolonged exposure to acetic acid causes sore throat, cough, headache, dizziness, shortness of breath and labored breathing. Workers with potential exposure to acetic acid need to be provided with protective gloves, protective clothing and breathing protection. Leaking acetic acid liquid must be collected in sealable containers and cautiously neutralized with sodium carbonate. Acetic acid is hannful to aquatic organisms and therefore it must not be disposed into water bodies without adequate treatment and/or dilution.

141

Hydrogen is even more flammable then acetic acid and it undergoes many reactions with air, oxygen, chlorine, fluorine, strong oxidants that cause fire or explosions. Exposure to hydrogen also causes dizziness, asphyxia, labored breathing and unconsciousness. Therefore, in addition to the safety precautions that need to be taken for acetic acid, hydrogen gas cylinders must not be handled with oily hands and must be stored in a cool place. In case of spillage, the danger area must be evacuated and the vapor must be removed with fine water spray. Because of the dangers associated with storing hydrogen, we receive our supply via a pipeline. Another aspect taken into consideration was that the furnace operates at temperatures around 600°F. Therefore, steps must be taken to ensure that faults in the process do not make it necessary for the entire process to shut down since it will be very economically unfeasible and wasteful to have to shutdown and restart the furnace, especially since it will take an extended period of time to reach the desired temperature again. Thus, there is a storage tank for the reactor effl uent before it is fed to the acetaldehyde distillation column. If other parts of the system fail, the furnace can still operate and feed its product to that tank. It would be more beneficial to have a storage tank immediately following the reactor, but the high temperature and high hydrogen composition makes that unfeasible. There will also not be difficulty with a supply of feed to the furnace if other systems break down, since the acetic acid and hydrogen feedstocks can be fed virtually directly to the furnace if it is necessary to keep the reaction proceeding. Also, there is a storage tank for the bottoms of the acetaldehyde distillation column. This allows the acetaldehyde recovery section and the acetic acid separation section to operate if the other experiences difficulties and must be shutdown for a short time. Startup is a special concern for this facility because ofthe importance of recycle streams to the operation of the absorber AB-320 and the acetic acid distillation column DC-610. A tank

142

holding acetic acid should be positioned near the absorber to provide solvent to the top stage during startup. This stream is usually furnished from the bottoms product of the acetaldehyde distillation column, but that will not be operating at the beginning of the process. Ethyl acetate must also be purchased and stored so that it can be used to form the azeotrope in the acetic acid distillation column. Aspen simulation results imply that without an initial charge of ethyl acetate to this column, there is no phase separation in the decanter DE-720, and no ethyl acetate product is recovered. More energy in the form of natural gas must also be supplied at startup. This is partially because of the need to heat a cold furnace, but also because there are no waste streams that can be burned for fuel, and there is no hot reactor effluent to preheat the reactor feeds. Because waste streams are used for fuel in the furnace, careful control is necessary to ensure that small irregularities in process conditions do not lead to either excessive or insufficient heating in the fired heater. Plant-wide control is also a major issue in this complicated design. Controls should also be placed before the compressor CP-41 0 in order to ensure that the entering stream will be only vapor. If the feed stream is cooled below its dew point, a valve may open to reduce pressure and vaporize the entire stream. This would increase the duty on the compressor, but is necessary for its long-tenn operation. There is similar attention paid to ensuring that the feed to the recycle pump P-730 is entirely liquid. The distillate of the near azeotrope distillation column DC-900 is subcooled to limit the chances that the pressure drop associated with the mixer would partially vaporize the feed to the pump. The composition of the stream should be monitored, and ifthere is any vapor a small cooling jacket can be used to decrease the temperature and produce a total liquid.

143

The amount of acetic acid and hydrogen feeds, as well as their ratio must also be controlled, for two reasons. First, the plant design is optimized for the flow rates that were used; if the amount of either feed changed substantially, then unexpected difficulties may result when the effects of recycle streams are considered. Second, in order to keep the proper oxidation state for the catalyst, it was determined that a hydrogen/acetic acid mole ratio of 511 is optimal. If this is not maintained, then the performance of the catalyst may degrade quickly.

144

Operating Cost and Economic Analysis The Economics Spreadsheet developed by Holger Nickish was used to evaluate the process. Two different scenarios were considered in evaluating the economic viability of this design process. In the first, the acetic acid feed was available at $0.161Ib. In the second case, legislation to eliminate MTBE from gasoline created a glut of methanol, which can be used to produce acetic acid. In this situation, the cost of acetic acid is $0.12/Ib. Besides these costs (and the associated change in the working capital), all costs are the same under both scenarios. The case in which acetic acid is available at $0.16/Ib is considered first. The annual costs associated with operating the plant under these conditions are summarized in the Fixed Costs and the Variable Costs tables on pages 146 and 147. Heuristics for calculating the annual costs are based on the cost sheet outline provided in Table 10.1 of Seider, Seader, and Lewin. We do not need to purchase the steam and water utilities because we built the dedicated facilities and assigned the price to allocated costs, part of the Direct Permanent Investment. Costs for natural gas, electricity, and wastewater disposable were supplied by Fabiano and Vrana. We assumed three operators per shift, each earning an annual salary of $40,000. The major fixed costs we encountered stemmed from the wages and services for maintenance. The total maintenance costs amount to $2,447,000/year. The cost for replacement catalyst is also considered here. $543,500 per year is set aside for the catalyst, which we assume we must replace every five years. The variable costs are based primarily on the cost of the hydrogen and acetic acid feedstocks. Acetic acid is especially expensive, costing $0.27 per pound of acetaldehyde produced. Because of the allocated facilities for stean1 and cooling water, the utility costs are

145

Fixed Costs Acetaldehyde Production. Acetic Acid $0, 16/1b April 9, 2002

TOTAL

Operation IWages and Benefits

- - -$6-:-:0-0-,0-0-0""

Direct Salaries and Benefits $90,000 Operating Su plies an _ d_S_e_rv__i_c e_s__ _ _ __ __ _ __ __ $36,OQ~ Tec hnical As~~sta~ce=___t.:..::.o.:..::.M .:..::..:.:..: an::::.::u:..:. fa::::.::c:..:. tu.:..::.r_= in::£ g'_____ __ __ __ _ __ ____'$::...::5 2 ,000 $57,000 Control Laboratory

Maintenance \vageSandBene~~_ _ __ __ _ _ __ __ _ __ _ _ ~$~ 1,~0_64~,~00_0~1' Salaries and Benefits Materials and Services Maintenance Overhead

$266,000 . $ 1,064,000 $53,000

Operating Overhead General Plant Overhead ----~~----------Mechanical De artment Services Employ~~. Relations Department Business Services

--- ---

Overhead:

146

_

_

.. ~143,000 $48,000 $11 9,000 $149,000 I

Variable Costs

Acetaldehvde Production. Acetic Acid $0,16I1b

TOTAL

April 9, 2002

Raw Materials

147

only $0.005/lb of acetaldehyde. For the production level used in this plant, the annual amount of variable costs is $31,009,000. The working capital was determined by assuming a 14-day supply of the products acetaldehyde and ethyl acetate, and a one-day supply of acetic acid. This supply can be so low because our site is shared with a major chemical company. Hydrogen is piped directly to the facility, so it is not stored. We also hold 30 days of accounts receivable to account for payment occurring monthly. Additionally, a spare charge of catalyst is held because it is a special catalyst that could not be ordered quickly if its performance declined. The total working capital for this process is $12,580,684. This is added to the total permanent investment (TPI) to find the total capital investment (TCI). The TCI is $47,242,990. A summary of the steps taken to determine the TPI is found in the Venture Guidance Appraisal on p. 149. Finally, the profitability of this design was examined. The return on investment (ROI) in the third year is 11.4%. Investor's rate of return (IRR) and the net present value (NPV) were calculated based on a cost of capital of 15 %. Using a five-year depreciation cycle and a 20-year plant life, the IRR is 11.1 % and the NPV is -$5 ,830,000. The annual cash flows are presented in the table labeled Cash Flows on p. 150. Clearly, construction should not proceed under these conditions.

148

Venture Guidance Appraisal Acetaldehyde Production, Acetic Acid $O.16/1b April 9, 2002

TOTAL

Working Capital Inventory IAcetaldehyde Ace,tic Acid H yd~'ogcn

Total Inventory: Accounts Receivable:

3,891,000 Ibs 465 ,070 Ibs Ibs

$ 1.868,000 $74,000 1 SO

$1 ,942,000 I 30 days

149

S4,430,000

or,:..,.'

Cash- Flows .~

~

l/$ · '!,.CJ

.l;

o

0\0

~

~ ., I. ~ /'/'/' /'~. . ~ ~

~,

:1:fJ;ll.'

T

~. ~.,1

Acetaldehvde Prodllction.Acetic Add '$n.t.6Llh

Apri l 9, 2002

~

~

0" (j ~ .~

~ I'.-'t:i

-J

v

.~

v ~

tf

$

.$

~O::,,'ri

vO

",0

$

~ ~

" tf

~

(>0

,c::-

vo.~ ~ q,(>

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.
0

.§

!;

.,
V'l';"'';:J'''-~

,,'&

/

~? ~~·;i~~~ ~~~F "

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...

v'ri

...... ~'ri

.

~q,

4.

.

~

.

•.:.q,

c::-

~

of

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d

=

($11,554,000)

($11,554,000)

($11,554,000)

($21,601,000)

($24.135.000)

($24,13~~

($39,851,000)

$3,233,000

($37,725,000)

($3.699.000)

__ _

/'

~

($11,554,000)

($11.554,000)

.. $7,221.000 .- -".-,,-- ..... . _ J~~~ ~~~~!OOO) $9,523.000 ($28.861,000) ._----_.__ ..._---. -----_... _....._..•.... _-_. ($25,170,000) $4,545,0~~~ _ _ $~,538.000

i~3,8!_1..:?9_~) $2.868,000 -_._

1'1--'--'- -'---' 11

0'0

~

~

,,'ri q, ~ 0

,

'f

~

~~~~~~~~~FJ~~-----iH~~:~~~ II ~:~i~~~:~6~1

_~.!.~OOO

$7.061.000

I_ -:;::--:-'-:-::..::..:.::..:.:::...••_~'~_~ .,~.. ~61.000

$ 7.061.000"

-

($17,403,000)

----_.

($15,658.000)

$7.061,000

$7,061 ,000

$7,061.000 I $7.061 ,000

$7,061. ,-,000- t----i~~~.820.:...000)" $7.061.000 ($11,672,000)

$7.061.000

$7.061.000

($10,674,000)

$7,061,000

$7,061,000

($9.806,000)

$7,061 ,000

$7,061 ,000

($9,051,000)

$7,061,000

$7,061 ,000

($8,395,000)

'i:7 nR1 non

-;.

,

;~.i"'~ 1 ~~.

..,,; 1:Jl:'" 1.

"'-'

($14,1 40.000)

$7,061,000

$7,061,000

$7,061,000

$7,061,000

$7,061 ,000

($6 ,897,000)1 _

$7,061,000

$7,061,000

($6,522,000)

'1:1<1 Qil7 nnn

$14,987,000

($7,328.000)

-I

Our group also examined the economic viability of the process under the conditions of acetic acid being available at $0.12/Ib. The input summary for this case is presented on pages 152 and 153. The annual costs associated with operating the plant were calculated in the same manner as they were in the first scenario. The results are summarized on the pages 154 and 155 in the Fixed Costs and Variable Costs sheets. Under both circumstances the total fixed cost sums to the same amount: $4,740,500. The variable cost does change dramatically, however, as acetic acid costs only $0.20/1b of acetaldehyde formed, rather than $0.27/Ib as in the first case. This result leads to a savings in raw material costs of nearly $7,000,000/year, the costs decrease from $30,290,000 to $23,495,000. Other variable costs were not affected by the acetic acid price. The working capital is affected somewhat by the lower price of acetic acid because the one-day supply of acetic acid is not worth as much when acetic acid is less expensive. Thus, the amount of working capital required for the supply of acetic acid decreases from $74,000 to $56,000. The working capi tal under these circumstances is $12,562,684, and the TCI is $47,224,990. These results are summarized in the Venture Guidance Appraisal on p. 156. The economics of this process was analyzed using the same metrics used to examine the first scenario. As a result of the substantial decrease in variable costs, the ROI in the third year improved to 19.5 %. Using the same five-year depreciation schedule and 20-year plant life as before, the IRR is 18.5 % and the NPV is $12,162,000. The annual cash flows are summarized in the table Cash Flows on p. 157. The economics of this process is strongly dependent on the cost of acetic acid. If acetic acid is available at $0.12/Ib, then it is profitable to follow this design. The rate ofretum is not significantly higher than the cost of capital (15 %), so the potential reward for building this plant would be relatively small. Thus, more research should be done to ensure acetic acid can be purchased at the lower price before production proceeds.

151

Input Summary April 9.1001

- - - -- -- - - - -- - - -- - - -_....

General Information

__ - - - ..

Title of Process: Acetaldehyde Production, Acetic Acid $0.12/1b Plant Site: Gulf Coast Startil1g Year: 2002 Years of Design: 1 Years of Conshl.lction: 2 Years of Plant Life: 20 2005 First Year of Production:

Product Information _ _ __ __ __ _ T_h_e p. rocess yields a singLe product:

Acetaldehyde

---------------

C apacity Operating Hours p er Year: The Process will Yield:

7,920 12,818.22

lb per hour

101,520,287

Ib per year of Acetaldehyde

- - - - - _ ... _-

Market Price 0.4800000

The Price per Ib of Acetaldeh yde is:

Equ ipment C osts

s

IBL TOTAL BARE MODULE COST Total Capital Investment

20,047,306

of Total Bare Module Costs for Site Preparation and Service Facilities: to .OO ~/o Allocated Utility and Related Facility Costs (see Table 9.4): 54,387,000 Percentagc of Direct Pel1lJi1l1ent Investment for Contingencies: 15.00 % 2.00 % Enter either a dollar value or a percentage ofTowl Depreciable Capital: Percentage of Total Depreciable Capital for Roya lties: % Percentage ofTota.1 Depreciable Capital for SUitt-Up: 12.00 % Site Factor (see Tablc'_9_._5'):_ _ __1.00 _ _ _ _ __

Working Capital Inventory will be kept of the follO\ving Materials: Acetaldchyde: 14 days 4,306,921 Ib Acetic Acid : 1 days 514,748 lb Accounts Receivable: 30 days Other Working Capital Items : 1. Catalyst Charge $ $ ._ .._ _ _ _. . _ . _ . 2. Ethyl Acetate-14 days _ _ __

5,979,000 229.684

Raw Materials Ib Acetic Acid per lb Acetaldehyde:

1.6732300

lb H '~~~.}2~1 P2~ !b Acetaldel~.y'de: . (~QQ..~~OO

Cost ($) per Ib Acetic Acid: _Cost ( S~2erlb!-l.2:'ir~g~1~_

0. 1200000 0.5000000

Utilities MMBnl Natural Gas per Ih Accr:aldehyde: 0.0005261

Cost per MMBtu Natural Gas: Cost per kWh Electricity: Cost per lbor~ Water !re~ trnent:

kWh Electricity per Ib Acetaldehyde: 0.04.16670 org\\i~t~rT r~~Ll!l.~!1tper

Jb AcetalctehY0~:

O~~780 140

Other Variable Costs Selling/Transfer Expense: Direct Research: Allocated Research: Administrative Expense: Managemcllt Incentive Compensation:

3.00 % ofsalcs 4.80 'Yo of sales 0.50 % of sales 2.00 % ofsales 1.25 ~~) of sales

152

2.3000000 0.0350000 0.0300000

1.25 % of sales

Management Incentive Compensation: PackHging Labor: M aterials:

0.00 per Ib Acetaldehyde 0.00 per lb Acetaldehyde

Byproducts lb Ethyl

Acetat~per

lb Acetaldehyde:

0.0888820

Price per lb Ethyl Acetate:

$0.6000

Fixed Costs Operations Number of Operators per Sh 3 Annual Wages per Operator: $40,000 Employee Benefits: Direct Salaries and Benefits: 15 'a ting Supplies and Selvices: 6 $52,000 TechIlical Assistance to Mar Control Laboratory: $57,000 Maintenance Wages: 3.50 Employee Benefits: Salalies and Benefits : 25.00 Materials and Services: 100.00 Maintenance Overhead: 5.00 Operating Overhead General Plant Overhead: 7.10 Mechan.ical Department Sep 2.40 loyee Relations Department: S.90 Business Services: 7.40 Property Taxes and Insurance roperty Taxes and Insurance 1.50 Depreciation Direct Plant 8.00 Allocated Plant 6.00 Catalyst Replacement ~.a.~~yst Rep!aCC1n~~.~_._ S_4_3-',S -_0_0_.0_0_

(assuming 5 Shifts) Including Benefits % of wages % of wages % of wages per labor year per labor year Including Benefits % of Total Depreciable Capital, % of wages % of Maintenance Wages and Benefits % of Maintenance Wages and Benefits % ofI'vlaintenance Wages and Benefits % % % %

of Mainlenance of Maintenance of Maintenanee of Maintenance

and and and and

Operations Operations Operations Operations

Salaries, Wages Salaries, Wages Salaries, Wages Salaries, Wages

and Benefits and Benefits and Benefits and Benefits

% of Total Depreciable Capital % of Total Depreciable Capital % of Allocated Costs

$c...I-"'y_e_aT_ _ __ _ __ _

Financial Information Cost of Capital:

15.00 %

GeneTallnflation Rate :

% % % % 37.00 %

Product Price Inflation Rate: variable Cost Inflation Rate: Fixed Cost Inflation Rate: Income Tax Rate: MACRS Tax-Basis YEAR 1 YEAR 2 YEAR 3 YEAR 4 YEAR 5 YEAR 6

Depreciation Schedu le 20.00'Yo 32.00% 19.20% 11 .52% 11 .52% 5.76%

Distribution of Investment

153

I

DLSI(]N I

33 ~o

CONSTRUCTION I

33%

CONSTRUCTION 2

33"10

Fixed Costs Acetaldehvde Production. Acetic Acid $0. l21lb April 9, 2002

TOTAL

Operation Wages and Benefits Direct SalaJies and B-' e-.n-e-fit-s- - - - -_- - . _- _._-

$600,000

- s90,oooJ

-

,Operatin o Supplies and Services [Technical As~;stance to Manufacturing

$36,0001 $52 ,000 !

!-=IC-.::.-=on~ol tr.:..;,.:..:L ;";,,a-=-b:..:.ra o=-=-,;,.:.. to r-'-y'---'-.:..:..:....=..=..:.~c-=-~"'----------$·57,000 -1

ITotal Operations:

, J(

,

'

$835,000

$835,000

Maintenance Wages and Beneiits i ~_al~Ei~~~nd B=-e__r-'w-'. fi_ts_ _ __ Materials and Services Maintenance Overhead-- -

I

S 1,064,-000 . ____ $266,000 S 1.064,000

$53,000 I

$3,282~000 1

aintenance:

I

Operating Overhead iGeneralPiant Overhead Mechanical Deparlrrl~nt Services Employee Relations Department Business Services

I

$3741,000

head: IJ'r.n.n ,o r t ... ,

T axes and Insurance:'

$4,197,000! $4,740,500 I

154

Variable Costs Acetaldehyde Production. Acetic Acid $0,12/1b

Aprij 9. 2002

IAcetic Acid

TOTAL 20 ,08¢ per Ib Acetaldehyde --~--------3,O/¢ per Ib Acetaldehyde

------------~~,

IHydrogcn

Total Raw Materials:

23.J 4¢

pel' Ib Acetaldehyde

$23,496,O(fO

$23,496,000

Utilities , N3tur~ _SJas

O. 12¢ O,lS¢ O.23¢ O,QO¢

__

-lectriCiiY

~

W~~er Treatment Eleetricitv

it~i

ITotal;Utilities:

O.SO¢

pcr Ib_~~etal<:lehyde per Ib Acetaldehyde

per Ib Acetaldehyde per Ib Acetaldehyde

_

,__ ___ I

per Ib .Acetaldehyde

$508,000

BVDroducts

IEthyl Aceta-;-

(S. 33¢) per Ib Acetaldehyde

--(5.iJ¢)

jTotal Byproducts:

perlb Acetalde,h yde

Other Variable Costs r-

I __ ~241j 904,OOO I

Sellin_g:Trallst~rF~p(;n~e

Direct

R csear~l

:\IIDcalcd Research AuministrJlive bpense \ ·18nagement

C o m2en3~.?n

, Pacbg~~~ ~~at.:rial,~

Packaging Labor

;1

($5,414,000) 1 I

,

1.44¢ per Ib Acetaldehyde

_ _ ___ ~} O¢ per lb Acetaldehyde

O.24c

pCI'

Ib

Acctaldehx~,~_

O,96¢ J~_e~~ ~el:Jld.ehyd 7__

O.60e per Ib Acewldehydc

OOO¢ per lb O.OO¢

Al'CIaldchy~e

155

$18,590,000

Venture Guidance Appraisal Acetaldehyde Production. Acetic Acid $O.12/1b April 9, 2002

Working Capital

Accounts Receivable:

30 da~s._ _ _ __ _ _$_4---',4_3_0,'0_00_1

$5,979,000 $229,684 $6,208,684 $12,562,684

156

:Cash Flows 14. l:.;...

." " f-pl'll ~1; 2002 ,

~

1-

"

I

it', gj

., .~

.,

,'"

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158

Conclusions and Recommendations We have developed a method to produce 100,000,000 pOlmds per year of acetaldehyde '.

by the hydrogenation of acetic acid over a palladium-iron oxide catalyst, as described in the patent filed by Eastman Chemical. The acetaldehyde is recovered by first absorbing it with an acetic acid-rich solvent, then separating the acetaldehyde from water and acetic acid in a distillation column. In order to attain high recovery of the low boiling (b.p.

=

70 OF)

acetaldehyde at the purity required for sale, the vapor distillate from the primary acetaldehyde distillation column is fed to a smaller column with a condenser operating at 10 °F that condenses the acetaldehyde while allowing lighter gases such as carbon dioxide, methane, and ethylene to escape. Large amounts of both hydrogen and acetic acid can be recycled to the reactor in order to minimize the amount of fresh feedstock that must be purchased. Ethyl acetate, which forms as a by-product in the acetaldehyde distillation column can be purified and sold, generating approximately 12 % of the sales revenue. The profitability of this facility is very sensitive to the price of acetic acid. If the price of acetic acid remains at its current level of $0.16/Ib , then this design would not be profitable and should not be pursued. If the price of acetic acid decreases to $0.12 /Ib, there is an opportuni ty to profit from manufacturing acetaldehyde by the process we have described. Further studies are needed to project the market for acetaldehyde and whether we will be able to sell the $100,000,000 pounds per year we produce. In addition, there should be a study to determine the probable price of acetic acid in the near future. If acetic acid can be purchased as cheaply as $0.12 /Ib and the market will support the introduction of 100,000,000 Ib/yr of acetaldehyde, then

we recommend implementing this process for the production of acetaldehyde.

159

160

Acknowledgements

We would like to express our appreciation to Prof. Leonard Fabiano, our advisor, Dr. John Vohs, our faculty advisor, and Dr. Bruce Vrana, who gave us this problem, for helping us and guiding us with this design project. We would also like to thank the following people who also helped us with our design project: Dr. Warren Seider Mr. Miles Juilian David Kolesar, Rohn & Haas Dr. Frank Petrocelli, Air Products and Chemicals Mr. Henry Sandler Mr. John Wismer, Atochem North America Dr. Rob Becker, Environex Dr. Wen Hsieh All Industrial Consultants Fellow Students

161

Bibliography Agreda, Victor and J.R. Zoeller Ed., Acetic Acid and its Derivatives, Marcel Dekker, New York

(1993).

Eastman Chemical product safety infonnation. http://www.eastman.com.

Kirk-Othmer Encyclopedia of Chemical Technology, 4th ed. Wiley, New York (1991).

Levenspiel, Octave. Chemical Reaction Engineering, 3rd ed., Wiley, New York, (1999).

McKetta, John J. Ed. Encyclopedia of Chemical Processing and Design. Marcel Dekker, New

York (1997).

Perry, R.H. and D.W. Green, Ed., PeID's Chemical Engineers' Handbook, 7th ed. McGraw-Hill,

New York (1997)

Peters, M.S. and K.D. Timmerhaus, Plant Design and Economics for Chemical Engineers, 4th

ed., McGraw-Hill, New York (1991)

Seader, J.D. and EJ. Henley, Separation Process Principles, Wiley, New York (1998)

Seider, Warren D., J.D. Seader, and Daniel R. Lewin. Process DesignPrinciples,Wiley, New

York (1999).

Tustin, G.c., et a1. "Method for Producing Acetaldehyde from Acetic Acid." U.S. Patent No.

6,121,498.

Ullman's Encyclopedia ofIndustria1 Chemistry Online.

Ulrich, G.D., A Guide to Chemical Engineering Process Design and Economics, Wiley, New

York (1984)

Walas, S.M., Chemical Process Equipment, Buttersworth, London (1988)

162

£91

SNOI.LV'ln:)'lY:) .LSO:) .LINn

:y XIUN:tIddV

164

Current CE

=405

C~002:= 405

CE I982 := 315

COMPRESSOR CP-410 Powernet := 443.8hp Powernet = 330.942 kW

11 := 0.72

Power

Power:= net

0.72

Power = 459.641 kW

From Cost Charts, Cp in 1982

= $280,000

C~002 C p := 280000·-- CE 1982

C p = 3.6 x 10

Cp

5

= $360,000

F BM := 7.3

C BM := FBM·C p

C BM = 2.628 x 10

6

C_BM = $2,628,000

DISTILLATION COLUMN DC-500 Use Fenske-Underwood-Gilliland Method to determind stages, reflux ratio . Fenske method for minimum stages:

165

d·1

=moles of light key (acetaldehyde) in distillate

=

d moles of heavy key (water) in distillate

j

b j

=moles of heavy key (water) in bottoms

bi

=moles of light key (acetaldehyde) in bottoms

a

=relative

volatility of light key and heavy key at average temperature

d j := 291.3229

b'= J . 1113 b i := 0.21 7

a := 2

j IOg(di . b ;

d·J b·I

Nmjn := -J"O"og....::,(a-)~

Nmin = 19.737

Underwood method to find minimum stages

J

dj i _ d - afeed·( _ Xj.feed l).feed Lmin - ....0.-_ _ _ _ _- - " - _ - " afeed - I

Xj .feed := .112

l) .feed := 0.423

166

To find relative volatility of the feed, use the geometric mean of the relative volatilities on equilbrium stages 27 and 28.

CX

feed := (3· 13) 2

CX feed

= 6.245

J

(

d,I d·J - - - cxfeed'- xi.feed l).feed

Lmin :=

cxfeed - 1

Lmin = 491.106

D

= moles of distillate

D:= 304 .8

Lmin = 1.611

o Rmin

:= 1.61 I

R:= 1.3·R min

R = 2.094

At 1.3 times the minimum reflux ratio, the actual number of required stages can be determined by the Gilliland Correlation.

R - Rmin X:=

R+I

X=0.156

y=

N - Nmin

N+ I

y.= I - exp

1 + 54.4· X ) .[X ---I [( I 1+ 117.2·X XO.5

J]

167

Y = 0.499 Y + Nmin N := - - - 1-Y

N = 40.422 The actual conditions used in the simulation was a reflux ratio of 2.40, with 40 equilibrium stages.

SIZING AND COSTING DISTILLATION COLUMNS

These calculations were done using Excel spreadsheets. The following explanation outlines the equations and assumptions used in performing the calculations. As a first step to finding the dimensions of the column tower, the flow parameter (FP) was calculated from the values of the liquid and vapor flow rates in the top stage of the column and the liquid and vapor densities which we got from the Aspen simulation of our process. Additionally, the surface tension of the liquid gives us the flooding velocity. We assumed a tray spacing of 24 inches (61 Omm) Using the known variables for the vapor flow rate, flooding velocity and the density of the vapor phase, the diameter of the column was determined from the following equation :

Where: D = Tower diameter

V = Vapor mass flow rate

p = Density

U = Velocity = 85% of flooding velocity

Ib V:= 151800·

hr

1b

P v := 0.464·

ft3

m

U:= 1.16·

s

D = 10.3·ft

Since towers are fabricated in increments of 0.5 ft., the calculated diameter of 10.3 ft. is rounded up to 10.5 ft.

168

The tower height was computed by multiplying the number of trays with the tray spacing and allowing a 10-ft high bottoms sump below the bottoms tray and a 4-ft disengagement height above the top tray. All other distillation columns are computed similarly. The absorber does not have either of the additional heights because there is no condenser or reboiler. The stripper does not have a reboiler, and thus there is no need for a 10-ft. bottoms sump. The bare module cost of the tower is estimated from the following equation:

CBM = I 780·L o 87. D I.23.[ (2.S6) + l.694.F Where,

L D FM P

M

·(1O.01 -7.40S·ln(P) + l.395.ln(p)2)]

=tower height in meters

=tower diameter in meters

= material factor = 4.0 for stainless steel

=design pressure in barg

This equation holds for operating pressure> 7 barg. For lower pressure, the pressure factor is approximately 1. The bare module cost of the trays are estimated from the following equation :

C BM = [(193 .04) + 22 .72·0 + 60.3S.D2].FBMoNofq Where,

D Tower diameter in meters

FBM = Material factor for trays

N = actual number of trays

fq =Tray frequency factor

=

The actual number of trays is computed by dividing the number of equilibrium stages used in the simulation by the tray efficiency. The O'Connell Correllation is used to find the tray efficiency for distillation columns (Seader and Henley):

Eo

=0.503.(aopf 00226

For the absorber and stripper, the tray efficiency is calculated as follows:

Log(Eo)

= 1.597 -

L L 00199010g KMLO PL /lLJ - 0.0896· ((KM log PL'/l JJ2 (

Where

a

= relative volatility of key components

/l

=viscosity of liquid

169

K

=K-value of species being absorbed or stripped

PL ML

=density of the liquid =molecular weight of the liquid

For the reflux accumulator, the total liquid (reflux + distillate) flow rate leaving the accumulator = the vapor flow rate from the top tray. The accumulator volume is calculated using the following equation :

Accumulator volume (V)

=(Volumetric flow rate)(residence time)

The diameter is then determined from the volume. Assuming a cylindrical vessel with aspect ratio of 4,

The length can then be found from the Length/Diameter ratio, and figure 9.3 (a) of Seider, Seader, and Lewin can be used to estimate the cost. The following pages summarize the calculations of the cost for the various columns. The reboilers and condensers were priced separately using B-JAC because it is more rigorous and precise.

170

ACETALDEHYDE DISTILLATION COLUMN DC-510

Input Liquid Flow rate (Ib/hr) Density (lb/ft"3) Molecular weight Surface tension (dyne/cm)

Vapor 143500 83.60459256

51950 0.464469959

34 n/a

Trays and tower Design pressure in barg Material factor for tower Number of Equilibrium Stages Efficiency Number of Trays Actual Trays (rounded to whole) Tray spacing (mm) Tray frequency factor Material factor for trays

1.6 4 40 0 .564554408 70.85233851 71 610 TS (ft) 1 2

Reflux Accumulator top stage vol (ft"3/hr) Vol. flow rate (ft"3/min) Accumulator Volume (ft"3) Diameter (L to D = 4) Length Rounded diameter (ft) Rounded length (ft) Fm Fp Fbm Cp Cbm

685 11 .41666667 114.1666667 3.312298574 13.2491943 1.06707317 3.5 meters 3.04878049 10 meters 4 1.1 8.004210526 Current Price 4000 $5,192 32016.84211 $41,560

Calculations Bare module cost of tower Purchased Cost

Current Price 753757.9552 $978,436 75566.2224 $98,091

Surface tension factor/Fst Flow parameter Flooding capacity factor/Cf (m/s) C Flooding velocity/Uf (m/s) U (85% of Uf) Diameter (m) Diameter (ft) Rounded Tower Diameter (ft) Heigh of tower (ft)

1.111961586 0.205887555 0.080473439 0.089483373 1.197205939 1.017625048 1.223823297 4.014140413 4.5 157.0303831

Bare Module Cost of trays Purchased Cost

27023.83808 337.797976

Bare Module Trays + Tower Purchased Cost

$780,781.79 $1,013,515 $75,904 .02 _ _ $98,529 171

Current Cost $35,079 $438

viscosity alpha

0.3 2

2

ACETIC ACID DISTILLATION COLUMN DC-610

Input

I Vapor

Liquid Flow rate (Ib/hr) Density (lb/ft"3) Molecular weight Surface tension (dyne/cm)

210500 80.63198482

151800 0.464469959

34 n/a

Tra~s

and tower Design pressure in barg Material factor for tower Number of Equilibrium Stages Efficiency Number of Trays Actual Trays (rounded to whole) Tray spacing (mm) Tray frequency factor Material factor for trays

5 4 18 0.614443808 29.29478624 30 610 TS (ft) 1 2

Reflux Accumulator top stage vol (ft"3/hr) Vol. flow rate (ft"3/min) Accumulator Volume (ft"3) Diameter (L to D =4) Length Rounded diameter (ft) Rounded length (ft) Fm Fp Fbm Cp Cbm

2243 37.38333333 373.8333333 4.918609886 19.67443954 5 meters 20 meters 4 1.1 8.004210526 Current Price 9000 $11 ,683 72037.89474 $93,511

Calculations

viscosity alpha

2

Bare module cost of tower Purchased Cost of Tower

Current Price $1,449,963 1117008.686 111983.0659 $145,363

Surface tension factor/Fst Flow parameter Flooding capacity factor/Cf (m/s) C Flooding velocity/Uf (m/s) U (85% of Uf) Diameter (m) Diameter (ft) Rounded Tower Diameter (ft)

1.111961586 0.105245968 0.093182831 0.103615728 1.361275663 1.157084313 3.145051187 10.31576789 10.5

Bare Module Cost of trays Purchased Cost of Trays

31831.73264 884.2147955

$41,320 $1,148

$1,148,840.42 $112,867.28

$1,491,283 $146,510


172

1.65 0.25

1.52439024 6.09756098

ACETONE DISTILLATION COLUMN DC-810

Input Liquid Flow rate (Ib/hr) Density (lb/ft"3) Surface tension (dyne/cm)

Vapor

2324 1858

0.371575967 74.31519339 32 n/a

Tra~s

and tower Design pressure in barg Material factor for tower Number of Equilibrium Stages Efficiency Number of Trays Actual Trays (rounded to whole) Tray spacing (mm) Tray frequency factor Material factor for trays

1.6

4

11 0.607967721 18.09306583 19 610 TS (ft) 1 2


40 0.666666667 6.666666667 1.285047805 5.140191221 0.457317

1.5 meters 1.676829 5.5 meters 4 1.1 8.004210526 Current Price $2,207

1700 $17,663 13607.15789

Calculations

viscosity alpha

2

Bare module cost of tower Purchased Cost

Current Price

$97,404 75037 .31296

$9,765 7522 .688471

Surface tension factor/Fst Flow parameter Flooding capacity factor/Cf (m/s) C Flooding velocity/Uf (m/s) U (85% of Uf) Diameter (m) Diameter (ft) Rounded Tower Diameter (ft) Rounded Diameter (m) Height of tower (ft)

1.098560543 0.056532031 0.100927522 0.110874993 1.564084258 1.32947162 0.052382717 0.1 71 81 5311 1.5 0.45720556 52


Current Price

$6,170

4753 .085915

$280 216.0493598

Bare Module Trays + Tower Purchased Cost -

$79,790.40 $7,738.74

173

0.262 1.65

$103,574

$10,045

• NEAR AZEOTROPE DISTILLATION COLUMN DC-900

Input Liquid Flow rate (Ib/hr)

Density (lb/ft"3)

Molecular weight Surface tension (dyne/cm)

Vapor

20350

0.464469959

21700 79.33146894 16 n/a

Trays and tower Design pressure in barg Material factor for tower

Number of Equilibrium Stages Efficiency Number of Trays Actual Trays (rounded to whole) Tray spacing (mm) Tray frequency factor Material factor for trays

1.2

4 12 0.60247906 19.91770469 20 610 TS (ft) 1 2

Reflux Accumulator

top stage vol (ft"3/hr)

Vol. flow rate (ft"3/min) Accumulator Volume (ft"3) Diameter (L to D =4) Length

Rounded diameter (ft)

Rounded length (ft)

Fm Fp Fbm

Cp Cbm

150 2.5 25 1.996471156

7.985884624

2 meters 8 meters 4 1.1

8.004210526 Current $2,726 2100 $21,819 16808.84211

Calculations

viscosity alpha

2

Current Price

$143,388

$14,375

Bare module cost of tower

Purchased Cost

110461.6642 11074.07308

Surface tension factor/Fst Flow parameter

Flooding capacity factor/Cf (m/s) C

Flooding velocity/Uf (m/s)

U (85% of Uf)

Diameter (m)

Diameter (ft)

Rounded Tower Diameter (ft)

Height of tower (ft)

0.9563525

0.081592715 0.096763678

0.092540186

1.205866443

1.024986476

0.475956465

1.561137206

2

54

Current Cost

$7,144

5503.89044 $298 229.3287683

Bare Module Cost of trays

Purchased Cost


$115,965.55 $11,303.40 174

0 .3 1.5

$150,532

$14,673

0.609756

2.439024

ETHYL ACETATE DISTILLATION COLUMN DC-910

Input Liquid Flow rate (Ib/hr) Density (lb/ft"3) Molecular weight Surface tens ion (dyne/cm) Trays and tower Design pressure in barg Material factor for tower Number of Equilibrium Stages Efficiency Number of Trays Actual Trays (rounded to whole) Tray spacing (mm) Tray frequency factor Material factor for trays

Vapor

3222 86 .39141231

L

2789 0.46446996

V 36814 930

73444 5

17 n/a

1.6 4 23 0 .515120908 44 .6497116 45 610 TS (ft) 1 2

viscosity alpha

0.3 3 viscosity alpha

2


38 0 .633333333 6 .333333333 1.263263126 5.053052502 0.457317 1.5 meters 5.5 meters 1.676829 4 1.1 8.004210526 Current Price 1700 $2,207 13607.15789 $17,663

Calculations

Current Price $417,581 $41,864


321692 .0029 32250.47148

Surface tension factor/Fst Flow parameter Flooding capacity factor/Cf (m/s) C Flooding velocity/Uf (m/s) U (85 % of Uf) Diameter (m) Diameter (ft) Rounded Tower Diameter (tt) Bare Module Cost of trays Purchased Cost ,

0 .968018785 0 .084707244 0.09627479 0 .093195805 1.2676 1.07746 0 .06205379 0.203536431 3 Higher because .2 ft is too small, and want aspect ratio <-30 Current Pages 12157.89285 $15,782 $343 264 .3020185


$333,849 .90 $32,514 .77

I I

$433,363 $42,207 175

0 .3 3

STRIPPER ST -800

,

Input

Liquid Flow rate (Ib/hr) Density (lblft"3) Molecular weight Surface tension (dyne/cm)

Vapor

14550 83 .60459256

7637 0.33441837

60 n/a

Trays and tower Design pressure in barg Material factor for tower Number of Equilibrium Stages Efficiency Number of Trays Rounded number of Trays Tray spacing (mm) Tray frequency factor Material factor for trays

0 .8 4 4 0.348058807 11 .49231085 12 610 TS (ft) 1.3 2


53 0.883333333 8.833333333 1.41142534 5.645701361 1.5 meters 6 meters 4 1 7.424736842 Current Price 2,337 1800 13364.52632 17,348

Calculations

I,:


219579.8593 2666.115202

Surface tension factor/Fst Flow parameter Flooding capacity factor/Cf (m/s) C Flloding velocity/Uf (m/s) U (85% of Uf) Diameter (m) Diameter (ft) Rounded off Tower diameter (ft.) Height of tower (ft)

1.24573094 0.120495325 0 .091018966 0.113385142 1.789187361 1 .520809257 0.167200087 0.548556716 1 28


2137.975232 205 .5745416

Current Cost 2,775 267

$221,717 .83 $2,871 .69

287,807 3,728


176

285,032 3,461

K Molar Mas viscosity, cP density of liq, Ib/cuft Kmmu/rho 2

0.457317073 1 .829268293

10 30 .23 0.5 85 1.778235

ABSORBER AB-320

Iii1:J/;j

Input

Liquid Flow rate (Ib/hr) Density (lb/ft"3) Molecular weight Surface tension (dyne/cm) Trays and tower Design pressure in barg Material factor for tower Number of Equilibrium Stages Efficiency Number of Trays Rounded number of Trays Tray spacing (mm) Tray frequency factor Material factor for trays

Calculations

Vapor

105300 86.984076

23160 0.33441837

31.839 n/a K Molar Mas viscosity, cP density of liq, Ib/cuft Kmmu/rho

15 4 15 0.50726453 29.57037 30 610 TS (ft) 1 2

0.475 40 0 .5 85 0.111764706

2

I


82886.3851 20349.1044

Surface tension factor/Fst Flow parameter Flooding capacity factor/Cf (m/s) C Flloding velocity/Uf (m/s) U (85% of Uf) Diameter (m) Rounded off Tower diameter Height of tower (m)

1.09745289 0.28191293 0.07273938 0.07982805 1.28497261 1.09222672 0 .70601546 0.8 22 .5552

Current Price $107,593 $26,415

2.31631672 ft 0.7620023 74 ft

2.5

Current Price Bare Module Cost of trays Purchased Cost Bare Module Trays + Tower Purchased Cost -- -

$9'73~1

7495.776 249.8592 $90,382.16 $20,598.96

$324

$117,323 $26,~9

177

-

-

REFRIGERATED ACETALDEHYDE RECOVERY DC-510

Input Vapor

Liquid 2429 69.6704938

Flow rate (Ib/hr)

Density (lb/ft"3) Molecular weight Surface tension (dyne/cm)

2848 0 .343707769

19 n/a

Trays and tower Design pressure in barg Material factor for tower

Number of Equilibrium Stages Efficiency Number of Trays Actual Trays (rounded to whole)

Tray spacing (mm)

Tray frequency factor

Material factor for trays

1.2

4 2 0.259184073 7.716523525

8

610 TS (ft) 1.9

2

Reflux Accumulator top stage vol (ft"3/hr) Vol. flow rate (ft"3/min)

Accumulator Volume (ft"3) Diameter (L to D = 4)

Length

Rounded diameter (ft)

Rounded length (ft)

Fm Fp Fbm

Cp Cbm

40

0.666666667 6.666666667

1.285047805

5.140191221

1.5 meters 5.5 meters 4 1.1

8.004210526 Current Price $2 ,077 1600 $16,624 12806.73684

Calculations

.

viscosity alpha

2

Bare module cost of tower

Purchased Cost of Tower

Current Price

$60,360 46499.66847 $6,051 4661.714367

Surface tension factor/Fst Flow parameter

Flooding capacity factor/Cf (m/s) C

Flooding velocity/Uf (m/s) U (85% of Uf)

Diameter (m)

Diameter (ft)

Rounded Tower Diameter (ft) Height of tower (ft)

0.989793782

0.059904267 0.1 00340717

0.099316617 1.410515226

1 .198937942

0.076954233

0.252409884 1.5

30


1641 .975134 216 .0493598

Bare Module Trays + Tower

IPurchased Cost

$48,141 .64 $4,877.76 178

0.188 100

$2,131

$193 $62,492 $6,332

0.457317

1.676829

DECANTER DE-720 Horizontal Cylindrical Process Vessel Necessary Volume: 10 minute holding time at half-full

ft3 Flow := 643

hr

V:= Flow·(lO·min)·2

v=

214 .333 ft3

=3

Assume UD 2

n ·D ·L

V=- 4 3

n·D ·3

V=- 4 I

D:= (4.V) 3 3 ·n

D = 4.497ft

Round up to nearest 0.5 ft

D:= 4.5·ft L:= 3·D L = 13.5ft

L=4.115m D=1.372m

179

From cost chart, Cp in 1982 is $7,000

C~002 Cp := 7000·- -

CE I982

9 x 10

3

Cp

=

Cp

= $9,000

Pressure Factor: Fp:= I

Material Factor:

FM := 4.0

Based on chart, Bare Module factor is determined

C BM = 6.3x 10

4

FIRED HEATER F-230

Costs are from Walas, using CE index of 325 CE l985 := 325

Q is heat duty in Million Btu/hr

In Aspen:

Qca 1c:= 12.692

Estimate a stack temperature of 670 F. Using a table found in McKetta. find the efficiency. efficiency:= 0 .83

Ocalc

Q:=--

efficiency

Q= 15.292

180

Use Q

=20 MMBtu/hr for design

Q:= 20

k is material factor k:= 42

Design Factor fd := 0

Pressure factor f p .= . 0

Installed Cost for cylindrical fired heater: C 1nsta \led.1985 := JOOO.k(1 + fd + f p ).QO.S2

Clnstalled:= JOOO.k(J + fd + f ).QO.82. p

Clnstalled = 6.1 05 x 10

C_lnstalled

C~002

CE J985

5

= $610,500

Estimate bare module cost and purchase costs using table based on estimates for bare module costs as a function of purchased cost found in Seider (343)

C p :=

ClnstaJled

2.34

C p = 2.609 x 10

5

Cp = $260,900

CBM := 3.18·C p C

BM = 8.296 x 105

C_BM = $829,600

181

FLASH VESSEL (FV-310)

Estimate volume required by using a holdup time of 5 minutes at half full. ft3 flowrate:= 101146· hr V := flowrate·(5 ·min) ·2 4 3 V = 1.686 x 10ft

Because required volume will be large, in order to limit the size of the radius, so that it can be transported directly, instead of fabricating it on site, an aspect ratio of 4.5 is selected. I 2 -·n·D ·L 4

=V

1 2 . -·n ·D ·(4.5-D) 4

D '=

=V

4.Y ) 3 - ( 4.5-n

D = 16.833 ft

Round up the diameter to the nearest half-foot:

D:=17 ·ft L:= 4.5·D

L = 76.5 ft

In order to use the cost charts, length and diameter must be in meters. D=5.182m

L = 23.317m

The length of 5.182 m is beyond the cost chart's range, but we will extrapolate based on the lines that are present

C~002 C p := 150000· - - CE 1982 C p = 1.929 x 10

5

Cp = $192,900

182

Pressure Factor Fp:== 1

Material Factor FM :== 4 .0

Bare Module Factor FSM :== 9.5 C BM :== FBM·C p

6

C BM == 1.832 x 10

C_BM

=$1,832,000

ACETIC ACID HEAT EXCHANGER HX-200 Compare cost estimated using B-JAC with estimates from cost chart. Surface area calculated using B-JAC is used because it is more accurate than the area from the Aspen results. 2 SA :== 8343.ft

2

SA == 775 .09m

From cost chart, for shell and tube heat exchangers:

CE2002

C p :== 40000 · CE

I982

4

C p == 5.143 x 10

Cp = $51,430 Pressure factor at 15 barg: Fp:== 1.05

Material factor for stainless steel

FM := 3.0

Fp·FM == 3.15

FSM := 6

183

C BM := 6·51430 C BM

= 3.086 x

10

5

C_BM = $308,600 Using B-JAC, the estimated purchase cost was $83,255. Bare-Module cost estimate was $265,000 The prices are comparable, but the bare module cost estimated from B-JAC (and used for calculating the total cost) is 14% lower than the bare module cost using cost charts.

ACETIC ACID PUMP P-110 Power required is the output divided by the efficiency. The efficiency is estimated

by Aspen .

Powernet := 13·hp Powernet = 9.694 kW

YJ := 0.52

Powernet

Power:= - - YJ

Power = 18.642 kW

Power = 25hp

C~002 C p := 9000· - -

CE 1982

C p =1.157 x l0

4

Cp = $11,570 Material Factor

FM := 1.9 Pressure Factor

Fp:= 1.1

184

C BM := FBM·Cp

C BM

= 5.786 x

10

4

C_BM = 57,860 Power requirement for this pump can also be calculated by hand, without using the Aspen results. This can be done using the following equation , found on p. 804 in Seider, Seader, and Lewin.

(gpm)(psidifference) hpower = ...:='---'....:..:....----' (1714)·( efficiency) ft3

gpm:= 719.6·

hr

gpm = 89.716 gal

min

psi difference := 263·psi - 14.7·psi

psidifference = 248.3 psi

efficiency:= 0.52

efficiency used is the value used by the Aspen simulation

(89 .7)·(248.3)

hpower:= (1714)(0.52)

hpower = 24.989

The power requirement of 25 hp used for the calculations agrees well with this result.

ABSORBER SOLVENT PUMP P-540

Powernet := 15.6·hp Powernet = 11.633 kW 11 := 0.57

Powernet

Power:= - - - 11 Power = 20.409 kW

CE 2002

C p := 9000·--

CE I982

185

C p = U57 x 10

4

Cp=$11,570

Fp:= 1.1

4 CBM = 5.786 x 10

C_BM

= $57,860

ACETIC ACID PUMP P-600

Powernet := 2.49· bp Powernet

= 1.857 kW

0.485 Powernet Power := - -

1'] :=

1']

Power = 3.828kW

C~002

C p := 4800·-- CE I982 C p = 6.171 x 10

3

Cp = $6,171

4 CBM = 3.086 x 10

186

ETHYL ACETATE PUMP P-620

Powernet := 1.83·hp

Powernet = 1.365 kW

:= 0.44

Power

Power := net

T]

T]

Power=3 .10IkW CE2002

C p := 4500·- -

CE I982

C p = 5.786 x 10

3

Cp = $5,786

C mV1 := FBM·C p

C BM = 2.893 x 10

4

C_BM = $28,930 RECYCLE PUMP P-730

Powernet := 0.11 ·hp 0.30

Powernet

Power :=

11

T] :=

Power = 0.273 kW CE2002 C p := 2000·- - CE I982 C p = 2.571 x 10

3

Cp = $2,571 C BM := Cp-FBM

C BrvI

= 1.286 x

10

4 187

THE REFLUX AND REBOILER PUMPS WERE NOT SIZED USING ASPEN. THE POWER REPORTED IS TAKEN TO BE THE TOTAL INPUT REQUIREMENT (CONSIDERS EFFICIENCY) ACETALDEHYDE DISTILLATION COLUMN REBOILER PUMP PB-SOO Power:= 7.46·kW

C~002 C p := 2800·- - . CE I982 C p =3 .6 x 10

Cp

3

=$3,600

C BM = 1.8 x 10

4

ACETIC ACID DISTILLATION COLUMN REBOILER PUMP PB-610 Power:= Il .2·kW

C~002 C p := 7000·-- CE I982 C p = 9 x 10

3

Cp = $9,000

C BM = 4.5 x 10

4

ACETONE DISTILLATION COLUMN REBOILER PUMP PB-810 Power := 0.097·kW 188

C p := 1700. CI1002 CE I982

= 2.186 x

Cp

10

3

Cp = $2,186 C BM := FBM·C p

C BM = 1.093 x 10

C_BM

4

= $10,930

NEAR AZEOTROPE DISTILLATION COLUMN REBOILER PUMP PB-900 Power:= O.37 ·kW C := 2200. CI1002

p CE I982

Cp

= 2.829 x

Cp

= $2,829

10

3

C BM := FBM·C p

~M = 1.414 x C_BM

10

4

= $14,140

ETHYL ACETATE DISTILLATION COLUMN REBOILER PUMP PB-910 Power:= 0.30·kW

C := 2J 00 . CI1002

p CE I982

C p = 2.7 x 10

Cp

3

= $2,700

C BM := FBM·C p

C BM = 1.35

x

10

4

189

ACETALDEHYDE REFLUX PUMP PR-500

Power:= 1.49·kW

C~002 C p := 3300·- -

CE 1982

C p = 4.243 x 10 Cp

3

= $4,243

C BM

=

4

2.121 x 10

ACETALDEHYDE CONDENSER REFLUX PUMP PR-510

Power := 0.25·kW

C~002 C p := 2000· - - CE 1982 C p = 2.571 x 10 Cp

3

= $2,571

C BM

=

4

1.286 x 10

ACETIC ACID DISTILLATION COLUMN REFLUX PUMP PR-610

Power:= 5.6·kW

190

C := 5500. CE:2002

p CE I982

C p = 7.071 x 10

3

Cp = $7,071

C BM := FBM·Cp

CBM = 3.536 x 10

C_BM

4

= $35,360

STRIPPER REFLUX PUMP PR-800

Power:= 0.25·kW

C~002

C := 2000. p

Cp = 2.571

CE I982

x

10

3

Cp = $2,571

C BM := FBM·C p

4

CBM = 1.286 x 10 C_BM = $12,860 ACETONE DISITLLATION COLUMN REXLUX PUMP PR·810

Power:= 0.097·kW

CE 2002

C p := 1600·--

CE 1982

C p = 2.057 x 10

3

Cp = $2,057

CBM := FBM·C p

191

Cp

= $2,057

C BM = 1.029 x 10

4

NEAR AZEOTROPE DISTILLATION COLUMN REFLUX PUMP PR-900

Power:= 1.l2·kW

C~002 C p := 3100·-- CE l982 Cp

= 3.986 x J 0

Cp

= $3,986

C BM

3

= 1.993 x 10

4

ETHYL ACETATE DISTILLATION COLUMN REFLUX PUMP PR-910

Power := 0.097·kW C~002 C p := 1600·--

CE 1982

C p = 2.057 x ]0 Cp

3

= $2,057

C BM = 1.029 x 10

4

192

REFRIGERATION SYSTEM RF-520 The cost calculations are based on table 20.2 in Walas. The amount of cooling required for the condenser C-520 is 613,000 Btu/hr. Assuming 33% of cooling is lost to "heat leak" 900,000 Btu/hr of cooling is required of the refrigeration system .

Q := 0.9 MM Btu/hr Temperature factor for refrigeration at -20 C

F:= 2.10 Cinstalled:= 1000.146.f.QO.65.

C~002

CE 1985

5

Cinstalled = 3.568 x J 0

Since it is unclear what is included in the purchase cost of the refrigeration system, in finding the total cost of equipment, we assume an installed price of $500,000 to ensure that all pumps, tanks, and the glycol solution are accounted for.

REACTOR RX-240 Amount of catalyst required is determined by the space velocity. GHSV

= vreactants Vcatalyst

GHSV:= 2600.hr- J

v

ft3 reactants:= 224307· hr

Vcatalyst:=

Vreactants GHSV

Vcatalyst = 86.272 ft3

Take the diameter of the reactor to be 4 ft., and find the required height of the catalyst bed . Vcatalyst = (

~ }11' D2. h

D := 4.ft V h := 4 . catalyst

11·D

2

193

h = 6.865 ft

Additional reactor height is needed for the following:

Footer: 6 ft.

Catalyst Support: 0.5 ft.

Distributor: 0.5 ft.

Header: 3.0 ft.

Total is 10.0 ft. of additional space Total length: L:= h + lO·ft

L = 16.865 ft

Round this up : L :=17·ft

L

-

= 4.25

D

This is a reasonable aspect ratio; the diameter does not need to be re-evaluated. To estimate costs using cost charts. the dimensions must be in meters: L = 5.182m D= l.219m

For a vertical process vessel:

C~002

C p := 13000·- -

CE 1982

C p = 1.671 x 10

4

Cp = $16,710 Stainless Steel Reactor:

F M := 4.0

Pressure is 16 barg

Fp := 2.0

F BM := 16

194

C BM := FBM·C p

C BM = 2.674 x J0

5

C_BM = $267,400

CATALYST COSTS

Assume density of catalyst: p :=

42.~

ft3

Weight of catalyst required: Weightcatalyst := p .Vcatalyst

Weightcatalyst

= 3.623 x

J03 1b

Unit price of catalyst is $1650/Ib :

1650

Costcatalyst := - -

Ib

COS~otal := Costcatalysf Weightcatalyst

COS~otal = Cost

6

5.979 x 10

= $5,979,000

Catalyst Replacement Costs

Estimate that catalyst must be replaced every 5 years, budget 20% replacement per year 900 Salvage:= Ib Replacecos ts := 0.2· Weightcatalysd Costcatalysl - Salvage) Replacecosts = 5.435 x 10

5

Replacement = $543,500Iyr

195

ACETIC ACID HOLDING TANK T-1 Use 1-day supply of acetic acid, since facility is located on the site of major chemical manufacturer ft3

vACOH := 320·

hr time := 24· hr

V := v ACOH" time

V = 217.473m

3

Use cubic meters, because those are the units required for cost chart. C~002 C p := 20000 ·

CE l982

Cp

= 2.571

Cp

=$25,710

x 10

4

FBM := 4 .5

C BM = l.l5 7 x 10

5

C_BM = $115,700 ACETIC ACID BOTTOMS RECYCLE (5-103) HOLDING TANK T-2 Need 12 hour supply of S-103. ft3

v:= 401.4-

hr

t :=

12·hr

V: = v·t

V = 136.397m

3

C~002 C p := 9000·

CE I982

C P = 1.157 x 10

Cp

4

=$11,570 196

C BM := FBM·C p

4

CBM = 5.207 x 10 C_BM = $52,070

ACETIC ACID HOLDING TANK (T-3) Need 12-hour supply of stream S-102 ft3

v:= 7.542·

hr

V:= v· 1

v=

3

2.56 3m

CEz002

C p := 1200·- -

CE 1982

C p = 1.543

Cp

10

x

3

= $1,543

CBM := FBM·Cp CBM = 6.943

x

10

3

C_BM = $6,943

ETHYL ACETATE PRODUCT STOARAGE TANK T-4 Require a 14-day supply of the ethyl acetate product. 1 := 1=

14·24·h 336 h ft3

v:= 21.753·

h

V:= v·1

V

3

= 206.968 m

C := 20000. CEz002 p CE 1982 C p = 2.571 x 10

Cp

4

= $25,710 197

CBM = 1.157 x 10

5

C_BM = $115,700 ACETALDEHYDE PRODUCT STORAGE TANK (T-5) Must hold a 14-day supply of the combined acetaldehyde products ft3 ft3 v := 221.854- + 52.593 · hr hr ft3 v = 274.447

hr

t := 14·24·hr V:= v·t 3

3

V =2 .61I x 10 m

CE:2002 C p := 52000· - - CE 1982 C p = 6.686 x 10 Cp

4

= $66,860

This tank must be refrigerated in order to keep the temperature of acetaldehyde below 60 F. Assume that this doubles the bare module cost.

CBM = 6.0 17 x 10

5

C_BM = $601 ,700

ACETALDEHYDE DISTILLATION COLUMN DC-500 FEED STORAGE TANK (T-6) This tank must hold 12 hours of S-501, the feed to the acetaldehyde distillation column . t := 12· hr ft 3

v:= 181 0.42·

hr

198

V:= v·!

3

V=615.1 85 m

C := 22000. CE:z002

p CE 1982

C p = 2.829 x 10

4

Cp = $28,290

C BM := FBM·C p

C BM

= 1.273 x

10

5

C_BM = $127,300 STORAGE TANK FOR BOTTOMS OF ACETALDEHYDE DISTILLATION COLUMN (T-7) This tank must hold a 12-hour supply of the acetaldehyde distillation column's bottoms, stream S-506. ft3

v:= 1699.945·

hr

V := v·! 3 V = 577.645 m

C := 20000. C"E:z002

p CE I982

Cp = 2.571 Cp

x 10

4

= $25,710

C BM := FBM ·C p

C BM = 1.157 x 10

5

C_BM = $115,700

199

200

lOZ

SNOILV'lil:)'lV:) ISO:) XII'lIIil

:gXION3ddV

202

UTILITY COST ESTIMATES COOLING WATER Required cooling water is 385,000 gal/hr. Annual cost is determined considering a cost of $0.33/1000gal, and operation at 7920 hr/yr.

cw:= 385000·

total

cw

gal hr

:= cwo 7920 hr . .00033

yr gal

6 - I total cw = 1.006 x 10 yr

Annual Cost = $1 ,006,000/yr Find cost if allocated facility is built instead:

According to Table 9.4 in Seider, Seader, and Lewin, the cost is $58/gpm

This book also lists the cooling water cost as $0.05/1 OOOgal, which is considerably

less expensive than our estimate. Thus, assume the allocated cost is $300/gpm.

3 gaJ cw = 6.417 x 10 mm

Cost:= 6417·300

Cost = 1.925 x 10 Allocated Cost

6

=$1,925,000

It appears to be very beneficial to pay this amount as an allocated cost instead of the annual cooling water utility.

203

STEAM COSTS

35 psig steam : Ib

F35 := 2898 ·

hr

c

.00246 lb

'=-

35'

-I

C 35 = 7.129hr

75 psig steam: lb

F75 := 16703 · hr -I

c75 := .00255·1b

C 75 = 42 .593 hr

-I

600 psig steam :

lb F600 := 29636· hr .0028 c600:= - lb

C 600 = 82 .981 hr

C tot = 132 .703 hr

-I

-I

Cannual = l.051 x 10

6

204

C_annual

=$1,051 ,00/yr

Find Cost for allocated plant.

Cost for steam is allocated facility is $50 per pound per hour

Ib

SteaTTtot := 49238·

hr

c:= -

50

Jb

hr C alloc := SteaTTto(c CalJoc = 2.462 x 10

C_alloc

6

= $2,462,000

If generating the initial capital is not a concern, it appears to be more profitable to build an allocated steam plant.

205

206

LOZ

S.LIflS:[}I Sflld N3:dSdV

:3 XIGN3:ddV

208

VESSELS ITEM: AB-320

BLOCK:

ABSORBER MODEL: RADFRAC

- SOLVENT ABSFEED OUTLETS - RECYCLE RECOVERY PROPERTY OPTION SET: HENRY-COMPS ID: INLETS

STAGE 1 STAGE 15 STAGE 1 STAGE 15 NRTL-RK HC-1

RENON (NRTL)

/ REDLICH-KWONG

MASS AND ENERGY BALANCE IN

***

TOTAL BALANCE MOLE (LBMOL/HR) MASS (LB/HR ) ENTHALPY (BTU/HR

5524.62 85747.6 -0.282589E+09

***

OUT

RELATIVE DIFF.

5524.62 85747.6 -0.282590E+09

O.OOOOOOE+OO -0.339413E-15 0.176865E-05

**********************

INPUT DATA

****

****

**********************

INPUT PARAMETERS

****

****

NUMBER OF STAGES ALGORITHM OPTION ABSORBER OPTION INITIALIZATION OPTION HYDRAULIC PARAMETER CALCULATIONS INSIDE LOOP CONVERGENCE METHOD DESIGN SPECIFICATION METHOD MAXIMUM NO . OF OUTSIDE LOOP ITERATIONS MAXIMUM NO. OF INSIDE LOOP ITERATIONS MAXIMUM NUMBER OF FLASH ITERATIONS FLASH TOLERANCE OUTSIDE LOOP CONVERGENCE TOLERANCE COL-SPECS

****

****

MOLAR VAPOR DIST / TOTAL DIST CONDENSER DUTY (W/O SUBCOOL) REBOILER DUTY PROFILES

****

P-SPEC

1.00000 0.0 0.0

BTU/HR BTU/HR

****

STAGE

1

PRES, PSI

233.500

*******************

****

RESULTS

****

*******************

***

COMPONENT SPLIT FRACTIONS

***

OUTLET STREAMS RECYCLE COMPONENT: HYDROGEN C02

METHANE ETHYLENE

15 STANDARD YES STANDARD NO BROYDEN NESTED 25 10 50 0.00010000 0.00010000

1.0000 .97692 .98156 .96964

RECOVERY .33439E-05 .23077E-01 .18437E-01 .30358E-01

209

VESSELS ITEM: AB-320 (CONTINUED) *** COMPONENT SPLIT FRACTIONS

***

OUTLET STREAMS

-------------RECYCLE COMPONENT: ETHANE ACETALD ACETONE ETHYLACE ETHANOL WATER HOAC

***

RECOVERY

.96448 .92922E-01 .31952 .31643 .12114 .68472E-01 .33743E-01

.35519E-01 .90708 .68048 .68357 .87886 .93153 .96626

SUMMARY OF KEY RESULTS

TOP STAGE TEMPERATURE BOTTOM STAGE TEMPERATURE TOP STAGE LIQUID FLOW BOTTOM STAGE LIQUID FLOW TOP STAGE VAPOR FLOW BOTTOM STAGE VAPOR FLOW CONDENSER DUTY (W/O SUBCOOL) REBOILER DUTY

***

LBMOL / HR LBMOL / HR LBMOL / HR LBMOL/HR BTU/HR BTU/HR

MAXIMUM FINAL RELATIVE ERRORS

****

DEW POINT BUBBLE POINT COMPONENT MASS BALANCE ENERGY BALANCE

****

PROFILES

159.440 126 .39 1 1,560.49 1,627.95 3,896.66 3,950 .83 0.0 0.0

F F

****

0.20933E-03 0 . 51743E-03 0 . 25660E-15 0 . 35640E-05

STAGE= STAGE= STAGE= STAGE=

8 4 2 COMP=ETHYLACE 1

****

**NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS FROM THE STAGE EXCLUDING ANY SIDE PRODUCT. FOR THE FIRST STAGE, THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW . FOR THE LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW.

STAGE TEMPERATURE

1 2 14 15 STAGE

1 2 14 15

F

PRESSURE PSI

159.44 157.76 133.17 126.39

233.50 233.60 234.80 234.90

FLOW RATE LBMOL /HR VAPOR LIQUID 3897 . 1560. 3907. 1564. 3940. 1604. 1628. 3951.

ENTHALPY BTU/LBMOL LIQUID VAPOR -0.15764E+06 -0.15731E+06 -0.15377E+06 -0.15223E+06

LIQUID 1550.0000

FEED RATE LBMOL /HR VAPOR

-8922.0 -9046.4 -9031.9 -9118.6

MIXED

3974.6166

210

HEAT DUTY BTU / HR

PRODUCT RATE LBMOL/HR LIQUID VAPOR 3896 " 6629

1627.9537

VESSELS ITEM: AB-320 (CONTINUED) **** MASS FLOW PROFILES FLOW RATE LB/HR VAPOR LIQUID O.6269E+05 0.1988E+05 0.6286E+05 O.2029E+05 0.6478E+05 0.2186E+05 0.6587E+05 0.2238E+05

****

STAGE

1 2 14 15

LIQUID .62278+05

FEED RATE LB/HR VAPOR

MIXED

.23470+05

MOLE-X-PROFILE METHANE CO2 0 . 11598E-02 0.71186E-03 O. 11960E- 02 0.73350E-03 0 . 15743E-02 0.99416E-03 0.17162E-02 0.10895E-02

****

STAGE 1 2 14 15

HYDROGEN 0.60809E-05 0.61050E-05 0.68827E-05 0.72221E-05

PRODUCT RATE

LB/HR

LIQUID VAPOR .19877+05

. 65871+05

**** ETHYLENE 0.40053E-03 0.41622E-03 0.53756E-03 0.59411E-03

MOLE-X-PROFILE **** ACETONE ETHYLACE ETHANOL 0.85172E-02 0.19824E-Ol 0.15239E-02 0 . 83450E-02 0.19430E-Ol o .15056E-02 0.13473E-02 0.65621E-02 0.15246E-Ol 0.65127E-02 0.13831E-Ol 0.16901E-02

ETHANE 0.52185E-03 0.54047E-03 0.62258E-03 0.65202E-03

****

STAGE 1 2 14 15

ACETALD 0.64862E-02 0.11212E-Ol 0.64546E-Ol 0.85999E-Ol

STAGE 1 2 14 15

HOAC

0.48004

0.47829

0.45827 0.44897

HYDROGEN 0.90233 0.89991 0.89246 0.88996

MOLE-Y-PROFILE CO2 METHANE 0.30353E-Ol 0.24232E-Ol 0.30734E-Ol 0.24451E-Ol 0.30626E-Ol 0.24347E-Ol 0.30576E-Ol 0 . 24303E-Ol

****

STAGE 1 2 14 15

ACETALD 0.36806E-02 0.62237E-02 0.25070E-Ol 0.29801E-Ol

MOLE-Y-PROFILE **** ACETONE ETHYLACE 0 . 12776E-02 0.26749E-02 0.12127E-02 0.25221E-02 0.58479E-03 0.11246E-02 0.49963E-03 0.85471E-03

****

STAGE 1 2 14 15

****

MOLE-X-PROFILE

****

**** STAGE 1 2 14 15

HOAC

0.65502E-02

0.62734E-02

0.32669E-02 0 . 26719E-02

STAGE 1 2 14 15

HYDROGEN 0.14835E+06 0.14734E+06 0.12966E+06 0.12323E+06

MOLE-Y-PROFILE

K-VALUES **** CO2 METHANE 26.167 34.036 25 . 690 33.327 19.454 24.489 17.816 22.307

211

WATER 0.48081 0.47833 0.45029 0 . 43893

****

ETHYLENE 0.79277E-02 0.80664E-02 0.80469E-02 0.80373E-02

ETHANOL 0.97326E-04 0.90711E-04 0.35850E-04 0.34814E-04

ETHANE 0.73968E-02 0.75853E-02 0.75610E-02 0.75481E-02

WATER 0.13479E-Ol 0.12930E-Ol 0.68750E-02 0.57111E-02

****

**** ETHYLENE 19.787 19.370 14.968 13.528

ETHANE 14.171 14.028 12.143 11.576

VESSELS ITEM: AB-320 (CONTINUED) K-VALUES **** ACETALD STAGE 0.56738 1 0.55500 2 0.38841 14 15 0.34653

**** ETHYLACE ACETONE 0.13494 0.15000 0.12980 0.14532 0.89122E-Ol 0.73773E-Ol 0.76719E-Ol 0.61800E-Ol K-VALUES

****

MASS-X-PROFILE **** CO2 METHANE 0.12705E-02 0.28425E-03 o .13096E-02 0.29278E-03 0.39496E-03 0.17157E-02 0.18667E-02 0.43197E-03

****

**** STAGE 1 2 14 15

STAGE 1 2 14 15

ETHANOL 0.63870E-Ol 0.60261E-Ol 0.26616E-Ol 0.20602E-Ol

WATER 0.28036E-Ol 0.27035E-Ol 0.15269E-Ol o .13012E-Ol

HOAC O.13646E-Ol 0.13118E-Ol 0.71298E-02 0.59517E-02

HYDROGEN 0.30512E-06 0.30620E-06 0 . 34359E-06 0.35982E-06

STAGE 1 2 14 15

ACETALD 0 .7 1122E-02 0.12289E-Ol 0.70414E-Ol 0.93631E-Ol

STAGE 1 2 14 15

HOAC 0.71753 0 . 71463 0.68151 0.66635

ETHYLENE 0.27968E-03 0.29052E-03 0.37345E-03 0 . 41191E-03

MASS-X-PROFILE **** **** ACETONE ETHYLACE ETHANOL o .12313E-Ol 0.43473E-Ol 0 . 17475E-02 0.42594E-Ol 0.17257E-02 0.12059E-Ol 0.94382E-02 0.33265E-Ol 0.15370E-02 0.93485E-02 0.30118E-Ol 0 . 19243E-02

****

MASS-X-PROFILE

ETHANE 0.39058E-03 0.40435E-03 0.46359E-03 O.48455E-03

WATER 0.21560 0.21440 0.20089 0.19543

****

STAGE 1 2 14 15

HYDROGEN 0.35659 0.34927 0.32417 0.31674

MASS-Y-PROFILE **** **** METHANE ETHYLENE CO2 0.26187 0.76209E-Ol 0 . 43599E-Ol 0.75522E-Ol 0.43568E-Ol 0.26042 0.70381E-Ol 0.40677E-Ol 0.24286 0.68836E-Ol 0.39808E-Ol 0.23757

ETHANE 0.43602E-Ol 0.43913E-Ol 0.40967E-Ol 0.40072E-Ol

STAGE 1 2 14 15

ACETALD 0.31786E-Ol 0.52786E-Ol 0.19900 0.23178

MASS-Y-PROFILE **** ACETONE ETHYLACE 0.14546E-Ol O.46202E-Ol 0.42783E-Ol O.13561E-Ol 0.61200E-02 0.17854E-Ol o .13295E-Ol 0.51232E-02

WATER 0 . 47604E-Ol 0.44848E-Ol 0.22317E-Ol 0.18165E-Ol

**** STAGE 1 2 14 15

MASS-Y-PROFILE

HOAC 0.77113E-Ol 0.72532E-Ol 0.35350E-Ol 0 . 28329E-Ol

212

**** ETHANOL 0.87898E-03 0 . 80457E-03 0.29759E-03 0.28316E-03

****

VESSELS UNIT: DC-SO~ BLOCK: HACDIST

MODEL: RADFRAC

---------- - - - - - - - - - - - - - - - - - - - - -

- DFEED - UP HAC PROD BOTTOMS PROPERTY OPTION SET: HENRY-COMPS ID: INLETS OUTLETS

STAGE 28 STAGE 1 STAGE 1 STAGE 40 NRTL-RK HC-l

/ REDLICH-KWONG

MASS AND ENERGY BALANCE OUT IN

***

DIFF. TOTAL BALANCE MOLE (LBMOL/HR) MASS (LB/HR ) ENTHALPY (BTU/HR

RENON (NRTL)

*** GENERATION

RELATIVE

2598.01 2 598.01 O.OOOOOOE+OO 0.875184E-15 105380. 105380. 0 . 635216E-14 -0.389505E+09 -0.3831 7 3E+09 -0 . 162575E-Ol **********************

INPUT DATA

****

****

**********************

INPUT PARAMETERS

****

****

NUMBER OF STAGES ALGORITHM OPTION INITIALIZATION OPTION HYDRAULIC PARAMETER CALCULATIONS INSIDE LOOP CONVERGENCE METHOD DESIGN SPECIFICATION METHOD MAXIMUM NO. OF OUTSIDE LOOP ITERATIONS MAXIMUM NO. OF INSIDE LOOP ITERATIONS MAXIMUM NUMBER OF FLASH ITERATIONS FLASH TOLERANCE OUTSIDE LOOP CONVERGENCE TOLERANCE COL-SPECS

****

40 STANDARD STANDARD NO NEWTON NESTED 60 10 50 0.00010000 0.00010000

****

MOLAR VAPOR DIST / TOTAL DIST MOLAR REFLUX RATIO MOLAR DISTILLATE RATE

0.22508 2 . 41000 304 .8 01

LBMOL/HR

**** REAC-STAGES SPECIFICATIONS ****

STAGE 39 *****

TO

STAGE 39

REACTIONS/CHEMISTRY ID R-l

REACTION PARAGRAPH R-l ***** **** REACTION PARAMETERS ****

RXN NO . TYPE EQUILIBRIUM

1 **

RXN NO. 1 RXN NO . 1

PHASE LIQUID

CONC. TEMP APP TO EQUIL BASIS F MOLE-GAMMA O. OOOOOE+OO

STOICHIOMETRIC COEFFICIENTS HYDROGEN O.OOOOE+OO ACETALD O.OOOOE+OO

CO2 O.OOOOE+OO ACETONE O.OOOOE+OO

CONVERSION

**

METHANE O.OOOOE+OO ETHYLACE 1.000

213

ETHYLENE O.OOOOE+OO ETHANOL - 1 . 000

ETHANE O.OOOOE+OO WATER 1.000

VESSELS

UNIT: DC-SOO RXN NO. 1

(CONTINUED) HOAC -1.000

PROFILES

**** **** STAGE P-SPEC

1

PRES, PSI

32 . 0000

*******************

****

RESULTS

****

*******************

***

COMPONENT SPLIT FRACTIONS ***

OUTLET STREAMS

--------------

UP COMPONENT:

HYDROGEN CO2 METHANE ETHYLENE ETHANE ACETALD ACETONE ***

HAC PROD

1.0000 .97495 .95251 .83855 .91215 .19677 .21410E-10

.78425E-07 .25046E-01 .47485E-01 .16145 .87851E-01 .80248 .26357E-09

BOTTOMS

.11383E-24 .45731E-27 .73020E-27 .12866E-26 .12675E-26 .74528E-03 1.0000

COMPONENT SPLIT FRACTIONS ***

OUTLET STREAMS

--------------

UP COMPONENT :

ETHYLACE ETHANOL WATER HOAC

HAC PROD

.28611E-22 .90396E-30 .17208E-03 .47139E-23

.97230E-21 .66439E-28 .13630E-02 .36445E-21

SUMMARY OF KEY RESULTS *** TOP STAGE TEMPERATURE BOTTOM STAGE TEMPERATURE TOP STAGE LIQUID FLOW BOTTOM STAGE LIQUID FLOW TOP STAGE VAPOR FLOW BOTTOM STAGE VAPOR FLOW MOLAR REFLUX RATIO MOLAR BOILUP RATIO CONDENSER DUTY (W/O SUBCOOL) REBOILER DUTY

BOTTOMS

1.0000 1.0000 .99846 1.0000

***

PROFILES

101.848 262.664 734.571 2,293.21 68.6041 1,154.40 2.41000 0.50340 -0.105598+08 0.168921+08

F F

LBMOL/HR LBMOL/HR LBMOL/HR LBMOL/HR

BTU/HR BTU/HR

**** **** MAXIMUM FINAL RELATIVE ERRORS DEW POINT o .11384E-03 BUBBLE POINT 0.13731£-03 COMPONENT MASS BALANCE 0.31476E-06 ENERGY BALANCE 0.12321E-04 ****


32 32 31 COMP=ACETONE 31

****

**NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS FROM THE STAGE EXCLUDING ANY SIDE PRODUCT. FOR THE FIRST STAGE, THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW. FOR THE LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW.

214

VESSELS

UNIT:

DC-SO~

(CONTINUED)

STAGE TEMPERATURE F 1 2 26 27 28 29 30 31 39 40

101.85 114.95 119.83 122.41 155.33 156.90 159.84 168.92 255.53 262.66

STAGE

1 2 26 27 28 29 30 31 39 40

****

ENTHALPY BTU/LBMOL LIQUID VAPOR

PRESSURE PSI 32.000 34.000 36.400 36.500 36.600 36.700 36.800 36.900 37.700 37.800

FLOW RATE LBMOL / HR VAPOR LIQUID 68.60 734.6 1039. 755.7 1018. 699.9 1005. 630.6 935.3 3509. 1215. 3511. 1218. 3498. 1205. 3472. 1155. 3448. 1154. 2293.

-82123. -73730. -81954. -71409. -84461. -72240. -91045. -72669. -0.13349E+06 -76234. -0.13366E+06 -76308. -0.13465E+06 -76916. -0.13749E+06 -79206. -0.15265E+06 -0.12956E+06 -0.15643E+06 -0.13051E+06

LIQUID

PRODUCT LBMOL / LIQUID 236.1971

RATE HR VAPOR 68.6041

2293.2091

FLOW RATE LB/HR VAPOR LIQUID 2885. 0.3220E+05 0.3314E+05 0.4544E+05 0.3002E+05 0.4395E+05 0.2673E+05 0.4326E+05 0.1442E+06 0.3997E+05 0.1443E+06 0.5209E+05 0.1438E+06 0.5219E+05 0.1429E+06 0.5169E+05 0.1338E+06 0.4440E+05 0.9214E+05 0.4165E+05

HYDROGEN 0.66888E-11 0.49086E-12 0.14772E-11 0.44824E-11 o .13770E-11 0.48965E-17 0.17610E - 22 0.66254E-28 0.10000E-29 0.10000E-29

.16892+08

.65637-01

MASS FLOW PROFILES

STAGE 1 2 26 27 28 29 30 31 39 40

MIXED

- . 10560+08

2597.9448

****

STAGE

1 2 26 27 28 29 30 31 39 40

FEED RATE LBMOL/HR VAPOR

HEAT DUTY BTU/HR

LIQUID


MIXED

PRODUCT RATE LB/HR LIQUID VAPOR .10355+05 885.3956

1.6931 .10538+06

.92140+05

MOLE-X-PROFILE **** CO2 METHANE 0.53174E-03 0.63137E-03 0.34473E-04 0 . 50854E-04 0.56288E-04 0.43948E-04 0.84081E-04 0.40888E-04 0.45678E-04 0.21243E-04 o .11037E-05 0.37999E-06 0.26134E-07 0.65422E-08 0.58621E-09 0.10123E-09 0.58843E-24 0.10579E-26 0 . 10000E-29 0 . 10000E-29

215

****

ETHYLENE 0.12183E-02 0 . 14360E-03 0.10980E-03 0.11003E-03 0.45112E - 04 0.29442E-05 0.18403E-06 0.10230E-07 0.91180E-20 0.10000E-29

ETHANE 0.67295E-03 0.62903E-04 0.51164E-04 0 . 48350E-04 0.30441E-04 0.13547E-05 0.59121E-07 0.24565E-08 0.20488E-20 0.10000E-29

VESSELS

UNIT: DC-SOO

(CONTINUED)

MOLE-X-PROFILE ACETONE ETHYLACE 0.22339E-I0 0.19187E-21 0.61500E-I0 0.23368E-20 0.11977E-02 0.35829E-02 0.80995E-02 0.69879E-02 0.79118E-02 0.10710E-Ol 0.89707E-02 o .11227E-Ol 0.12462E-Ol 0.13469E-Ol 0.21380E-Ol 0.21172E-Ol 0.16277E-Ol 0.36185E-Ol 0.87298E-02 0.20325E-Ol

****

STAGE 1 2 26 27 28 29 30 31 39 40

ACETALD 0.99051 0.99193 0.94338 0.85026 0.30917 0.30551 0.28841 0.24067 0.36284E-03 0 . 94749E-04

**** STAGE 1 2 26 27 28 29 30 31 39 40

MOLE-X-PROFILE

**** ETHANOL 0.10000E-29 0.10000E-29 0.10380E-03 o .13095E-02 0.56740E-02 0 . 57204E-02 0.59498E-02 0.68345E-02 0.25265E-02 0.15503E-02

****

HOAC 0.17124E-20 0.11276E-21 0.17743E-02 0.32810E-Ol 0.32859 0.32905 0.33251 0.34139 0.41681 0.48394

HYDROGEN 0.29364E-03 0.19382E-04 0.19784E-04 0.20050E-04 o .11193E-05 0.39752E-ll 0.14117E-16 0.51120E-22 0.82659E-24 0.10075E-23

MOLE-Y-PROFILE CO2 METHANE 0.71263E-Ol 0.43604E-Ol 0.52004E-02 0.34678E-02 0.49552E-02 0.31152E-02 0.50300E-02 0.31563E-02 0.54041E-02 0.33746E-02 0.61326E-04 o . 13187E-03 0.31822E-05 0.10956E-05 0.75863E-07 0.18991E-07 0.21550E-21 0.54467E-24 0.41556E-27 0.51968E-27

****

STAGE 1 2 26 27 28 29 30 31 39 40

ACETALD 0.83620 0.98033 0.95724 0.94714 0.88469 0.89234 0.88065 0.83704 0.32215E-02 0.89540E-03

MOLE-Y-PROFILE ACETONE ETHYLACE 0.19438E-22 0 . 62475E-11 0.21277E-I0 0.30466E-21 o .11606E-02 0.14311E-03 0.24960E-02 0.83436E-03 0.54604E-02 0.47109E-02 0.50931E-02 0.63684E-02 0.94243E-02 0.65951E-02 0.13053E-Ol 0.19563E-Ol 0.57959E-Ol 0.12349 0.31269E-Ol 0.67690E-Ol

****

STAGE 1 2 26 27 28 29 30 31 39 40

****

****

**** STAGE 1 2 26 27 28

WATER 0.64326E-02 0.77785E-02 0.49697E-Ol 0.10025 0.33781 0.33951 0 . 34719 0.36855 0 . 52784 0.48536

MOLE-Y-PROFILE

HOAC 0.76255E-22 0.66303E-23 0.83708E-04 0.12360E-02 0.22120E-Ol

216

ETHYLENE 0.21785E-Ol 0.25759E-02 0.18263E-02 0.18504E-02 0.19763E-02 0.13023E-03 0.84886E-05 0.53420E-06 0.11427E:"17 0.12438E-27

ETHANOL 0.46844E-31 0.69785E-31 0.65611E-05 0.72313E-04 0.88281E-03 0.92948E-03 0.10726E-02 0.16899E-02 0.68290E-02 0.44658E-02

****

ETHANE 0.24056E-Ol 0.22164E-02 0.18129E-02 0.18364E-02 o .19638E-02 0 . 87879E-04 0.39058E-05 0.17162E-06 0.23538E-18 0.10994E-27

WATER 0.27961E-02 0.61926E-02 0.29633E-Ol 0.36324E-Ol 0.69414E-Ol 0.71930E-Ol 0.77375E-Ol 0.96925E-Ol 0.59016 0.61222

VESSELS UNIT: DC-SOO (CONTINUED) 29 0.22931E-01 30 0 . 24868E-01 31 0.31729E-01 39 0.21834 40 0.28346

HYDROGEN 0.43899E+08 0.39484E+08 0.13394E+08 0.44734E+07 0.81288E+06 0 . 81190E+06 0.8018SE+06 0.77205E+06 0.82659E+06 0.10075E+07

K-VALUES **** METHANE CO2 69.062 134.02 150.85 68.191 70.884 88.036 77.193 59.825 118.31 158.86 119.48 161.39 167.47 121. 77 187.63 129 . 44 514.85 366.23 415.56 519.68

****

STAGE 1 2 26 27 28 29 30 31 39 40

ACETALD 0.84421 0.98830 1. 0147 1.1139 2.8615 2.9208 3.0534 3.4782 8.8786 9.4503

**** K-VALUES ACETONE ETHYLACE 0.10131 0.27966 0.13037 0.34597 0.11949 0 . 32393 0.11940 0.30816 0.69016 0.43986 0.45362 0.70990 0 . 48959 0.75621 0.91483 0.61634 3.5608 3.4128 3.5819 3.3304

****

STAGE 1 2 26 27 28 29 30 31 39 40

STAGE 1 2 26 27 28 29 30 31 39 40

HOAC 0.44530E-01 0.58798E-01 0.47178E-01 0.37673E-01 0.67316E-01 0 . 69685E-01 0.74779E-01 0.92914E-01 0.52384 0.58572

****

**** STAGE 1 2 26 27 28 29 30 31 39 40

HYDROGEN O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO

CO2 O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO

K-VALUES

ETHYLENE 17.882 17.938 16.632 16.817 43.809 44.232 46.127 52 . 220 125.32 124.38

ETHANOL 0.46843E-01 0.69784E-01 0.63209E-01 0.55222E-01 0.15559 0.16247 0.18023 0.24711 2.7029 2 . 8806

WATER 0.43467 0.79610 0.59628 0.36236 0.20548 0.21186 0.22286 0 . 26297 1.1181 1.2614

****

RATES OF GENERATION LBMOL/HR METHANE ETHYLENE O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO

217

ETHANE 35.748 35.235 35.432 37.982 64.511 64.872 66.072 69 . 886 114.89 109.94

**** ETHANE O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO

ACETALD O. OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO

VESSELS UNIT: DC-SOO

STAGE 1 2

26 27 28 29 30 31 39 40

(CONTINUED) **** ACETONE

O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO

RATES OF GENERATION **** LBMOL/HR WATER ETHYLACE ETHANOL

O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO 15.22 O.OOOOE+OO

**** STAGE

HYDROGEN 0 . 30758E-12 0.22568E-13 0.69433E-13 0.21317E-12 0.67528E-13 0.24011E-18 0 . 86348E-24 0.32445E-29 0.51948E-31 0.50172E-31

1

2

26 27 28 29 30 31 39 40

STAGE 1 2 26 27 28 29 30 31 39 40

ACETALD 0.99535 0.99662 0.96903 0.88366 0.33132 0 . 32739 0.30904 0.25755 0.41191E-03 0.10388E-03

1

2

26 27 28 29 30 31 39 40

STAGE 1 2 26

O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO 15.22 O.OOOOE+OO

MASS-X-PROFILE METHANE

C02 0.53381E-03 0.34602E-04 0.57761E-04 0.87298E-04 0.48904E-04 0.11816E-05 0.27975E-07 0.62671E-09 0.66734E-24 O.10953E-29

0.23105E-03 0.18607E-04 0.16440E-04 0.15475E-04 0 . 82905E-05 0.14829E-06 0.25528E-08 0.39450E-10 0.43736E-27 0.39928E-30

MASS-X-PROFILE **** ACETONE ETHYLACE 0.29596E-10 0.81465E-10 o .48521E-02 0 . 1l098E-01 0.11179E-01 0.12674E-01 0.17604E-01 0.30166E - 01 0.24362E-01 0.12619E-Ol

**** STAGE

O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO -15.22 O.OOOOE+OO

0.38561E-21 0.46958E-20 0.24605E-02 0.14525E-01 0.22955E-01 0.24062E-01 0.28863E-01 0.45315E-01 0.82155E-01 0.44569E-01

MASS-X-PROFILE

HOAC

O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO O.OOOOE+OO -15.22 O.OOOOE+OO

****

ETHYLENE 0.77963E-03 0 . 91878E-04 0.71827E-04 0.72823E-04 0.30787E-04 0.20092E-05 0.12557E-06 0.69719E-08 0.65917E-20 0.69821E-30

ETHANE 0.46158E-03 o .43139E-04 0.35873E-04 0.34298E-04 0.22268E-04 0.99090E-06 0.43241E-07 0.17944E-08 0 . 15876E-20 0.74839E-30

****

ETHANOL 0.10509E-29 0.10507E-29 0.11150E-03 0.14232E-02 0.63589E-02 0.64105E-02 0.66670E-02 0.76486E-02 0.29994E-02 0.17775E-02

WATER 0 . 26434E-02 0 . 31960E-02 0.20876E-01 0.42605E-Ol 0 . 14804 0.14878 0.15214 0.16129 0.24504 0.21762

****

HOAC 0.23457E-20 0.15444E-21 0.24845E-02 0 . 46483E-01 0.48003 0.48068 0.48569 0.49803 0.64503 0.72331

HYDROGEN 0.14074E-04 0.89365E-06 0.92398E-06

MASS-Y-PROFILE **** C02 METHANE 0.74569E-01 0.16632E-01 0.52346E-02 0.12724E-02 0.50524E-02 O.11579E-02

218

****

ETHYLENE 0 . 14531E-01 0.16528E-02 0.11870E-02

ETHANE 0.17199E-01 0.15243E-02 0.12630E-02

VESSELS UNIT: DC-SO~ (CONTINUED) 27 0.93878E-06 28 O.52804E-07 29 0.18698E-12 30 0.66398E-18 31 0.24027E-23 39 0.43340E-2S 40 0.56299E-25

STAGE 1 2 26 27 28 29 30 31 39 40

ACETALD 0.87586 0.98776 0.97699 0.96912 0.91205 0.91723 0.90514 0 . 85974 0.36913E-02 0.10934E-02

0.51417E-02 0.55658E-02 o .13541E-03 0.32675E-05 0 . 77844E-07 0.24668E-21 0.50694E-27

0.12057E - 02 0.12975E-02 0.85246E-04 0.55560E-05 0.34942E-06 0.83377E-18 0.96721E-28

MASS-Y-PROFILE **** ACETONE ETHYLACE 0.86274E-11 0.40719E-22 0 . 28265E-10 0.61395E-21 0.15617E-02 0.29212E-03 0.33670E-02 0.17074E-02 0.74217E-02 0 . 97133E-02 0.86304E-02 0.10470E-01 0.12771E-01 o .13557E-01 0 . 26491E-01 0.26815E-01 0 . 87556E-01 0.28300 0.50341E-01 0.16531

0.12826E-02 0.13819E-02 0.61658E-04 0.27402E-05 0 . 12032E-06 0.18409E-18 0.91632E-28

**** ETHANOL 0.51310E-31 0.73532E-31 0.70029E-05 0.77376E-04 0.95176E-03 0.99913E-03 0.11529E-02 0 . 18152E-02 0 . 81828E-02 0.57026E-02

MASS-Y-PROFILE

**** STAGE 1 2 26 27 28 29 30 31 39 40

0.11761E-02 0.12669E-02 0.22956E-04 0.41007E-06 0.71035E-08 0.22727E-24 0.23109E-27

WATER 0.11977E-02 0.25516E-02 0.12368E-01 0.15199E-01 0.29264E-01 0.30236E-01 0.32522E-01 0.40712E-01 0.27653 0.30572

****

HOAC 0.10888E-21 0.91069E-23 0.11646E-03 0 . 17241E-02 0.31086E-01 0.32131E-01 0.34843E-01 0.44425E-01 0.34104 0.47184

UNIT: DC-SID BLOCK: COND

MODEL: RADFRAC

- UP STAGE 3 - OFFGAS STAGE 1 HACPROD2 STAGE 3 NRTL-RK PROPERTY OPTION SET: HC-1 HENRY-COMPS ID: INLETS OUTLETS

***

RENON (NRTL)

/



68.6041 2885.40 -0.505817E+07

REDLICH-KWONG

*** OUT

RELATIVE DIFF.

68.6041 2885.40 -0.567106E+07

O.OOOOOOE+OO -0.126240E-12 0 . 108073

**********************

****

INPUT DATA

****

**********************

INPUT PARAMETERS **** NUMBER OF STAGES ALGORITHM OPTION ABSORBER OPTION INITIALIZATION OPTION

**** 3

STANDARD NO STANDARD

219

VESSELS UNIT: DC-510 (CONTINUED) HYDRAULIC PARAMETER CALCULATIONS INSIDE LOOP CONVERGENCE METHOD DESIGN SPECIFICATION METHOD MAXIMUM NO. OF OUTSIDE LOOP ITERATIONS MAXIMUM NO. OF INSIDE LOOP ITERATIONS MAXIMUM NUMBER OF FLASH ITERATIONS FLASH TOLERANCE OUTSIDE LOOP CONVERGENCE TOLERANCE COL-SPECS

****

****

MOLAR VAPOR DIST / TOTAL DIST MOLAR DISTILLATE RATE REBOILER DUTY PROFILES

****

1.00000 12.5112 0.0

LBMOL/HR BTU/ HR

****

STAGE

P-SPEC

NO BROYDEN NESTED 25 10 50 0.00010000 0.00010000

1

28.0000

PRES, PSI

*******************

RESULTS

****

****

*******************

***


***

OUTLET STREAMS - - - - - - - - - -

OFFGAS COMPONENT: HYDROGEN CO2 METHANE ETHYLENE ETHANE ACETALD ACETONE WATER

***

1.0000 .99396 .98875 .95529 .97804 .28451E-01 .56151E-03 .54628E-04

HACPROD2 .15998E-07 .60437E-02 .11253E-01 .44715E-01 .21961E-01 .97155 .99944 .99995


TOP STAGE TEMPERATURE BOTTOM STAGE TEMPERATURE TOP STAGE LIQUID FLOW BOTTOM STAGE LIQUID FLOW TOP STAGE VAPOR FLOW BOTTOM STAGE VAPOR FLOW MOLAR REFLUX RATIO CONDENSER DUTY (W/O SUBCOOL) REBOILER DUTY ****

***

F F

LBMOL/HR LBMOL/HR LBMOL/HR LBMOL/HR BTU/HR BTU/HR



****

0.44646E-04 0.17678E-03 0.10043E-05 0.15624E - 04

220

10.0089 98.2806 47.3888 56.0929 12.5112 68.6010 3.78770 -612,887. 0.0


1 1

2 COMP=HYDROGEN 1

VESSELS UNIT: DC-SI0 (CONTINUED) PROFILES **** **** **NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS FROM THE STAGE EXCLUDING ANY SIDE PRODUCT. FOR THE FIRST STAGE, THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW. FOR THE LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW.

STAGE TEMPERATURE F 1 2 3 STAGE

1 2 3

10.009 94.612 98.281

28.000 30.000 30.100

FLOW RATE LBMOL/HR VAPOR LIQUID 47.39 12.51 56.09 59.90 68.60 56.09

-84621. -82008. -82057.

LIQUID

-85381. -74548. -73689.


MASS FLOW PROFILES FLOW RATE LB/HR VAPOR LIQUID 421.8 20 7 0. 2492. 2465 . 2887. 2464.

HEAT DUTY BTU/HR -.61289+06

PRODUCT RATE LBMOL/HR LIQUID VAPOR 12.5112

MIXED

68.6041

**** STAGE

1 2 3


PRESSURE PSI

56.0929

****

LIQUID

FEED RATE LB / HR VAPOR

PRODUCT RATE LB/HR LIQUID VAPOR 421.8406

MIXED

2885 . 3956

MOLE-X-PROFILE CO2 METHANE 0.17955E-01 0.37418E-02 0.73964E-03 0.72101E-03 0.52675E-03 0.60013E-03 ****

2463.5549

****

STAGE 1 2 3

HYDROGEN 0.20020E-09 0.63351E-11 0.57453E-11

ETHYLENE 0.98833E-02 0.17242E-02 0.11914E-02

STAGE 1 2 3

ACETALD 0.96188 0.99434 0.99362

STAGE 1 2 3

HYDROGEN 0.16102E-02 0.33631E-03 0.29366E-03

STAGE 1 2 3

ACETALD 0.13045 0.78822 0.83678

MOLE-Y-PROFILE **** **** ACETONE WATER 0.19236E-13 0.83755E-06 0.65762E-12 0.52993E-03 0.21072E-11 0.13349E-02

STAGE 1 2 3

HYDROGEN 0.80441E+07 0.53090E+08 0.51113E+08

K-VALUES **** CO2 METHANE 21.631 63.211 128.89 72.593 135.62 72 . 826

ETHANE 0.58676E-02 0.84723E-03 0.64615E-03

MOLE-X-PROFILE **** **** ACETONE WATER 0.82616E-12 0.66962E-03 0.25729E-11 0 . 16325E-02 0.76367E-11 0.34196E-02 MOLE-Y-PROFILE **** CO2 METHANE 0.38840 0.23641 0.95329E-01 0.52338E-01 0.71440E-01 0.43704E-01

221

**** ETHYLENE 0 . 11412 0.31654E-01 0.22222E-01

ETHANE 0.12901 0.31589E-01 0.24222E-01

**** ETHYLENE 11.550 18.360 18 . 652

ETHANE 21.995 37 . 286 37.487

VESSELS UNIT: DC-SI0

(CONTINUED) K-VALUES **** ACETONE WATER 0.23279E-01 0.12491E-02 0.25559 0 . 32458 0.27593 0.39036

****

STAGE 1 2 3

ACETALD 0.13562 0.79271 0.84216

STAGE 1 2 3

HYDROGEN 0.92372E-11 0.29057E-12 0 . 26371E-12

STAGE 1 2 3

ACETALD 0.96988 0.99665 0.99665

STAGE 1 2 3

HYDROGEN 0.96269E-04 0.16295E-04 0.14066E-04

STAGE 1 2 3

ACETALD 0.17044 0.83457 0.87593

MASS-X-PROFILE **** CO2 METHANE 0.18086E-01 o .13740E-02 0.74063E-03 0.26318E-03 0.52784E-03 0.21921E-03

**** ETHYLENE 0 . 63462E-02 O . 1l005E- 02 0.76102E-03

ETHANE 0.40384E-02 0.57964E-03 0.44239E-03

MASS-X-PROFILE **** ACETONE WATER 0.10983E-ll 0.27611E-03 0.34001E-11 0.66915E-03 0.10099E-10 0 . 14027E-02

****

MASS-Y-PROFILE CO2 METHANE 0.50697 0.11248 0.10083 0.20180E-01 0.74708E-01 0 . 16660E-01

****

**** ETHYLENE

O. 11506

0.2l343E-01

0.22830E-01 0.17307E-01

O. l4 813E- 01

MASS-Y-PROFILE **** ACETONE WATER 0.33136E-l3 0.44751E-06 0.91798E-12 0.22945E-03 0.29081E-ll 0.57144E-03

****

RADFRAC CONDHCURVE: COND INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID:

HCURVE 1 DUTY CONSTANT NRTL-RK HC-1

DUTY

PRES

TEMP

BTU!HR

PSI

F

RENON

(NRTL)

! REDLICH-KWONG

VFRAC

!============!============!============!============! 28.0000 94 . 0763 1.0000 0.0 28 . 0000 90.8666 DEW>1.0000 - 2480.7655 89.5678 28.0000 0.9189 -5.5717+04 28.0000 87.9270 0.8345 - 1.1143+05 28.0000 85.9013 0 . 7510 -1.6715+05 !------------+------------+--- - --------+ - -----------! -2 . 2287+05 28.0000 83.3465 0.6687 28.0000 80.0428 0.5879 -2.7859+05 28.0000 75.6490 0.5095 -3.3430+05 28.0000 -3 . 9002+05 69.6249 0.4346 28.0000 61.1175 -4.4574+05 0.3649 !-------- -- --+------------+---- - -------+------------! 28.0000 48 . 8093 -5.0145+05 0.3025 28.0000 ! 32.1052 ! 0.2517 ! ! -5.5717+05 ! 28.0000 ! ! -6 . 1289+05 ! 10.0064 ! 0.2088 !

222

ETHANE

o . 9494 9E - 01

VESSELS ITEM: DC-610 BLOCK : ACOHDIST MODEL: RADFRAC

INLETS

- ACOHFEED ETACREC2 - DIST OUTLETS ACOHREC PROPERTY OPTION SET: HENRY-COMPS ID:

STAGE 10 STAGE 2 STAGE 1 STAGE 18 NRTL-RK HC-1

RENON (NRTL)

/ REDLICH-KWONG


***

TOTAL BALANCE MOLE (LBMOL / HR) MASS (LB/HR ) ENTHALPY (BTU/HR

1093.21 52187.9 -0.176431E+09

*** OUT

RELATIVE DIFF.

1093.21 52187.9 -0.173480E+09

0.207987E-15

o .139418E-15 -0.167214E-01

**********************

INPUT DATA

****

****

**********************

****

INPUT PARAMETERS

****

NUMBER OF STAGES ALGORITHM OPTION ABSORBER OPTION INITIALIZATION OPTION HYDRAULIC PARAMETER CALCULATIONS INSIDE LOOP CONVERGENCE METHOD DESIGN SPECIFICATION METHOD MAXIMUM NO. OF OUTSIDE LOOP ITERATIONS MAXIMUM NO. OF INSIDE LOOP ITERATIONS MAXIMUM NUMBER OF FLASH ITERATIONS FLASH TOLERANCE OUTSIDE LOOP CONVERGENCE TOLERANCE

****

COL-SPECS

18 3-PHASE NO STANDARD NO BROYDEN NESTED 25 10 50 0.00010000 0.00010000

****

MOLAR VAPOR DIST / TOTAL DIST MOLAR REFLUX RATIO MOLAR BOTTOMS RATE

LBMOL / HR

0.0 2.50000 359.653

**** L2-STAGES SPECIFICATIONS ****

TWO LIQUID PHASE CALCULATIONS ARE PERFORMED FOR **** L2-COMPS SPECIFICATIONS **** KEY COMPONENTS IN THE SECOND LIQUID PHASE

PROFILES **** **** P-SPEC STAGE

1

PRES,

PSI

RESULTS

****

*******************

223

TO

STAGE 17

COMPONENT ETHYLACE WATER

95.0000

*******************

****

STAGE 1

VESSELS ITEM: DC-610 (CONTINUED) *** COMPONENT SPLIT FRACTIONS

***

OUTLET STREAMS --------------

COMPONENT:

HYDROGEN CO2 ACETALD ACETONE ETHYLACE ETHANOL WATER HOAC ***

DIST

ACOHREC

1.0000 1.0000 1.0000 1.0000 1.0000 1.0000 .95559 . 12359

.32415E-99 .61792E-46 .21697E-08 .27937E-05 .83950E-06 .23878E-05 .44408E-Ol . 87641


TOP STAGE TEMPERATURE BOTTOM STAGE TEMPERATURE TOP STAGE LIQUID FLOW BOTTOM STAGE LIQUID FLOW TOP STAGE VAPOR FLOW BOTTOM STAGE VAPOR FLOW MOLAR REFLUX RATIO MOLAR BOILUP RATIO CONDENSER DUTY (W/O SUBCOOL) REBOILER DUTY

***


BTU/HR BTU/HR


****

DEW POINT BUBBLE POINT COMPONENT MASS BALANCE ENERGY BALANCE PROFILES

****

275.183 369.912 2,567.45 359.653 0.0 3,530.02 2.50000 9.81508 -0.365866+08 0.395348+08

F F

****

0.23796E-06 0 . 38326E-05 0.21642E - 05 0.20501E-03

STAGE= 1 PHASE=L2 STAGE= 2 PHASE=L2 STAGE= 10 COMP=ACETALD STAGE= 1

****

**NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS FROM THE STAGE INCLUDING ANY SIDE PRODUCT .

STAGE TEMPERATURE

1

2 3 9

10 11

16 17 18 STAGE

1 2

F

PRESSURE PSI

275 . 18 297.32 321.48 326.04 327.18 327.86 344 . 44 358.24 369.91

95.000 97.000 97.100 97.700 97.800 97.900 98.400 98.500 98.600

FLOW RATE LBMOL/HR LIQUID VAPOR 2567. O.OOOOE+OO 2119. 2567.

ENTHALPY

BTU/LBMOL LIQUID VAPOR -0.14477E+06 -0.13170E+06 -0.12969E+06 -0.13673E+06 -0.14121E+06 -0.14159E+06 -0.17006E+06 -0.18094E+06 -0.18708E+06

LIQUID

-0.13766E+06 -0.13052E+06 -0.11528E+06 -0.11789E+06 -0.12041E+06 -0 . 12049E+06 -0.14102E+06 -0.15601E+06 -0.16911E+06


350.0000

224

MIXED

HEAT DUTY

BTU/HR

-.36587+08

.39535+08

PRODUCT RATE LBMOL/HR VAPOR LIQUID 733.5560

VESSELS ITEM: 3 9 10 11 16 17 18

DC-610 2154. 2252. 3063. 3070 . 3609. 3890. 359.7

(CONTINUED) 2502. 2601. 2635. 2703.

2998.

3250.

3530.

743.2091

359.6530

FLOW RATE LBMOL/HR LIQUIDI LIQUID2 725.6 1842. O. OOOOE+OO 2119. 2154. O.OOOOE+OO O.OOOOE+OO 2252. 3063. O.OOOOE+OO 3070. O.OOOOE+OO O.OOOOE+OO 3609. O.OOOOE+OO 3890.

STAGE

1 2 3 9 10 11 16 17

****

ENTHALPY

BTU/LBMO

LIQUIDI LIQUID2

-0.15347E+06 -0.12268E+06 -0.13170E+06 -0.13170E+06 -0.12969E+06 -0.12969E+06 -0.13673E+06 -0.13673E+06 -0.14121E+06 -0.14121E+06 -0.14159E+06 -0.14159E+06 -0.17006E+06 -0.17006E+06 -0.18094E+06 -0.18094E+06

MASS FLOW PROFILES

****

FLOW RATE FEED RATE LB/HR LB/HR VAPOR LIQUID VAPOR LIQUID 0.110IE+06 O.OOOOE+OO 0.5738E+05 0.110IE+06 .22326+05 0.5333E+05 0.6650E+05 0.6469E+05 0.6937E+05 0.9590E+05 0.7381E+05 .29862+05

0.9662E+05 0 .7 516E+05

0.1724E+06 0.1158E+06

0.2103E+06 0.1516E+06

0.2074E+05 0.1896E+06

STAGE

1 2 3 9 10 11 16 17 18

MIXED

PRODUCT RATE

LB/HR

LIQUID VAPOR .31444+05

.20744+05

FLOW RATE

LB/HR

LIQUIDI LIQUID2

0.9481E+05 0.1524E+05

O.OOOOE+OO 0.5738E+05





0.1724E+06 O. OOOOE+OO

0.2103E+06 O.OOOOE+OO

0.2074E+05 O.OOOOE+OO

STAGE

1 2 3 9 10 11 16 17 18

MOLE-X-PROFILE ACETALD CO2 0.64777E-03 0.65881E-13 O.OOOOOE+OO 0.12314E-03 O.OOOOOE+OO 0.16039E-04 0.39833E-05 O.OOOOOE+OO O.OOOOOE+OO 0.41966E-05 O.OOOOOE+OO 0.66024E-06 O.OOOOOE+OO 0.94462E-I0 O.OOOOOE+OO 0.16870E-I0 0.28667E-ll O.OOOOOE+OO ****

STAGE 1 2 3 9 10 11 16 17 18

HYDROGEN 0.52175E-07 0.15629E-12 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O . OOOOOE+OO

225

****

ACETONE 0.46370E-Ol 0.99465E-02 0.15170E-02 0.62289E-03 0.77624E-03 0.23011E-03 0.16689E-05 0.70158E-06 0.26423E-06

ETHYLACE 0.28673 0.38722E-Ol 0.30194E-02 0.10106E-02 o .14212E-02 0.35273E-03 0.22613E-05 0.11131E-05 0.49096E-06

VESSELS

ITEM: DC-610

(CONTINUED)

MOLE-X-PROFILE **** WATER HOAC 0.59617 0.65230E-Ol 0.80923 0.14055 0.84135 0.15381 0.74579 0.25246 0.68461 0.31306 0.68012 0.31926 0.29245 0.70755 0.14236 0.85764 0.56508E-Ol 0.94349 MOLE-XI-PROFILE **** **** CO2 ACETALD ACETONE 0.90669E-13 O.82120E-03 0.60785E-Ol O.OOOOOE+OO 0.12314E-03 0.99465E-02 O.OOOOOE+OO 0.16039E-04 0.15170E-02 0.39833E-05 0.62289E-03 O.OOOOOE+OO O.OOOOOE+OO 0.41966E-05 0.77624E-03 O.OOOOOE+OO 0.66024E-06 0.23011E-03 O.OOOOOE+OO 0.94462E-I0 0.16689E-05 O.OOOOOE+OO 0.16870E-I0 0.70158E-06 O.OOOOOE+OO 0.28667E-ll 0.26423E-06

****

STAGE 1 2 3 9 10 11 16 17 18 STAGE 1 2 3 9 10 11 16 17 18

ETHANOL O.48428E-02 O.14249E-02 O.28506E-03 O.11385E-03 o .13193E-03 0.36939E-04 0.16533E-06 0.65214E-07 0.23586E-07 HYDROGEN O.72522E-07 0 . 15629E-12 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

ETHYLACE 0.39323 0.38722E-Ol 0.30194E-02 0.10106E-02 0.14212E-02 0 . 352 7 3E-03 0.22613E-05 0.11131E-05 0.49096E-06

MOLE-XI-PROFILE **** WATER HOAC 0.46130 0.77837E-Ol 0.80923 0.14055 0.84135 0.15381 0.74579 0.25246 0.68461 0.31306 0.68012 0.31926 0.29245 0.70755 0.14236 0.85764 0.56508E-Ol 0 . 94349

****

STAGE 1 2 3 9 10 11 16 17 18

ETHANOL 0.60270E-02 0.14249E-02 0.28506E-03 o .11385E-03 0.13193E-03 0.36939E-04 0.16533E-06 0.65214E-07 0.23586E-07

MOLE-X2-PROFILE CO2 ACETALD 0.29593E-14 0.20754E-03 O.OOOOOE+OO 0.12314E-03 O.OOOOOE+OO 0.16039E-04 O.OOOOOE+OO 0.39833E-05 O.OOOOOE+OO 0.41966E-05 O.OOOOOE+OO 0.66024E-06 O.OOOOOE+OO 0.94462E-I0 O.OOOOOE+OO 0.16870E-I0 O.OOOOOE+OO 0.28667E-ll

****

STAGE 1 2 3 9 10 11 16 17 18

HYDROGEN 0.52511E-09 0 . 15629E - 12 O. OOOOOE+OO O. OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O. OOOOOE+OO

ETHANOL 0.18369E-02 o .14249E-02 0.28506E-03 0.11385E-03 o .13193E-03 0.36939E-04 0.16533E-06 O. 65214E- 07 0.23586E-07

ACETONE 0.97805E-02 0.99465E-02 0.15170E-02 0.62289E-03 0.77624E-03 0.23011E-03 0.16689E-05 0.70158E-06 0.26423E-06

MOLE-X2-PROFILE **** WATER HOAC 0.93855 0.33228E-Ol 0.80923 0.14055 0.84135 0.15381 0.74579 0.25246 0.68461 0.31306 0.68012 0.31926 0.29245 0.70755 0.14236 0.85764 0.56508E-Ol 0.94349

****

STAGE 1 2 3 9 10 11 16 17 18

****

226

ETHYLACE 0.16400E-Ol 0 . 38722E-Ol 0.30194E-02 0 . 10106E-02 o .1421 2 E-02 0 . 35273E-03 0.22613E-05 O. 11131E- 05 0.49096E-06

VESSELS ITEM: DC-610

STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18 STAGE 1 2 3 9 10 11 16 17 18

(CONTINUED)

HYDROGEN 0.51337E-03 0.52175E-07 o .13233E-12 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

ETHANOL 0.74092E-02 0.48428E-02 0 . 16669E-02 0.53067E-03 0.53447E-03 0.14948E-03 0.44808E-06 0.18102E-06 0.69455E-07

HYDROGEN 7078.8530 MISSING MISSING MISSING MISSING MISSING 6.0067+05 1.2353+06 2.4399+06

WATER 1.0064 MISSING MISSING MISSING MISSING MISSING 1.7421 2 . 2376 2.6740 HYDROGEN 9.7764+05 3.3384+05 8.3176+05 6.0099+05 5.0771+05 5.1002+05 MISSING MISSING MISSING

MOLE-Y-PROFILE **** CO2 ACETALD 0.14465E-ll 0.12867E-02 0.65881E-13 0.64777E-03 O. OOOOOE+OO 0.13240E-03 0.30349E-04 O.OOOOOE+OO O.OOOOOE+OO 0.30124E-04 0.47550E-05 O.OOOOOE+OO O.OOOOOE+OO 0.57477E-09 0.10460E-09 O.OOOOOE+OO 0.18296E-I0 O.OOOOOE+OO

**** ACETONE 0 . 87261E-Ol 0.46370E-Ol 0.11015E-Ol 0.29458E-02 0.29941E-02 0.87948E-03 0.40904E-05 0 . 18243E-05 0.74614E-06

ETHYLACE 0.42390 0.28673 0.38824E-Ol 0 . 64778E-02 0.65953E-02 0.16102E-02 0.48266E-05 0.24572E-05 0.11765E-05

MOLE-Y-PROFILE **** **** WATER HOAC 0.46427 0.15357E-Ol 0.59617 0.65230E-Ol 0.82122 0.12714 0.79810 0.19192 0.76641 0 . 22343 0.76817 0 . 22918 0.50947 0.49052 0.31856 0.68144 0.15111 0.84889 K-VALUES: V-Ll **** ACETALD ACETONE 1.5668 1.4355 MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING 6.0847 2.4510 6.2005 2.6003 6.3824 2.8238

ETHYLACE 1.0780 MISSING MISSING MISSING MISSING MISSING 2.1344 2.2076 2.3962

ETHANOL 1.2293 MISSING MISSING MISSING MISSING MISSING 2.7102 2.7757 2.9447

K-VALUES: V-Ll **** **** HOAC 0.1972 MISSING MISSING MISSING MISSING MISSING 0.6932 o .7945 0.8997 K-VALUES: V-L2 **** **** ACETALD CO2 ACETONE 6 . 1996 488.8010 8.9219 5.2605 296.3349 4.6619 719 . 4065 8.2549 7.2608 581.2255 7.6189 4.7292 500.1802 7.1780 3.8572 503.6339 7.2019 3.8220 MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING

ETHYLACE 25.8475 7.4047 12.8576 6.4100 4.6406 4.5652 MISSING MISSING MISSING

ETHANOL 4.0335 3.3987 5.8474 4.6610 4.0511 4.0468 MISSING MISSING MISSING

**** CO2 15.9536 MISSING MISSING MISSING MISSING MISSING 305.8569 299.8558 312.8603

227

VESSELS

ITEM: DC-610

STAGE 1 2 3 9 10 11

16 17 18

STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18 STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18

(CONTINUED)

K-VALUES: V-L2 **** HOAC 0.4621 0.4641 0.8265 0.7602 0.7137 0 . 7178 MISSING MISSING MISSING

WATER 0.4946 0.7367 0.9760 1.0701 1.1194 1.1294 MISSING MISSING MISSING

HYDROGEN 7.2408-03 MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING

**** CO2 3.2638-02 MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING

WATER 2.0345 rUSSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING HYDROGEN 0.24537E-08 o .11635E-13 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

ETHANOL 0.52048E-02 0.24241E-02 0.53036E-03 0.18259E-03 o .19413E-03 0.54073E-04 0.15948E-06 0.55565E-07 0.18839E-07

****

K-VALUES: L2-Ll **** ACETALD ACETONE ETHYLACE 0.2527 0 . 1609 4.1706-02 MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING

K-VALUES: L2-Ll **** **** HOAC 0 . 4268 MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING MASS-X-PROFILE **** **** ACETALD CO2 ACETONE 0.67640E-13 0.66572E-03 0.62829E-Ol O.OOOOOE+OO 0.20032E-03 o .21333E-Ol 0.28535E-04 O.OOOOOE+OO 0.35581E-02 0.61084E-05 O.OOOOOE+OO 0.12594E-02 0.59047E-05 O.OOOOOE+OO 0.14399E-02 O.OOOOOE+OO 0.92421E-06 0.42468E-03 0.87132E-10 0.20295E-05 O.OOOOOE+OO O. OOOOOE+OO o .13745E-10 0.75364E-06 O.OOOOOE+OO 0.21895E-l1 0.26607E-06 MASS-X-PROFILE **** **** WATER HOAC 0.25056 0.91385E-01 0.31169 0.53836 0.61211 0.37303 0.46770 0.52775 0.39391 0.60045 0.38933 0.60921 0.11031 0.88968 0.47434E-01 0.95256 0 . 17650E-01 0.98235

228

ETHANOL 0.3047 MISSING MISSING MISSING MISSING MISSING MISSING MISSING MISSING

ETHYLACE 0.58936 0.12599 0.10744E-Ol 0.30995E-02 0.39993E-02 0.98751E-03 0.41716E-05 0.18138E-05 0.74998E-06

VESSELS

ITEM: DC-6l0

STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18

STAGE 1 2 3 9 10 11 16 17 18

(CONTINUED)

HYDROGEN O.28401E-08 o .11635E-13 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O. OOOOOE+OO O. OOOOOE+OO

ETHANOL 0 . 53940E-02 0.24241E - 02 0.53036E-03 0.18259E-03 0.19413E-03 0.54073E-04 0.15948E-06 0 . 55565E-07 0 . 18839E-07

HYDROGEN 0.50383E-10 0.11635E-13 O.OOOOOE+OO O.OOOOOE+OO O. OOOOOE+OO O. OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O . OOOOOE+OO

ETHANOL 0.40277E-02 0.24241E-02 0.53036E-03 0.18259E-03 0 . 19413E-03 0.54073E-04 0 . 15948E-06 0.55565E-07 0.18839E-07

HYDROGEN 0 . 19863E-04 0.24537E-08 0.10039E-13 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

MASS-X1-PROFILE **** CO2 ACETALD 0.77519E-13 O. 70280E-03 O.OOOOOE+OO 0.2003 2 E-03 O.OOOOOE+OO 0.28535E-04 0.61084E-05 O. OOOOOE+OO O.OOOOOE+OO 0.59047E-05 O.OOOOOE+OO 0.92421E-06 0.8713 2 E-10 O. OOOOOE+OO O.OOOOOE+OO o .13745E-10 0.21895E-11 O.OOOOOE+OO

**** ACETONE 0.68584E-01 0.21333E-01 0.35581E-0 2 0 . 12594E-02 0.14399E-02 0.42468E-03 0.20295E-05 0.75364E-06 0.26607E-06

ETHYLACE 0.67307 0.1 2 599 0.10744E-01 0.30995E-02 0.39993E-02 0.98751E-03 0.41716E-05 o . 18138E-05 0.74998E-06

MASS-X1-PROFILE **** **** WATER HOAC 0.16145 0.90808E-01 0.31169 0.53836 0.61211 0.37303 0.46770 0.52775 0 . 60045 0.39391 0.38933 0 . 60921 0.11031 0.88968 0.47434E-01 0.95256 0.176 5 0E-01 0.98235 MASS-X2-PROFILE **** CO 2 ACETALD 0. 6 1987E - 14 0.43515E-03 0.20032E - 03 O.OOOOOE+OO O. OOOOOE+OO 0.28535E-04 O.OOOOOE+OO 0.61084E-05 O.OOOOOE+OO 0.59047E - 05 O.OOOOOE+OO 0.92421E-06 O.OOOOOE+OO 0.87132E-10 O.OOOOOE+OO o .13745E-10 0.2189SE-11 O.OOOOOE+OO

****

ACETONE 0.27037E-01 0.21333E-01 0.35581E-02 0.12594E-02 0.14399E-02 0 . 42468E-03 0.20295E-05 0.75364E-06 0.26607E-06

ETHYLACE 0.68773E-01 0.12599 0.10744E-01 0.30995E-02 0.39993E-02 0.98751E-03 0 . 41716E-05 0.18138E-05 0.74998E-06

MASS-X2-PROFILE **** **** WATER HOAC 0.80475 0 . 94972E-01 0.53836 0.31169 0.61211 0.37303 0 . 46770 0.52775 0.39391 0.60045 0.38933 0.60921 0 . 11031 0.88968 0.47434E-01 0 . 95256 0.17650E-01 0.98235 MASS-Y-PROFILE **** CO2 ACETALD 0.10879E - 02 0.12218E-11 0.67640E-13 0.66572E-03 O.OOOOOE+OO 0.21951E-03 O.OOOOOE+OO 0.50128E-04 O.OOOOOE+OO 0.47384E-04 O.OOOOOE+OO 0.75345E-05 O.OOOOOE+OO 0.65536E-09 0.98753E-10 O.OOOOOE+OO O.OOOOOE+OO 0.15009E-10

229

****

ACETONE 0.97273E-01 0.62829E-01 0.24075E-01 0.64149E-02 0 . 62093E-02 0.18373E-02 0.61489E-05 0 .2 2707E-05 0 . 80699E-06

ETHYLACE 0.716 8 4 0 . 58936 0.12873 0.21399E-01 0.20749E-01 0 . 51030E-02 0.11007E-04 0.46397E-05 0.19302E-05

VESSELS ITEM: DC-610 STAGE 1 2 3 9 10 11 16 17 18

(CONTINUED)

ETHANOL 0.65513E-02 0.52048E-02 0.28900E-02 0.91664E-03 0.87919E-03 0.24770E-03 0 . 53428E-06 0.17872E-06 0.59584E-07

MASS-Y-PROFILE **** **** WATER HOAC 0.16053 0.17700E-01 0.25056 0.91385E-Ol 0.55676 0.28733 0.53909 0.43213 0.49301 0.47911 0.49777 0.49504 0.23756 0.76242

0.12299 0.87700

0.50693E-Ol 0.94930

RADFRAC REB-HCURVE: ACOHDIST HCURVE 1 INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID:

DUTY CONSTANT NRTL-RK HC-l

DUTY

PRES

TEMP

BTU/HR

PSI

F

RENON (NRTL)

/ REDLICH-KWONG

VFRAC

!============!============!============!============!

I

98.6000 358.2887 0.0

98.6000 BUB>O.O

358.3239 98.6000 7.6185-02

359.8340 361 . 2752 0.1540

98.6000 98.6000 362.6270 0.2333

____________ + ____________ + ____________ + ____________ ! 0.0 2832.5630 3.5941+06 7.1882+06 1.0782+07

363.8777 1.4376+07 98.6000 0.3141

98.6000 o .3961

1.7970+07 365.0224 0.4793

2.1564+07 98.6000 366.0619 2.5159+07 98.6000 367.0011 0.5634

2.8753+07 98.6000 367.8472 0.6485

!------ -- ----+------------+------------+------------!

3.2347+07 98.6000 368.6087 0.7342

3.5941+07 ! 98.6000 ! 369.2942 ! 0.8206 !

0.9075 !

3.9535+07 ! 98.6000 ! 369.9120 !

RADFRAC CONDHCURVE: ACOHDIST HCURVE 1 INDEPENDENT VARIABLE: PRESSURE PROFILE : PROPERTY OPTION SET: HENRY-COMPS ID:


DUTY

PRES

TEMP

BTU/HR

PSI

F

RENON (NRTL)

/ REDLICH-KWONG

VFRAC

I============!============!============!============!

230

VESSELS

ITEM: DC-610 (CONTINUED)

0.0 95.0000 297.1862 1.0000 -5.7254+04 95.0000 295.9248 DEW>1.0000 95.0000 0.9187 -3.3261+06 293.4058 -6.6521+06 95.0000 290.4442 0.8364 -9.9782+06 95.0000 287 . 0608 0.7539 ------------+------------+------------+----------- 95.0000 283.7629 -1.3304+07 0.6683 -1. 6630+07 95.0000 281.4700 0.5772 -1.9956+07 95.0000 279.7259 0.4837 -2.3282+07 95.0000 278.3978 0.3886 -2.6608+07 95.0000 277.3608 0.2923 ------------+------------+------------+----------- -2.9935+07 95.0000 276.5240 0.1953 -3.3261+07 95.0000 275.8255 9.7852-02 -3.6587+07 95 . 0000 275.1832 0.0

ITEM: DC-BIO BLOCK: ACETONE

MODEL: RADFRAC

- 45 STAGE 8 1 - WAS ACTON STAGE RECY STAGE 11 PROPERTY OPTION SET: NRTL-RK HC - l HENRY-COMPS ID: INLETS OUTLETS

***

RENON

(NRTL)

/ REDLICH-KWONG



20.1112 1194.31 -0.276805E+07

*** OUT

RELATIVE DIFF.

20.1112 1194.31 -0 . 294447E+07

-0.176654E-15 -0.886794E-12 0.599151E-Ol

**********************

****

INPUT DATA

****

**********************

****

INPUT PARAMETERS

****

NUMBER OF STAGES ALGORITHM OPTION ABSORBER OPTION INITIALIZATION OPTION HYDRAULIC PARAMETER CALCULATIONS INSIDE LOOP CONVERGENCE METHOD DESIGN SPECIFICATION METHOD MAXIMUM NO. OF OUTSIDE LOOP ITERATIONS MAXIMUM NO . OF INSIDE LOOP ITERATIONS MAXIMUM NUMBER OF FLASH ITERATIONS FLASH TOLERANCE OUTSIDE LOOP CONVERGENCE TOLERANCE

****

COL-SPECS

11 STANDARD NO STANDARD NO BROYDEN NESTED 25 10 50 0.00010000 0.00010000

****

MOLAR VAPOR DIST / TOTAL DIST MOLAR REFLUX RATIO MOLAR DISTILLATE RATE

LBMOL/HR

231

1.00000 4.00000 7.69389

VESSELS

ITEM: DC-S1D (CONTINUED)

PROFILES **** ****

STAGE

P-SPEC

1

PRES,

PSI

22.0000

*******************

****

RESULTS

****

*******************

***

COMPONENT SPLIT FRACTIONS *** OUTLET STREAMS --------------

WASACTON COMPONENT: HYDROGEN ACETALD ACETONE ETHYLACE ETHANOL WATER HOAC

***

1.0000 .95262 .78379 .22231 .46665 .27389 .10587E-05

RECY .11031E-18 .47380E-01 .21621 .77769 .53335 .72611 1.0000

SUMf1ARY OF KEY RESULTS


****

***


BTU/HR BTU/HR



167.616 184.338 30.7755 12.4173 7.69389 17.7904 4.00000 1.43271 -428,727. 252,312.

F F

****

0.24085E-06 0.54550E-05 0.50564E-06 0.83810E-04


6 1 7 COMP=HOAC 1

PROFILES **** **** **NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS FROM THE STAGE EXCLUDING ANY SIDE PRODUCT. FOR THE FIRST STAGE, THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW. FOR THE LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW.

STAGE TEMPERATURE F 1 2 3 6 7 8 10 11

167.62 174.99 176.99 180.08 180.62 181.34 183.14 184.34

PRESSURE PSI 22.000 24.000 24.100 24.400 24.500 24.600 24.800 24.900

ENTHALPY BTU/LBMOL LIQUID VAPOR -0.13985E+06 -0.14526E+06 -0.14909E+06 -0.15470E+06 -0.15639E+06 -0.15734E+06 -0.16028E+06 -0.16361E+06

232

-0.11865E+06 -0.12447E+06 -0.12879E+06 -0.13501E+06 -0.13611E+06 -0.13733E+06 -0.14088E+06 -0.14377E+06


.25231+06

VESSELS ITEM: DC-SIO STAGE

1 2 3 6 7 8 10 11

**** STAGE

1 2 3 6 7 8 10 11

(CONTINUED) FLOW RATE LBMOL/HR VAPOR LIQUID 7.694 30.78 38.47 30.77 38.46 30.52 30.29 37.99 30.36 37.98 17.94 30.31 30.21 17.83 12.42 17.79

LIQUID

12.4173

****

FLOW RATE LB/HR VAPOR LIQUID 439.3 1760. 2199. 1764. 2203. 1753. 2187. 1759. 1793. 2199. 1038. 1791. 1794. 1034. 1039. 755.0

HYDROGEN 0.15496E-l3 0.68273E-14 0.11526E-l3 0.22880E-13 0.24183E-13 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

LIQUID


STAGE 1 2 3 6 7 8 10 11

WATER 0.26316 0.298l3 0.32256 0.34723 0.33671 0.34316 0.35671 0.34832

HYDROGEN 0.12454E-08 0.24908E-09 0.24914E-09 0.25224E-09 0.25227E-09 0.40923E-13 O.OOOOOE+OO O.OOOOOE+OO

MIXED


1194.3096

755.0260

**** MOLE-X-PROFILE ACETALD ACETONE 0.38569E-02 0.39977 0.21622E-02 0.31529 0.16098E-02 0.25623 0.13917E-02 0.17887 0.l3897E-02 0.17040 0.10060E-02 0.15567 0.47615E-03 0.11477 0.28700E-03 0.87972E-Ol

**** ETHYLACE 0.32591 0.37711 0.41254 0.46645 0.48538 0.49404 0.52217 0.55747

MOLE-X-PROFILE HOAC 0.15028E-07 0.90382E-07 0.52631E-06 0.97032E-04 0.52657E-03 0.52800E-03 0.59186E-03 0.11750E-02

****

**** MOLE-Y-PROFILE ACETALD ACETONE 0.93129E-02 0.51469 0.42275 0.49481E-02 0.35927E-02 0.35518 0.30006E-02 0.25852 0.29962E-02 0.24689 0.21530E-02 0.22745 0.10029E-02 0.17158 0.60817E-03 0.13347

****

****

STAGE 1 2 3 6 7 8 10 11

MIXED


20.1111

MASS FLOW PROFILES

STAGE 1 2 3 6 7 8 10 11


233

ETHYLACE 0.25720 0.31217 0.35312 0.41278 0.42406 0.43548 0.46906 0.49754

ETHANOL 0.73056E-02 0.73126E-02 0.70625E-02 0.59611E-02 0.56026E-02 0.55902E-02 0.52791E-02 0.47830E-02

ETHANOL 0.67540E-02 0.71953E-02 0.72009E-02 0.64118E-02 0.61217E-02 0.61700E-02 0.60044E-02 0.56253E·02

VESSELS

ITEM: DC-810

(CONTINUED)

MOLE-Y-PROFILE HOAC

0.20077E-08

0.12424E-07

O. 72702E- 07

0.13779E-04

0.77378E-04

0.77710E-04

0.88395E-04

0.18483E-03

****

STAGE 1 2 3 6 7 8 10 11

STAGE 1 2 3 6 7 8 10 11

STAGE 1 2 3 6 7 8 10 11

STAGE 1 2 3 6 7 8 10 11

STAGE 1 2 3 6 7 8 10 11

STAGE 1 2

WATER 0.21205 0.25294 0.28091 0.31927 0.31985 0.32867 0.35226 0.36257

HYDROGEN 80348. 36476. 21612. 11024. 10432. 9116.9 6362.1 5231.8

WATER 0.80561 0.84818 0.87066 0.91942 0.94993 0.95775 0.98752 1.0410

HYDROGEN 0.54631E-15 0.24003E-15 0.40455E-15 0.79408E-15 0.82518E-15 O.OOOOOE+OO O. OOOOOE+OO O. OOOOOE+OO

WATER 0.82912E-01 0.93669E-01 0.10117 0.10770 0.10267 0.10463 0.10819 0.10320

HYDROGEN 0.43970E-10 0.87840E-11

K-VALUES **** ACETALD 2.4148 2.2886 2.2318 2.1561 2.1559 2.1403 2.1063 2 . 1191

****

**** ACETONE 1.2875 1. 3409 1.3862 1.4453 1.4489 1.4611 1.4950 1. 5172

K-VALUES

**** HOAC

0.13357

0 . 13742

0.13810

0.14199

0.14694

0.14718

0.14936

0.15731

MASS-X-PROFILE **** ACETALD ACETONE 0.29714E-02 0.40605 0.16612E-02 0.31935 0.12347E-02 0.25910 0.10555E-02 0.17886 0.10363E-02 0.16752 0.75004E-03 0.15302 O.35314E-03 0.11222 0.20793E-03 0.84031E-01

ETHYLACE 0.78927 0.82795 0.85612 0.88498 0.87368 0.88147 0.89829 0.89247 ****

**** ETHYLACE 0 . 50218 0.57944 0.63283 0.70756 0.72387 0.73670 0.77454 0.80778

MASS-X-PROFILE **** HOAC

0.15782E-07

0.94657E-07

0.55028E-06

0.10032E-03

0.53526E-03

0.53664E-03

0.59838E-03

O. 11605E- 02

****

MASS-Y-PROFILE **** ACETALD ACETONE 0.71856E-02 0.52357 0.38132E-02 0.42953

****

234

ETHANOL 0.92443 0.98387 1.0195 1.0756 1.0926 1.1037 1.1374 1.1761

ETHYLACE 0.39689 0.48114


ETHANOL 0.54496E-02 0.57988E-02

VESSELS

ITEM: DC-SIO (CONTINUED) 0.87665E-ll 3 6 0.88333E-11 7 0.87859E-11 o .l4252E-14 8 10 O.OOOOOE+OO O.OOOOOE+OO 11

0.27625E-02 0.22963E-02 0.22803E-02 0.16386E-02 0.76220E-03 0.45863E-03

0.36007 0.26084 0.24773 0.22822 0.17192 0.13270

MASS-Y-PROFILE HOAC 0.21117E-08 O. l3051E-07 0.76207E-07 0.14374E-04 0.80278E-04 0.80622E-04 0.91578E-04 0.19000E-03

**** STAGE 1 2 3 6 7 8 10 11

WATER 0.66908E-Ol 0.79715E-Ol 0.88333E-Ol 0.99920E-Ol 0.99550E-Ol 0.10229 0.10948 0.11181

RADFRAC REB-HCURVE: ACETONE INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID:

0.54305 0.63180 0.64549 0.66285 0.71297 0.75040

****

HCURVE 1


DUTY

PRES

TEMP

BTU/HR

PSI

F

RENON

(NRTL)

/

REDLICH-KWONG

VFRAC

!============!============!============!============! 0.0 24.9000 183.1507 0.0 245.4757 183 . 3695 BOO>O . O 24.9000 2.2937+04 24.9000 183.4705 5.3156-02 4.5875+04 24.9000 183.5689 0 . 1068 6.8812+04 24.9000 183.6639 0.1604 !------------+------------+------------+------------! 9.1750+04 24.9000 183.7557 0.2141 1.l469+05 24.9000 183.8446 0.2676 1.3762+05 24.9000 183.9310 0.3212 1.6056+05 184.0151 24.9000 0.3747 1.8350+05 24.9000 184.0974 0.4283 - -----------+------------+------------+----------- 184.1782 2.0644+05 24.9000 0 . 4818 2 . 2937+05 184 . 2581 24.9000 0.5353 2.5231+05 184.3375 24.9000 0.5889

RADFRAC CONDHCURVE: ACETONE INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID:

DUTY

PRES

HCURVE 1


RENON

TEMP

(NRTL)

VFRAC

235

/

REDLICH-KWONG

0.57904E-02 0.5l315E-02 0.4 8723E- 02 0.49106E-02 0.47721E-02 0.44363E-02

VESSELS ITEM: DC-B10

BTU/HR

(CONTINUED)

PSI

F

!============!============!============!============! 0.0 22.0000 174.4885 1.0000 22.0000 DEW>1.0000 -3317.0574 170.2403 22.0000 0.9339 -3 .8 975+04 170.0385 -7.7950+04 22.0000 169.8144 0.8614 -1.1693+05 22.0000 169.5862 0.7887 !--------- -- -+----------- - +------------+------- - ----! 22.0000 169.3540 0.7158 -1.5590+05 -1.9488+05 169.1176 0.6427 22.0000 -2.3385+05 168.8772 0.5695 22.0000 -2 . 7283+05 22.0000 168 . 6329 0.4960 0.4223 -3.1180+05 22.0000 168.3847 !------------+------------+------------+------------! -3 . 5078+05 22.0000 168.1326 0.3484

0.2743 !

! -3 .8975+05 ! 167.8765 ! 22.0000 ! 22.0000 ! 0.2000 !

! -4.2873+05 ! 167.6159 !

ITEM: DC-900 BLOCK: NEAZDIST MODEL: RADFRAC - NDFEED STAGE 6

- NEAZRECY STAGE 1

ETACACOH STAGE 12

PROPERTY OPTION SET: NRTL-RK HC-1

HENRY-COMPS ID: INLETS OUTLETS

RENON (NRTL)

/ REDLICH-KWONG


***


93.0149 5933.43 -0.159980E+08

*** OUT

RELATIVE DIFF.

93.0149 5933.43 -0 . 157592E+08

0.152780E-15 0.276982E-12 -0.149287E-01

**********************

****

INPUT DATA

****

**********************

****

INPUT PARAMETERS

****

NUMBER OF STAGES ALGORITHM OPTION ABSORBER OPTION INITIALIZATION OPTION HYDRAULIC PARAMETER CALCULATIONS INSIDE LOOP CONVERGENCE METHOD DESIGN SPECIFICATION METHOD MAXIMUM NO. OF OUTSIDE LOOP ITERATIONS MAXIMUM NO. OF INSIDE LOOP ITERATIONS MAXIMUM NUMBER OF FLASH ITERATIONS FLASH TOLERANCE OUTSIDE LOOP CONVERGENCE TOLERANCE

236

12 STANDARD NO STANDARD NO BROYDEN NESTED 25 10 50 0.00010000 0.00010000

VESSELS ITEM: DC-900 (CONTINUED) COL-SPECS **** ****

MOLAR VAPOR DIST I TOTAL DIST MOLAR REFLUX RATIO MOLAR DISTILLATE RATE DIST + REFLUX DEG SUBCOOLED PROFILES

****

P-SPEC

LBMOL/HR F

0.0 1.80000 72.7032 2.00000

**** STAGE

1

PRES,

25.0000

PSI

******************* **** RESULTS **** *******************

***


***

OUTLET STREAMS NEAZRECY COMPONENT: HYDROGEN C02

ACETALD ***

1.0000 1 . 0000 .99999

ETACACOH .21252E-41 . 22584E-11 .12760E-04


***

OUTLET STREAMS

COMPONENT: ACETONE ETHYLACE ETHANOL WATER HOAC

***

NEAZRECY

ETACACOH

.99790 .75141 .99188 .99615 .23235E-02

.20984E-02 .24859 .81152E-02 .38485E-02 .99768


TOP STAGE TEMPERATURE BOTTOM STAGE TEMPERATURE TOP STAGE LIQUID FLOW BOTTOM STAGE LIQUID FLOW TOP STAGE VAPOR FLOW BOTTOM STAGE VAPOR FLOW MOLAR REFLUX RATIO MOLAR BOILUP RATIO CONDENSER DUTY (W/O SUBCOOL) REBOILER DUTY DIST + REFLUX SUBCOOLED TEMP SUB COOLED REFLUX DUTY

****

*** F F


BTU/HR BTU/HR F

BTU/HR



****

0.25122E-05 0.10078E-04 0.10650E-06 0.63138E-05

237

183.909 221.036 130.866 20.3117 0.0 243.616 1.80000 11.9939 - 2,896,260. 3,150,280. 181. 909 -15,189.4

STAGE= 12 STAGE= 3 STAGE= 4 COMP=ACETALD STAGE= 12

VESSELS ITEM: DC-900 (CONTINUED) PROFILES **** **** **NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS FROM THE STAGE EXCLUDING ANY SIDE PRODUCT. FOR THE FIRST STAGE, FOR THE THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW. LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW.

STAGE TEMPERATURE F

PRESSURE PSI

1 SUBC 2 5 6 7 10

25.000 25.000 27.000 27.300 27.400 27.500 27.800 27.900 28.000

11

12

183.91 181.91 189.95 196.30 198.30 202.03 209.64 212.64 221. 04

FLOW RATE LBMOL/HR LIQUID VAPOR O.OOOOE+OO 1 130.9 SUBC 130.9 203.6 2 134.6 210.3 5 138 . 5 211.2 6 253.5 233.2 7 256.1 239.6 10 261.7 241.4 263.9 11 20.31 243.6 12

ENTHALPY BTU/LBMOL LIQUID VAPOR -0.16155E+06 -0.16162E+06 -0.16947E+06 -0.18451E+06 -0.18549E+06 -0.19134E+06 -0.19846E+06 -0 . 19855E+06 -0.19736E+06

STAGE

****

MASS FLOW PROFILES

FLOW RATE LB/HR VAPOR LIQUID 7841. O.OOOOE+OO 1 SUBC 7841. 2 8739. 0.1220E+05 5 0 . 1049E+05 0.1451E+05 6 0.1925E+05 0.1485E+05 7 0.2052E+05 0.1767E+05 10 0.2211E+05 0.2033E+05 11 0.2191E+05 0.2054E+05 12 1577. 0.2034E+05

LIQUID

HYDROGEN 0.13988E-06 0.26500E-I0 0.28227E-ll 0.20671E-ll O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

-0.14732E+06 -0.16091E+06 -0.16285E+06 -0.17095E+06 -0 . 18428E+06 -0.18550E+06 -0.18571E+06


MIXED

-.28963+07 -.15189+05

.31503+07 PRODUCT RATE LBMOL/HR VAPOR LIQUID 72.7031

93.0148

20.3116

****

STAGE

STAGE 1 2 5 6 7 10 11 12

-0.14187E+06

HEAT DUTY BTU/HR

LIQUID


MIXED


5933.4341

1577.3333

MOLE-X-PROFILE ****

**** CO2 ACETALD ACETONE 0.17419E-12 0.14553E-02 0.10041 0.98959E-14 0.66625E-03 0.65731E-Ol 0.21915E-14 0.23396E-03 0.35968E-Ol 0.22316E-14 0.21237E-03 0.33389E-Ol 0.65935E-04 O.OOOOOE+OO 0.19592E-Ol O.OOOOOE+OO 0.12641E-05 0 . 3l289E-02 O.OOOOOE+OO 0.31225E-06 0.16114E-02 O.OOOOOE+OO 0.66470E-07 0.75579E-03

238

ETHYLACE

0.53625

0.62779

0.78863

0.77815

0.84363

0.89247 0.83078 0.63500

VESSELS

ITEM:

DC-900

(CONTINUED)

STAGE 1 2 5 6 7 10 11 12


MOLE-X-PROFILE **** WATER HOAC 0.35295 0.23366E-03 0.29766 0.12561E-02 0.21184E-01 0.15013 0.13871 0.45841E-01 0.84134E-01 0.50136E-01 0.90222E-01 o .13634E-01 0.77673E-02 0.15948 0.48807E-02 0.35911

STAGE 1 2 5 6 7 10 11 12

HYDROGEN 0.80807E-03 0.13988E-06 0.48354E-07 0.48144E-07 0.22472E-11 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

MOLE-Y-PROFILE **** CO2 ACETALD ACETONE 0.29452E-11 0.30501E-02 0.15079 0.17419E-12 0.14553E-02 0.10041 0.61806E-13 0.68541E-03 0.61257E-Ol 0.61391E-13 0.65431E-03 0.58149E-01 0.23087E-03 0.24260E-14 0.36231E-01 O.OOOOOE+OO 0.53464E-05 0.63559E-02 O.OOOOOE+OO o .13649E-05 0.33286E-02 O.OOOOOE+OO 0.33274E-06 0.16827E-02

STAGE 1 2 5 6 7 10 11 12


MOLE-Y-PROFILE **** WATER HOAC 0.35544 0.35449E-04 0.35295 0.23366E-03 0.23973 0.63532E-02 0.21994 0.13973E-01 0.15036 0.18552E-01 0.27067E-01 0.40972E-01 0.14371E-01 0.67595E-01 0.80080E-02 0.14283

STAGE 1 2 5 6 7 10 11 12

HYDROGEN 5777.0 5277.7 17123. 23283 . 71363. 0.40074E+07 0.51337E+07 0.49047E+07

****

****

ETHYLACE 0.47990 0.53625 0.68608 0.70176 0.79062 0.92465 0.91413 0.84711

****

****

**** STAGE 1 2 5 6 7 10 11 12

ETHANOL 1.1467 1.2617 1.5302 1. 4 934 1.6405 1.7470 1.5879 1.4435

STAGE 1 2

HYDROGEN 0.47062E-08 0.82295E-12

K-VALUES

CO2 16.907 17.601 28.200 27.508 33 . 894 39.163 32.851 36.264

WATER 1.0071 1.1857 1.5967 1.5856 1.7872 1.9853 1.8502 1. 6407

**** ACETALD 2.0958 2.1842 2.9295 3.0809 3.5014 4.2295 4.3712 5.0057

K-VALUES

ACETONE 1. 5017 1 . 5276 1.7031 1.7416 1.8493 2.0314 2.0657 2.2265

ETHYLACE 0.89492 0.85421 0.86997 0.90184 0.93717 1.0361 1.1003 1.3340

****

HOAC 0.15171 0.18600 0.29989 0.30480 0.37002 0.45414 0.42385 0.39775

MASS-X-PROFILE **** CO2 ACETALD ACETONE 0.12795E-12 0.10700E-02 0.97336E-01 0.67091E-14 0.45214E-03 0.58810E-01

****

239

ETHYLACE 0.78855 0.85207

...

VESSELS ITEM: DC-900 (CONTINUED) 0.75130E-13 5 o .54 879E-13 6 7 O.OOOOOE+OO O.OOOOOE+OO 10 O.OOOOOE+OO 11 O.OOOOOE+OO 12

o .12734E-14 0.12934E-14 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

o .13609E-03 0.12321E-03 0.36259E-04 0.65900E-06 0.16568E-06 0.37708E-07

0.27583E-Ol 0.25539E-Ol o .14205E-Ol 0.21505E-02 o .11273E-02 0.56526E-03

STAGE 1 2 5 6 7 10 11 12

ETHANOL O. 66914E- 02 0.48950E-02 0.23442E-02 0.22437E-02 0.14015E-02 0.29759E-03 0.19931E-03 0.15119E-03

MASS-X-PROFILE **** WATER HOAC 0.10612 0.23419E-03 0.82609E-Ol 0.11620E-02 0.35711E-Ol 0.16797E-Ol 0.32909E-Ol 0.36255E-Ol 0.18920E-Ol 0.37584E-Ol 0.29067E-02 0.64117E-Ol 0.16854E-02 0.11535 0 . 11323E-02 0.27770

STAGE 1 2 5 6 7 10 11 12

HYDROGEN 0.28066E-04 0 . 47062E-08 0.14125E-08 o .13807E-08 0.59778E-13 O.OOOOOE+OO O.OOOOOE+OO O. OOOOOE+OO

MASS-Y-PROFILE **** CO2 ACETALD ACETONE 0.22332E-ll 0.23150E-02 0.15089 0 . 12795E-12 0 . 10700E-02 0.97336E-Ol 0.39417E-13 0.51557E-Ol 0.43755E-03 0.48047E-Ol 0.38437E-13 0.41007E-03 0.14089E-14 0.27769E-Ol o .13421E-03 0.27765E-05 0.43517E-02 O.OOOOOE+OO O.OOOOOE+OO 0.70672E-06 0.22723E-02 O.OOOOOE+OO 0.17561E-06 o .11709E-02

STAGE 1 2 5 6 7 10 11 12

ETHANOL 0 . 79206E-02 0.66914E-02 0.39368E-02 0 . 36195E-02 0 . 24305E-02 0.51788E-03 0.30883E-03 0.20304E-03

MASS-Y-PROFILE **** WATER HOAC 0.11032 0.36677E-04 0.10612 0.23419E-03 0.62584E-Ol 0.55288E-02 0.56368E-Ol 0.11938E-Ol 0 . 35746E-Ol 0.14702E-Ol 0.57483E-02 0.29005E-Ol 0.30430E-02 0.47712E-Ol 0.17283E - 02 0.10276

0.91743 0.90293 0.92785 0.93053 0.88163 0.72045

****

****

****

RADFRAC REB-HCURVE: NEAZDIST HCURVE 1 INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID:


DUTY

PRES

TEMP

BTU/HR

PSI

F

RENON

(NRTL)

/

REDLICH-KWONG

VFRAC

!============!============!============!============!

0.0 2510.6086 2.8639+05

28.0000 28.0000 28.0000

212.6416 212.8657 213.1768

240

0.0 BUB>O.O 8.2608-02

ETHYLACE 0.72848 0.78855 0 . 87596 0.87962 0.91922 0.96037 0.94666 0.89414

VESSELS

ITEM: DC-900 (CONTINUED)

28 . 0000 213.5200 5.7278+05 0.1660 8.5917+05 28.0000 213.9019 0.2496 ------------+------------+------------+----------- 28.0000 1.1456+06 214.3344 0.3332 28.0000 214.8328 1.4319+06 0.4170 28.0000 1.7183+06 215.4176 0.5009 2.0047+06 28.0000 216.1166 0.5849 2.2911+06 28.0000 216.9681 0.6691 !------------+------------+------------+----------- 2.5775+06 28.0000 218.0244 0.7534 219.3539 0.8380 28.0000 2.8639+06 28.0000 221.0362 3.1503+06 0.9230

RADFRAC CONDHCURVE: NEAZDIST HCURVE 1 INDEPENDENT VARIABLE: PRESSURE PROFILE : PROPERTY OPTION SET: HENRY-COMPS ID:

DUTY CONSTANT NRTL-RK HC-1

DUTY

PRES

TEMP

BTU/HR

PSI

F

RENON

(NRTL)

/

REDLICH-KWONG

VFRAC

!============!============!============!============! 0.0 25.0000 189.5595 1.0000

-1.7636+04 25.0000 185.5610 DEW>1.0000

-2.6468+05 25.0000 185.3809 0.9133

-5.2935+05 25.0000 185.2168 0.8209

-7.9403+05 25.0000 185.0710 0.7287

!------------+------------+------------+------------! -1.0587+06 25.0000 184.9356 0.6368 -1.3234+06 25.0000 184.8049 0.5450 -1.5881+06 25 . 0000 184.6750 0.4533 -1.8527+06 25.0000 184.5426 0.3616 25.0000 -2.1174+06 184.4055 0.2699 ------------+------------+------------+----------- -2.3821+06 25.0000 184.2614 0 . 1782

25.0000 -2.6468+06 184.1087 8.6488-02

25.0000 -2.8963+06 183.9088 BUB>O.O

-2.9114+06 25.0000 181.9088 0.0

UNIT: DC-910 BLOCK: ETACDIST MODEL: RADFRAC INLETS OUTLETS

- ETACACOH STAGE 13 - ETOAC STAGE 1 ACOHPROD STAGE 23 PROPERTY OPTION SET: NRTL-RK HENRY-COMPS 10: HC-1

RENON

241

(NRTL)

/

REDLICH-KWONG

VESSELS UNIT: DC-9I0

(CONTINUED) MASS AND ENERGY BALANCE IN

***

TOTAL BALANCE

MOLE (LBMOL/HR) MASS (LB/HR ) ENTHALPY (BTU/HR

20.3117

1577.33

-0.400864E+07

***

OUT

RELATIVE DIFF .

20.3117 1577.33 -0.403129E+07

-0.144151E-11 0.562018E-02

O.OOOOOOE+OO

**********************

INPUT DATA

****

****

**********************

INPUT PARAMETERS

****

****

NUMBER OF STAGES

ALGORITHM OPTION

ABSORBER OPTION

INITIALIZATION OPTION

HYDRAULIC PARAMETER CALCULATIONS

INSIDE LOOP CONVERGENCE METHOD

DESIGN SPECIFICATION METHOD

MAXIMUM NO. OF OUTSIDE LOOP ITERATIONS

MAXIMUM NO. OF INSIDE LOOP ITERATIONS

MAXIMUM NUMBER OF FLASH ITERATIONS

FLASH TOLERANCE

OUTSIDE LOOP CONVERGENCE TOLERANCE

COL-SPECS

****

PROFILES

P-SPEC

0.0 1.80000 1,139.31

****

STAGE

1

PRES, PSI

16.0000

*******************

****

RESULTS

****

*******************

***


***

OUTLET STREAMS ETOAC COMPONENT:

ACETALD ACETONE ETHYLACE ETHANOL ***

1.0000 .99999 .99870 . 99948

ACOHPROD

.13575E-09 .60485E-05 .12975E-02 .51786E-03


***

OUTLET STREAMS ETOAC COMPONENT:

WATER HOAC

25

10

50

0.00010000 0.00010000

****

MOLAR VAPOR DIST / TOTAL DIST

MOLAR REFLUX RATIO

MASS DISTILLATE RATE LB/HR

****

23

STANDARD

NO

STANDARD

NO

BROYDEN

NESTED

.99960 .33680E-02

ACOHPROD

.40020E-03

.99663

242

VESSELS (CONTINUED) SUMMARY OF KEY RESULTS

UNIT: DC-910

***


***

LBMOL/HR LBMOL/HR LBMOL/HR LBMOL / HR

BTU/HR BTU/HR

MAXIMUM FINAL RELATI VE ERRORS

****

DEW POINT BUBBLE POINT COMPONENT MASS BALANCE ENERGY BALANCE ****

PROFILES

174.959 2 62.932 23.4457 7.28629 0.0 47.0546 1.80000 6.45796 -509,575. 486,919.

F F

**** 0.48994E-04 0.51094E-04 o .19630E-05 0.19249E-03

STAGE= 9 STAGE= 9 STAGE= 13 COMP=HOAC STAGE= 17

****

**NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS FROM THE STAGE EXCLUDING ANY SIDE PRODUCT. FOR THE FIRST STAGE, THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW. FOR THE LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW .

STAGE TEMPERATURE F 1 2 11

12 13

14 21 22 23 STAGE

1 2 11

12 13 14 21 22 23

174 . 96 182.05 187.34 189.23 192 . 92 193.35 258.62 261.71 262 . 93


PRESSURE PSI 16.000 18.000 18.900 19.000 19.100 19.200 19.900 20.000 20.100

FLOW RATE LBMOL/HR LIQUID VAPOR 23.45 O.OOOOE+OO 23.97 36.47 24 . 42 37.32 24.60 37.45 36.32 43.63 36.34 43.66 53 . 95 45.53 54.34 46.67 7.286 47.05

- 0.20137E+06 -0.20150E+06 -0 . 20078E+06 -0.20030E+06 -0.19943E+06 -0.19947E+06 -0.19347E+06 -0.19333E+06 -0.19329E+06

LIQUID

-0.18651E+06 -0.18740E+06 -0.18751E+06 -0.18738E+06 -0.18715E+06 -0.18727E+06 -0.18328E+06 -0 . 18307E+06 -0.18299E+06


MIXED


.48692+06 PRODUCT RATE LBMOL/HR VAPOR LIQUID 13.0253

1.3058 19.0057

7.2862

243

VESSELS UNIT: DC-9ID

**** STAGE

1 2 11 12 13 14 21 22 23

(CONTINUED) MASS FLOW PROFILES

FLOW RATE LB/HR LIQUID VAPOR 2051. O.OOOOE+OO 3190. 2104. 2089. 3237. 2067. 3228. 3539. 3097. 3101. 3541. 3277. 2843. 2839. 3275. 2837. 438.0

****

LIQUID


109.2235 1468.1098

438.0283

MOLE-X-PROFILE ACETONE ETHYLACE 0.11786E-02 0.98893 0.53806E-03 0.99255 0.27172E-03 0.91129 0.27028E-03 0.85736 0.24582E-03 0.75436 o .13254E-03 0.75284 0.21373E-06 0.24239E-Ol 0.53084E-07 0.76123E-02 0.12744E-07 0.22967E-02

****

STAGE 1 2 11 12 13 14 21 22 23

ACETALD 0.10365E-06 0.21081E-07 0.87037E - 08 0.86100E-08 0.64211E-08 0.15149E-08 0.33483E-14 O.OOOOOE+OO O.OOOOOE+OO

**** STAGE 1 2 11 12 13 14 21 22 23

MOLE-X-PROFILE

ACETALD 0.51813E-06 0.10365E-06 0.41839E-07 0.41730E-07 0.32639E-07 0.77086E-08 0.42922E-13 0.38672E-14 O.OOOOOE+OO

MOLE-Y-PROFILE ACETONE ETHYLACE 0.25996E-02 0.97730 0.11786E-02 0.98893 0.58811E-03 0.95722 0.58715E-03 0.93830 0.54694E-03 0.90473 0.29510E-03 0.90515 0.95972E-06 0.85087E-Ol 0.24511E-06 0.27665E-Ol 0.59330E-07 0.84354E - 02

**** STAGE 1 2 11 12 13 14

**** ETHANOL 0.39722E-03 0.18052E-03 0.11860E-03 0.13464E-03 0.15451E-03 0.12950E-03 0.38914E-05 0.12230E-05 0.36792E-06

WATER 0.76079E-02 0.31573E-02 0.18132E-02 0.19847E-02 0.21860E-02 0.15095E-02 0.39920E-04 0.15080E-04 0 . 54450E-05

****

HOAC 0.18860E-02 0.35759E-02 0.86502E-Ol 0.14025 0.24305 0.24539 0.97572 0.99237 0.99770

****

STAGE 1 2 11 12 13 14 21 22 23

MIXED

PRODUCT RATE LB / HR LIQUID VAPOR 113 9.3050

MOLE-Y-PROFILE

HOAC 0.95836E-03 0.18860E-02 0.38209E-Ol 0.57070E-01 0 . 90704E-Ol 0.91746E-Ol

244

**** ETHANOL 0.86679E-03 0.39722E-03 0.20956E-03 0.21551E-03 0.22125E-03 0 . 18542E-03 0.13513E-04 0.44416E-05 o .13555E-05

****

WATER 0.18275E-Ol 0.76079E-02 0.37707E-02 0.38288E-02 0.38001E-02 0.26232E-02 0.11525E-03 0.45302E-04 0.16572E-04

VESSELS

UNIT: DC-910 (CONTINUED)

0.91478 21 22 0 . 97228 23 0.99155 K-VALUES ACETONE ETHYLACE 2.2058 0.98824 2.1904 0.99635 2.1644 1.0504 2.1724 1.0944 2.2250 1.1993 2.2266 1.2023 4.4904 3.5104 4.6175 3.6343 4.6557 3.6728

**** STAGE 1 2 11 12 13 14 21 22 23

ACETALD 4.9987 4.9170 4.8070 4.8467 5 . 0830 5.0885 12.819 13.195 13.301

**** STAGE 1 2 11 12 13 14 21 22 23

STAGE 1 2 11 12 13 14 21 22 23

ACETALD 0.52205E-07 0.10582E-07 0.44825E-08 0.45144E-08 0.34870E-08 0 . 82281E-09 0.24288E-14 O.OOOOOE+OO O . OOOOOE+OO

MASS X-PROFILE **** ACETONE ETHYLACE 0.78258E-03 0.99615 0.35609E-03 0.99645 0.18449E-03 0.93864 0.18684E-03 0.89907 0.17600E-03 0.81932 0 . 94907E-04 0 . 81781 0.20440E-06 0.35165E-01 0.51159E-07 0.11129E-Ol 0.12312E-07 0.33661E-02

WATER 2.4021 2.4096 2.0796 1.9293 1.7385 1.7379 2.8871 3.0041 3.0436

****

MASS-X-PROFILE

**** ETHANOL 0.20921E-03 0.94760E-04 0.63874E-04 0.73824E-04 0.87747E-04 0.73556E-04 0.29520E-05 0.93493E-06 0.28195E-06

WATER 0.15670E-02 0 . 64812E-03 0.38188E-03 0.42555E-03 0.48546E-03 0.33529E - 03 0.11842E-04 0.45080E-05 0 . 16317E-05

****

HOAC 0.12949E-02 0.24469E-02 0.60728E-Ol 0.10024 0.17993 0.18169 0.96482 0.98887 0.99663 MASS-Y-PROFILE ETHYLACE ACETONE 0.17418E-02 0.99334 0.78258E-03 0.99615 0.97226 0.39378E-03 0.39556E-03 0.95894 0.37254E-03 0.93483

****

STAGE 1 2 11 12 13

ETHANOL 2.1821 2.2004 1.7670 1.6008 1.4320 1.4319 3.4724 3.6316 3.6841

HOAC 0.50813 0.52743 0.44172 0.40694 0.37320 0.37391 0.93755 0.97976 0.99383

**** STAGE 1 2 11 12 13 14 21 22 23

K-VALUES

****

ACETALD 0.26332E-06 0.52205E-07 0.21248E-07 O. 21324E- 07 0.16862E-07

245

**** ETHANOL 0.46066E-03 0.20921E - 03 0.11130E-03 o .11516E-03 0 . 11953E-03

WATER 0.37980E-02 0.15670E - 02 0.78312E-03 0.80010E - 03 0.80286E-03

VESSELS UNIT: DC-910 (CONTINUED) 0.39796E-08 14 0.30286E-13 21 22 0.28008E-14 O.OOOOOE+OO 23

0.20086E-03 0.89279E-06 0.23404E-06 0.57157E-07

MASS-Y-PROFILE

**** STAGE 1 2 11

12 13 14 21 22 23

0 . 93458 0.12007 0.40072E-01 0.12328E-01

0.10010E-03 0.99708E-05 0.33640E-05 0.10358E-05

****

HOAC 0.66393E-03 0.12949E-02 0.26452E-01 0 . 39754E-01 0.63880E-01 0.64566E-01 0.87988 0.95991 0.98767

RADFRAC REB-HCURVE: ETACDIST HCURVE 1 INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID:


DUTY

PRES

TEMP

BTU/HR

PSI

F

RENON (NRTL)

/ REDLICH-KWONG

VFRAC

!============!============!============!============! 0.0 20.1000 261.7049 0.0 294.9185 BUB>O.O 20.1000 262.0238 4.4265+04 20 . 1000 262.2445 7.7763-02 8.8531+04 20.1000 262.4033 0.1562 20.1000 1.3280+05 262.5220 0.2349 !------------+------------+------------+------------! 1.7706+05 20.1000 262.6139 0.3136 2.2133+05 20.1000 262.6872 0.3924 2.6559+05 20.1000 0.4712 262.7469 3.0986+05 20 . 1000 262.7964 0.5501 20.1000 3.5412+05 262.8382 0.6290 !-------- - ---+------------+------------+------------! 20.1000 262.8739 0 . 7080 3.9839+05 4.4265+05 ! 20.1000 ! 0.7869 ! 262.9048 ! 4.8692+05 ! 20.1000 ! 0.8659 ! 262.9318 !

RADFRAC CONDHCURVE: ETACDIST HCURVE 1 INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID:

DUTY

PRES


RENON (NRTL)

TEMP

VFRAC

246

/ REDLICH-KWONG

0.55380E-03 0.33256E-04 0 . 13417E-04 0.49521E-05

VESSELS

UNIT: DC-910

BTU/HR

(CONTINUED)

PSI

F

!============!============!============!============! 0.0 16.0000 181.6249 1 . 0000 16 . 0000 175 . 4321 DEW>1.0000 -6816.3628 16.0000 175 . 4104 -4.6325+04 0.9213 -9.2650+04 16.0000 175.3842 0.8290 16.0000 -1.3897+05 175.3565 0.7368 ------------+------------+- - ----- - ----+----------- 16.0000 -1.8530+05 175.3266 0.6446 -2.3162+05 16.0000 175.2938 0.5524 16 . 0000 -2.7795+05 175.2572 0 . 4603 16 . 0000 175.2155 -3.2427+05 0.3681 16.0000 -3.7060+05 175.1674 0.2760 !------------+-------- - ---+-- - - - -------+----------- 16.0000 -4.1692+05 175.1107 0.1839 -4.6325+05 16.0000 175.0425 9.1967-02 16.0000 174.9589 0.0 - 5.0957+05

ITEM: DE-720

BLOCK:

DECANTER MODEL: DECANTER

INLET STREAM: FIRST LIQUID OUTLET : SECOND LIQUID OUTLET: PROPERTY OPTION SET: HENRY - COMPS ID:

14

DECETAC DECWATER NRTL-RK HC-l

***

RENON (NRTL)

/ REDLICH-KWONG



818.677 36555.2 -0.123667E+09

*** OUT

RELATIVE DIFF.

818.677 36555.2 -0.123670E+09

0.111093E-14 0.186056E-06 0.233092E-04

*** INPUT DATA *** LIQUID-LIQUID SPLIT, PQ SPECIFICATION SPECIFIED HEAT DUTY - BLOCK SPEC BTU/HR 0.0 SPECIFIED PRESSURE DROP PSI 0.50000 CONVERGENCE TOLERANCE ON EQUILIBRIUM 0.10000E-03 MAXIMUM NO ITERATIONS ON EQUILIBRIUM 30 EQUILIBRIUM METHOD EQUATION-SOLVING OPTION SET OR EOS KLL COEFFICIENTS FROM KLL BASIS MOLE NO KEY COMPONENT IS SPECIFIED

OUTLET TEMPERATURE OUTLET PRESSURE CALCULATED HEAT DUTY MOLAR RATIO 1ST LIQUID /

*** RESULTS *** F PSI BTU / HR TOTAL LIQUID

LI-L2 PHASE EQUILIBRIUM COMP F HYDROGEN 0.591754 - 07 0.747201-13 C02

Xl

117.51 35.500 -2882 . 6 0.54114

X2

0.109333-06 0.136155-12

247

0.255060-10 0 . 227032 - 14

K

0.000 2 3329 0.016675

VESSELS ITEM:

ITEM:

DE-720 (CONTINUED) 0 . 00071625 ACETALD ACETONE 0 . 051802 ETHYLACE 0 . 31299 0.0051848 ETHANOL 0.57082 WATER 0.058487 HOAC

0.0011375 0.078651 0.55781 0.0068579 0.27694 0.078601

0.00021945 0.020138 0.024284 0.0032117 0.91738 0.034766

0.19293 0.25604 0.043534 0.46833 3.31255 0.44230

ST-800

BLOCK:

STRIPPER MODEL: RADFRAC

- - - - - - - - - - - - - - - - - - - - - - - - - ------

- DECWATER STEAM - 45 OUTLETS WAS WATER PROPERTY OPTION SET: HENRY-COMPS ID :

INLETS

STAGE 2 STAGE 6 STAGE 1 STAGE 6 NRTL-RK HC-l

RENON (NRTL) / REDLICH-KWONG


***


495.662 10457.0 -0.597787E+08

***

OUT

RELATIVE DIFF.

495.662 10457.0 -0.607587E+08

O.OOOOOOE+OO -0.123991E-ll 0 . 161293E-Ol

**********************

INPUT DATA

****

****

**********************

INPUT PARAMETERS

****

****

NUMBER OF STAGES ALGORITHM OPTION ABSORBER OPTION INITIALIZATION OPTION HYDRAULIC PARAMETER CALCULATIONS INSIDE LOOP CONVERGENCE METHOD DESIGN SPECIFICATION METHOD MAXIMUM NO . OF OUTSIDE LOOP ITERATIONS MAXIMUM NO . OF INSIDE LOOP ITERATIONS MAXIMUM NUMBER OF FLASH ITERATIONS FLASH TOLERANCE OUTSIDE LOOP CONVERGENCE TOLERANCE COL-SPECS **** **** MOLAR VAPOR DIST / TOTAL DIST MOLAR DISTILLATE RATE REBOILER DUTY PROFILES

****

P-SPEC

LBMOL / HR BTU/HR

1.00000 20 . 1112 0.0

****

STAGE

1

PRES, PSI

25.0000

*******************

****

RESULTS

****

*******************

***

6

STANDARD NO STANDARD NO BROYDEN NESTED 25 10 50 0.00010000 0.00010000


***

248

VESSELS ITEM: ST-800

(CONTINUED) OUTLET STREAMS -------------

45 COMPONENT: HYDROGEN ACETALD ACETONE ETHYLACE ETHANOL WATER HOAC

WASWATER

1.0000 .91236 .66785 .97572 .92295E-Ol .12820E-Ol .11172E- 02

. 86878E-27 .87637E-Ol .33215 .24277E-Ol .90771 .98718 .99888


***

TOP STAGE TEMPERATURE BOTTOM STAGE TEMPERATURE TOP STAGE LIQUID FLOW BOTTOM STAGE LIQUID FLOW TOP STAGE VAPOR FLOW BOTTOM STAGE VAPOR FLOW MOLAR REFLUX RATIO CONDENSER DUTY (W/O SUBCOOL) REBOILER DUTY ****

***

LBMOL/HR LBMOL/HR LBMOL/HR LBMOL/HR BTU/HR BTU/HR


DEW POINT BUBBLE POINT COMPONENT MASS BALANCE ENERGY BALANCE ****

PROFILES

182.052 234.068 71.1622 475.550 20.1112 109.250 3.53844 -979,980. 0.0

F F

****

O.74175E-04 0.17600E-03 0.12572E-05 o .11998E-04


4

4

4 COMP=ETHYLACE 4

****

**NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS FROM THE STAGE EXCLUDING ANY SIDE PRODUCT. FOR THE FIRST STAGE, THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW. FOR THE LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW.

STAGE TEMPERATURE F 1 2 3 4

5 6

STAGE

1 2 3 4 5 6

182.05 181.81 181.89 181.80 200.33 234.07


PRESSURE PSI 25.000 27.000 27.100 27.200 27.300 27.400

FLOW RATE LBMOL/HR VAPOR LIQUID 20.11 71. 16 91.27 481. 4 125.9 481. 5 125.9 470.4 114.9 464.8 109.3 475.6

-0.16051E+06 -0.13152E+06 -0.13007E+06 -0.12664E+06 -0.12334E+06 -0.12194E+06

LIQUID

-0.13764E+06 -0.14473E+06 -O.14006E+06 -O.13452E+06 -0.12091E+06 -0.10658E+06


MIXED



375.6616

120.0000

249

475.5504

VESSELS ITEM: ST-800 (CONTINUED) **** MASS FLOW PROFILES FLOW RATE LB/HR LIQUID VAPOR 4467. 1194. 0.1475E+05 5661. 0.1457E+05 7644. 0.1274E+05 7469. 0.1008E+05 5638. 9263. 2982.

****

STAGE

1 2 3 4 5 6

STAGE 1 2 3 4 5 6

HYDROGEN 0.37543E-13 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

LIQUID


8295.1546

2161.8336 **** MOLE-X-PROFILE ACETALD ACETONE 0.16884E-02 0.17387 0.55181E-03 0.68200E-01 0.48698E-03 0.84100E-01 0.30684E-03 0.81901E-01 0.33847E-01 0.92474E-04 0.15193E-04 0.52837E-02 MOLE-X-PROFILE HOAC

0.43113E-02

0.28063E-01

0.28444E-01

0.31350E-01

0.34845E-01

0.27432E-01

****

STAGE 1 2 3 4 5 6

STAGE 1 2 3 4 5 6

WATER 0.28135 0.77683 0.77430 0.81800 0.91485 0.96450

HYDROGEN 0.47643E-09 0.10501E-09 0.27641E-14 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

STAGE 1 2 3 4 5 6

WATER 0.29619 0.28462 0.28058 0.27099 0.40172 0.79228

STAGE 1 2 3 4 5 6

HYDROGEN 12684. 0.14523E+06 0.19771E+06 0.69594E+06 0.61458E+07 0.12434E+08

MIXED


**** MOLE-Y-PROFILE ACETALD ACETONE 0.37400E-02 0.25122 0.21405E-02 0.19091 0.24087 0.20530E-02 0.18049E-02 0.30165 0.31348 0.11935E-02 0.32729E-03 0.12100 **** MOLE-Y-PROFILE HOAC

0.72549E-03

0.35212E-02

0.36938E-02

0.51540E-02

0.14821E-01

0.28836E-01

K-VALUES ACETALD ACETONE 2.2150 l.4449 3.8786 2.7992 4.2157 2.8638 5.8833 3.6826 12.908 9.2608 21.544 22.900

****

250

9262.6785

**** ETHYLACE 0.53391 0.12230 0.10724 0.60333E-01 0.93990E-02 0.46571E-03

ETHANOL 0.48728E-02 0.40599E-02 0.54299E-02 0.81096E-02 0.69620E-02 0.23030E-02

****

**** ETHYLACE 0.44259 0.51379 0.46597 0.40834 0.24511 0.37961E-01

ETHANOL 0.55370E-02 0.50191E-02 0.68272E-02 0.12065E-01 0.23674E-01 0.19595E-01

****

**** ETHYLACE 0.82897 4.2007 4.3439 6.7661 26.073 8l.508

ETHANOL 1.1363 1.2362 1.2571 l.4875 3.3999 8.5085

VESSELS

ITEM: ST-SOO

(CONTINUED)

**** STAGE 1 2 3 4 5 6

WATER 1.0527 0.36639 0.36237 0.33127 0.43910 0.82144

K-VALUES

MASS-X-PROFILE ACETONE ACETALD 0.11851E-02 0.16089 0.79370E-03 0.12933 0.70891E-03 0 . 16141 0.49918E-03 0.17566 0.18779E-03 0.90622E-01 0.34361E-04 0.15755E - 01

****

STAGE 1 2 3 4 5 6

STAGE 1 2 3 4 5 6

STAGE 1 2 3 4 5 6

HYDROGEN 0.12058E-14 O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO O.OOOOOE+OO

WATER 0.80753E-01 0.45693 0.46094 0.54421 0.75977 0.89208

HYDROGEN 0 . 16173E-10 0.34131E-11 0.91759E-16 O.OOOOOE+OO O. OOOOOE+OO O.OOOOOE+OO

WATER 0.89851E-01 0.82673E-01 0.83237E-01 0.82293E-01 0.14747 0.52294

**** ETHYLACE 0.74947 0.35181 0.31223 0.19631 0.38175E-01 0.21066E-02

MASS-X-PROFILE **** HOAC 0.41250E-02 0.55025E-01 0.56445E-01 0.69525E-01 0.96462E-01 0.84578E-01

****

MASS-Y-PROFILE **** ACETALD ACETONE 0.27744E-02 0.24570 0.17878 0.15204E-02 0.14893E-02 0.23038 o .13403E-02 0 . 29532 0.10714E-02 0.37102 0.52826E-03 0.25748

****

MASS-Y-PROFILE HOAC 0.73364E-03 0.34095E-02 0 . 36528E-02 0.52173E-02 0.18137E-01 0.63444E-01

****

STAGE 1 2 3 4 5 6

****

HOAC 0.16827 0.12547 0.12984 0.16437 0.42527 1.0511

251

ETHYLACE 0.65665 0.72989 0.67607 0.60646 0.44008 0.12254

****

ETHANOL 0.35765E-02 0.61068E-02 0.82661E-02 o .13797E-01 0 . 14785E-01 0.54470E-02

ETHANOL 0.42954E--02 0.37282E-02 0.51793E-02 0.93697E-02 0.22224E-01 0.33074E-01

HEATERS AND HEAT EXCHANGERS ITEM: F-230

BLOCK:

FURNACE

MODEL: HEATER

INLET STREAMS: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID: ***

HOACHOT RXFEED NRTL-RK HC-1

H2HOT RENON (NRTL)

/ REDLICH-KWONG



4958.76 62974.3 -0.158187E+09 ***

INPUT DATA

TWO PHASE TP FLASH SPECIFIED TEMPERATURE SPECIFIED PRESSURE MAXIMUM NO. ITERATIONS CONVERGENCE TOLERANCE

***

OUT

RELATIVE DIFF.

4958.76 62974.3 -0.145495E+09

O.OOOOOOE+OO O.OOOOOOE+OO

-O.802334E-01

***

599.000 252.000 30 0.00010000

F

PSI

***

RESULTS

***

OUTLET TEMPERATURE F OUTLET PRESSURE PSI HEAT DUTY BTU/HR OUTLET VAPOR FRACTION V-L PHASE EQUILIBRIUM F (I) COMP HYDROGEN 0.77844 0.23541E-01 CO2 METHANE 0.18794E-01 ETHYLENE 0.61486E-02 ETHANE 0.57369E-02 ACETALD 0.28449E-02 ACETONE 0.99096E-03 ETHYLACE 0 . 20783E-02 ETHANOL 0.75496E-04 WATER 0 . 14542E-01 HOAC 0.14681

599.00 252.00 0.12692E+08 1.0000

X (I) 0.21782E-04 0.21778E-03 0.78448E-03 0.13373E-02 0.20174E-02 0.76336E-02 0.46606E-02 o .11355E-01 0.32673E-03 O.26451E-01 0.94520

Y(I) 0.77844 0.23541E-01 0.18794E-01 0.61486E-02 0.57369E-02 0.28449E-02 0.99096E-03 0.20783E-02 0.75496E-04 o .14542E-01 0.14681

ITEM: HX-200

BLOCK:

HOACHEAT MODEL: HEATX

HOT SIDE: ---------

INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID: COLD SIDE:

RXHOAC

RX2

NRTL-RK HC-1


---------INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID:

2

HOACHOT

NRTL-RK HC-1


252

K(I) 0.45846E+06 1386.7 307.34 58.983 36.481 4.7808 2 . 7277 2.3480 2.9642 7.0528 1.9926

HEATERS AND HEAT EXCHANGERS ITEM: HX-200


***


2354.84 63355.2 -0.186509E+09 ***

INPUT DATA

***

OUT

RELATIVE DIFF.

2354.84 63355.2 -0.186509E+09

O.OOOOOOE+OO O.OOOOOOE+OO 0.798951E-15

***

FLASH SPECS FOR HOT SIDE: TWO PHASE FLASH MAXIMUM NO. ITERATIONS CONVERGENCE TOLERANCE

30 0.00010000

FLASH SPECS FOR COLD SIDE: TWO PHASE FLASH MAXIMUM NO. ITERATIONS CONVERGENCE TOLERANCE

30 0.00010000

FLOW DIRECTION AND SPECIFICATION: COUNTERCURRENT HEAT EXCHANGER SPECIFIED HOT VAPOR FRACTION SPECIFIED VALUE LMTD CORRECTION FACTOR PRESSURE SPECIFICATION: HOT SIDE PRESSURE DROP COLD SIDE PRESSURE DROP

1.0000 1.00000

PSI PSI

5 . 0000 8.0000

HEAT TRANSFER COEFFICIENT SPECIFICATION: HOT LIQUID COLD LIQUID BTU/HR-SQFT-R HOT 2-PHASE COLD LIQUID BTU/HR-SQFT-R HOT VAPOR BTU/HR-SQFT-R COLD LIQUID HOT LIQUID COLD 2-PHASE BTU/HR-SQFT-R HOT 2-PHASE COLD 2-PHASE BTU/HR-SQFT-R HOT VAPOR COLD 2-PHASE BTU/HR-SQFT-R HOT LIQUID COLD VAPOR BTU/HR-SQFT-R HOT 2-PHASE COLD VAPOR BTU/HR-SQFT-R HOT VAPOR COLD VAPOR BTU/HR-SQFT-R ***

OVERALL RESULTS

149.6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937

***

STREAMS: 1

RXHOAC ----->1 T= 5.5681D+02 1 P= 2.5092D+02 1 V= 1.0000D+00 I

HOT

1

HOACHOT <-----1 T= 4.6467D+02 I P= 2.5500D+02 1 V= 1.3360D-01 1

COLD

253

1 1-----> RX2 T= 1 P= 1 V= 1 1 1<----- 2 T= 1 p= 1 V= 1

2.8014D+02 2.4592D+02 1 . 0000D+00

2.4194D+02 2.6300D+02 O.OOOOD+OO

HEATERS AND HEAT EXCHANGERS ITEM: HX-200 (CONTINUED) DUTY AND AREA:

CALCULATED HEAT DUTY CALCULATED (REQUIRED) AREA

BTU/HR SQFT

HEAT TRANSFER COEFFICIENT:

AVERAGE COEFFICIENT (DIRTY)

4305262.2823

731.4923

BTU/HR-SQFT-R

96.0740

LOG-MEAN TEMPERATURE DIFFERENCE:

LMTD CORRECTION FACTOR LMTD (CORRECTED) F PRESSURE DROP:

HOTSIDE, TOTAL COLDSIDE, TOTAL

1.0000

61.2610

PSI PSI

***

5.0000

8.0000

ZONE RESULTS

***

TEMPERATURE LEAVING EACH ZONE: HOT

I

1

RXHOAC

VAP

VAP

1

------ >

1

556.8

HOACHOT

498.21

1

1

I

BOIL

LIQ

1

<- - ---

1

280 . 1 2

1<-----

1

464.7

RX2

1------ >

1

464.21

1

241. 9

I

1

COLD ZONE HEAT TRANSFER AND AREA: ZONE 1 2

HEAT DUTY BTU/ HR

AREA SQFT

941032.235 3364230.048

HEATX COLD-HCURVE:

DTLM F

107.8474 623.6448

58.2896 36 . 0367

149.6937 149.6937

HOACHEAT HCURVE 1

INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID:


DUTY

PRES

TEMP

BTU/HR

PSI

F

RENON (NRTL)

/ REDLICH-KWONG

VFRAC

!============!============!============!============! 0.0 3.9139+05 7.8277+05 1.1742+06

AVERAGE U BTU/HR-SQFT-R

255.0000 255.0000 255.0000 255.0000

241.9905 274.3506 305.1550 334.2501

254

0.0 0.0 0.0 0.0

HEATERS AND HEAT EXCHANGERS ITEM: HX-200 (CONTINUED) 255 . 0000 1 . 5655+06 361.5443 0.0 ------------+------------+-------- - ---+----------- 1.9569+06 255.0000 387 . 0089 0.0

2 . 3483+06 255.0000 410.6693 0.0

2.7397+06 432.5909 255.0000 0.0

3.1311+06 255 . 0000 452.8610 0.0

255.0000 3.3495+06 BUB>O.O

463.4916 ------------+------------+------------+----------- 255.0000 3 . 5225+06 463 . 7365 2.3952-02 255 . 0000 3 . 913 9+06 464.2370 7 . 8545-02 4 . 3053+06 255.0000 464.6727 0.1336

HEATX HOT-HCURVE:

HOACHEAT HCURVE 1

INDEPENDENT VARIABLE: PRESSURE PROFILE: PROPERTY OPTION SET: HENRY-COMPS ID :


DUTY

PRES

TEMP

BTU/HR

PSI

F

RENON (NRTL)

/ REDLICH-KWONG

VFRAC

!============!============!============!============! 245.9153 0.0 556 . 7709 1.0000

-3.9139+05 245.9153 532.4844 1.0000

-7.8277+05 245.9153 508.0415 1.0000

-1.1742+06 245.9153 483.4375 1.0000

245.9153 -1.5655+06 458.6674 1.0000

------------+------------+------------+----------- -1.9569+06 245.9153 433.7258 1.0000

245 . 9153 408.6071 1.0000

-2.3483+06 -2.7397+06 245.9153 383.3055 1.0000

245.9153 -3.1311+06 357.8145 1.0000

245.9153 -3.5225+06 332.1279 1.0000

------------+------------+------------+---------- - -3.9139+06 245.9153 306.2390 1.0000

- 4.3053+06 245.9153 1.0000

280.1406

ITEM: HX-210 BLOCK: H2HEAT

MODEL: HEATX

HOT SIDE: INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID :

RXH2 RX3 NRTL-RK HC-l

RENON (NRTL)

/

REDLICH-KWONG

RENON

/ REDLICH-KWONG

COLD SIDE: INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS 10:

7

H2HOT NRTL-RK HC-l

255

(NRTL)

HEA TERS AND HEAT EXCHANGERS ITEM: HX-210


***


7548.63 62598.8 -0.130228E+09 INPUT DATA

***

***

OUT

RELATIVE DIFF.

7548.63 62598.8 -0.130228E+09

O.OOOOOOE+OO O.OOOOOOE+OO -0.228848E-15

***

FLASH SPECS FOR HOT SIDE: TWO PHASE FLASH MAXIMUM NO. ITERATIONS CONVERGENCE TOLERANCE

30 0.00010000


30 0.00010000

FLOW DIRECTION AND SPECIFICATION: COUNTERCURRENT HEAT EXCHANGER SPECIFIED HOT VAPOR FRACTION SPECIFIED VALUE LMTD CORRECTION FACTOR PRESSURE SPECIFICATION: HOT SIDE PRESSURE DROP COLD SIDE PRESSURE DROP

1.0000 1.00000

5.0000 8.0000

PSI PSI

HEAT TRANSFER COEFFICIENT SPECIFICATION: HOT LIQUID COLD LIQUID BTU/HR-SQFT-R HOT 2-PHASE COLD LIQUID BTU/HR-SQFT-R HOT VAPOR COLD LIQUID BTU/HR-SQFT-R HOT LIQUID COLD 2-PHASE BTU/HR-SQFT-R COLD 2-PHASE BTU/HR-SQFT-R HOT 2-PHASE HOT VAPOR BTU/HR-SQFT-R COLD 2-PHASE HOT LIQUID COLD VAPOR BTU/HR-SQFT-R HOT 2-PHASE COLD VAPOR BTU/HR-SQFT-R HOT VAPOR COLD VAPOR BTU/HR-SQFT-R ***

OVERALL RESULTS

149.6937 149.6937 149 . 6937 149 . 6937 149 . 6937 149 . 6937 149.6937 149.6937 149 . 6937

***

STREAMS :

---- > RXH2 T= 5.56810+02 P= 2.50920+02 V= 1.00000+00

HOT

-- - >

RX3 T= 2.80140+02 P= 2.45920+02 V= 1.00000+00

<---- H2HOT T= 4.77610+02 P= 2.54820+02 V= 1.00000+00

COLD

<----

7 T= P= V=

DUTY AND AREA: CALCULATED HEAT DUTY CALCULATED (REQUIRED) AREA

BTU/HR SQFT

256

8740987.0580 745.1360

2.02600+02 2.62820+02 1.00000+00

HEATERS AND HEAT EXCHANGERS ITEM: HX-210 (CONTINUED) HEAT TRANSFER COEFFICIENT: AVERAGE COEFFICIENT (DIRTY)

BTU/HR-SQFT-R

149.6937

LOG-MEAN TEMPERATURE DIFFERENCE: LMTD CORRECTION FACTOR LMTD (CORRECTED) F PRESSURE DROP: HOTSIDE, TOTAL COLDSIDE, TOTAL

1.0000 78.3649

PSI PSI

***

ZONE RESULTS

5.0000 8.0000

***

TEMPERATURE LEAVING EACH ZONE: HOT 1

VAP

RXH2

1

RX3

1------>

------>

556.8

280.1

1

1

VAP

H2HOT

1

7

1< - ----

<-----

477.6

1

202.6

1

COLD ZONE HEAT TRANSFER AND AREA: ZONE 1

HEAT DUTY BTU/HR 8740987.058

HEATX COLD - HCURVE:

H2HEAT


DTLM

AREA SQFT 745.1360

F

78.3649

AVERAGE U BTU/HR-SQFT-R 149.6937

HCURVE 1 DUTY CONSTANT NRTL-RK HC-1

DUTY

PRES

TEMP

BTU/HR

PSI

F


VFRAC

!============!============!============!============! 0.0 254.8160 202.6189 1.0000 7.9464+05 254.8160 228.0044 1.0000 1.5893+06 254.8160 253.2984 1.0000 2.3839+06 254.8160 278.5066 1.0000 3.1785+06 254.8160 303.6343 1.0000 - ---- - ------+------------+------------+------ - ---- 3.9732+06 254.8160 328.6863 1 . 0000 4.7678+06 254 . 8160 1.0000 353.6667 5.5624+06 254.8160 378.5795 1 . 0000

257

HEATERS AND HEAT EXCHANGERS ITEM: HX-2~O (CONTINUED) 6.3571+06 ! 403.4280 ! 254.8160 l . 0000 ! 7.1517+06 ! 254.8160 428.2150 ! l . 0000 ! !------------+--- - --------+------------+------------!

7.9464+06 ! 254.8160 ! 452.9430 ! l . 0000 !

254.8160 ! 477.6140 ! 8 . 7410+06 ! l . 0000 !

HEATX HOT-HCURVE:

H2HEAT


HCURVE 1

DUTY

CONSTANT

NRTL-RK RENON (NRTL) HC-1

DUTY

PRES

TEMP

BTU/HR

PSI

F

/ REDLICH-KWONG

VFRAC

!============!============!============!============! 0.0 245.9153 556.7709 1.0000

-7.9464+05 245.9153 532.4844 1.0000

-1.5893+06 245.9153 508.0415 1.0000

-2.3839+06 245.9153 483.4375 1.0000

-3.1785+06 245.9153 458.6674 1.0000

!------------+------------+------------+------------!

-3.9732+06 245.9153 433.7258 1.0000 !

-4.7678+06 408.6071 245.9153 1.0000

-5.5624+06 383.3055 245.9153 1.0000

245.9153 357.8145 -6.3571+06 1.0000

-7.1517+06 245.9153 332.1279 1.0000

!---- - -------+------------+----- - ------+------------!

! -7 . 9464+06 ! 245.9153 ! 306.2390 ! 1.0000 !

245.9153 ! 280.1406 ! 1.0000 !

! -8.7410+06 !

ITEM: HX-530

BLOCK:

SOLVHEAT MODEL: HEATX

HOT SIDE: INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID: COLD SIDE:

SOLV

SOLVCOOL

NRTL-RK RENON (NRTL) HC - 1

INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID:

CW2

CW20

NRTL-RK HC-1

*** TOTAL BALANCE MOLE (LBMOL/HR) MASS (LB/HR ) ENTHALPY (BTU/HR

RENON (NRTL)

/ REDLICH-KWONG

/ REDLICH-KWONG

MASS AND ENERGY BALANCE IN 7514.65 169733. -0.973747E+09

258

*** OUT

RELATIVE DIFF.

7514 . 65 169733. -0.973747E+09


HEATERS AND HEAT EXCHANGERS ITEM: HX-S30

(CONTINUED) ***

INPUT DATA

***

FLASH SPECS FOR HOT SIDE:

TWO PHASE FLASH

MAXIMUM NO. ITERATIONS

CONVERGENCE TOLERANCE

30 0 . 00010000

FLASH SPECS FOR COLD SIDE:

TWO PHASE FLASH

MAXIMUM NO. ITERATIONS

CONVERGENCE TOLERANCE

30 0.00010000

FLOW DIRECTION AND SPECIFICATION:

COUNTERCURRENT HEAT EXCHANGER

SPECIFIED HOT OUTLET TEMP

SPECIFIED VALUE F

LMTD CORRECTION FACTOR

PRESSURE SPECIFICATION:

HOT SIDE PRESSURE DROP COLD SIDE PRESSURE DROP

158.0000 1.00000

PSI

PSI

6.0000 8.0000

HEAT TRANSFER COEFFICIENT SPECIFICATION: HOT LIQUID COLD LIQUID BTU/HR-SQFT-R HOT 2-PHASE COLD LIQUID BTU/HR-SQFT-R HOT VAPOR COLD LIQUID BTU/HR-SQFT-R HOT LIQUID COLD 2-PHASE BTU/HR-SQFT-R HOT 2 -PHASE COLD 2-PHASE BTU/HR-SQFT-R HOT VAPOR COLD 2-PHASE BTU/HR-SQFT-R HOT LIQUID COLD VAPOR BTU/HR-SQFT-R HOT 2-PHASE COLD VAPOR BTU/HR-SQFT-R HOT VAPOR COLD VAPOR BTU/HR-SQFT-R ***

OVERALL RESULTS

149.6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937

***

STREAMS:

HOT

1 1--- -- > SOLVCOOL

COLD

P= 3.1800D+01 1 V= O.OOOOD+OO 1 1 1<----- CW2

1

SOLV ----->1 T= 2.6266D +02 1

P= 3.78000+01 1

V= 0.00000+00 1

1

CW20 <-----1 T= 1.19940+02 I P= 2.20000+01 I V= 0.00000+00

I

T=

I

T= P= V=

1 1

1

DUTY AND AREA:

CALCULATED HEAT DUTY CALCULATED (REQUIRED) AREA

BTU/HR

SQFT

HEAT TRANSFER COEFFICIENT: AVERAGE COEFFICIENT (DIRTY)

BTU/HR-SQFT-R

LOG - MEAN TEMPERATURE DIFFERENCE:

LMTO CORRECTION FACTOR

LMTD (CORRECTED) F

259

1.5800D+02

9.0000D+01 3.0000D+01 O.OOOOD+OO

3029016.5758 200.7657

14 9.6937

1.0000

100.78 80

HEATERS AND HEAT EXCHANGERS ITEM: HX-530 (CONTINUED) PRESSURE DROP: HOTSIDE, TOTAL COLDSIDE, TOTAL

PSI PSI

***

ZONE RESULTS

6.0000 8.0000

***

TEMPERATURE LEAVING EACH ZONE: HOT

SOLV SOLVCOOL ----- > 262.7

LIQ

CW20 <----- 119.9

LIQ

1------ > 1 158.0 1 1 CW2 1<----- 90.0 1 1

COLD ZONE HEAT TRANSFER AND AREA: ZONE 1

HEAT DUTY BTU!HR 3029016.576

AREA SQFT 200.7657

DTLM F

100.7880

AVERAGE U BTUjHR-SQFT-R 149.6937

SOLVHEAT HCURVE 1

HEATX HOT-HCURVE:


DUTY CONSTANT NRTL - RK HC-l

DUTY

PRES

TEMP

BTU!HR

PSI

F

RENON (NRTL)

j

REDLICH-KWONG

VFRAC

!============!============!============!============! 31. 8000 252.2654 1.4239-02

0.0 31 . 8000 -2.7537+05 252.0160 2.1447-03

-3.2425+05 31.8000 251.9706 BUB >O.O

31.8000 -5.5073+05 244.4048 0.0

-8.2610+05 31.8000 235.1265 0.0

!------------+---------- - -+------------+------------!

-1.1015+06 31.8000 225.7630 0.0

31.8000 -1.3768+06 216.3158 0.0

31.8000 206.7872 -1.6522+06 0.0

31.8000 -1.9276+06 197.1795 0 .0

31. 8000 -2.2029+06 187.4945 0.0

!------------+------------+------------+------------!

-2.4783+06 31.8000! 177.7345 0.0

! -2.7537+06 ! 31.8000 ! 167.9023 ! 0.0 31.8000 ! ! -3.0290+06 ! 158.0000 ! 0.0

260

REATERS AND HEAT EXCHANGERS ITEM: HX-710

BLOCK:

COOLDIS

MODEL: HEATX

HOT SIDE: INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID: COLD SIDE:

INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID : ***

13

14

NRTL-RK HC-1

CW3

CW30

NRTL-RK HC-1

RENON (NRTL)




16385.7 317000. -0.202855E+10

***

INPUT DATA

***

OUT

RELATIVE DIFF.

16385.7 317000. -0.202855E+10

O.OOOOOOE+OO O.OOOOOOE+OO O.OOOOOOE+OO

***

FLASH SPECS FOR HOT SIDE: FLASH TWO PHASE MAXIMUM NO. ITERATIONS CONVERGENCE TOLERANCE

30 0.00010000


30 0.00010000

FLOW DIRECTION AND SPECIFICATION: COUNTERCURRENT HEAT EXCHANGER SPECIFIED HOT OUTLET TEMP SPECIFIED VALUE F LMTD CORRECTION FACTOR PRESSURE SPECIFICATION: HOT SIDE PRESSURE DROP COLD SIDE PRESSURE DROP

113.0000 1.00000

PSI PSI

HEAT TRANSFER COEFFICIENT SPECIFICATION: HOT LIQUID COLD LIQUID BTU/HR-SQFT-R COLD LIQUID HOT 2-PHASE BTU/HR-SQFT-R HOT VAPOR COLD LIQUID BTU/HR-SQFT-R COLD 2-PHASE HOT LIQUID BTU/HR-SQFT-R COLD 2-PHASE HOT 2-PHASE BTU/HR-SQFT-R COLD 2-PHASE HOT VAPOR BTU/HR-SQFT-R COLD VAPOR HOT LIQUID BTU/HR-SQFT-R HOT 2-PHASE COLD VAPOR BTU/HR-SQFT-R COLD VAPOR HOT VAPOR BTU/HR-SQFT-R

***

/ REDLICH-KWONG

OVERALL RESULTS

***

261

3.0000 5.0000

149 . 6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937 149.6937

HEATERS AND HEAT EXCHANGERS ITEM: HX-710 STREAMS:

(CONTINUED)

----- >

13 T= P= V=

----- > 14

HOT

2.1413D+02

3.9000D+01

1.0459D-01

T= P= V=

<---- CW30 T= 1.0408D+02

P= 2.5000D+01

O.OOOOD+OO

V=

COLD

< ----- CW3

T= P= V=

DUTY AND AREA: CALCULATED HEAT DUTY CALCULATED (REQUIRED) AREA

149.6937 1.0000 55.6049

PSI PSI

***

ZONE RESULTS

9.0000D+01 3.0000D+01 O.OOOOD+OO

3689136.6989 443.2090

BTU/HR SQFT

HEAT TRANSFER COEFFICIENT: AVERAGE COEFFICIENT (DIRTY) BTU/HR-SQFT-R LOG-MEAN TEMPERATURE DIFFERENCE: LMTD CORRECTION FACTOR LMTD (CORRECTED) F PRESSURE DROP: HOTSIDE, TOTAL COLDSIDE, TOTAL

1.1300D+02 3.6000D+01 O.OOOOD+OO

3.0000 5.0000

***

TEMPERATURE LEAVING EACH ZONE: HOT 1 1

COND

13

14

1------>

------>

214.1

1

113.0

1

CW30

LIQ

1

CW3

1<-----

<-----

104.1

1

90.0

I COLD ZONE HEAT TRANSFER AND AREA: ZONE 1

HEAT DUTY BTU/HR 3689136.699

AREA SQFT 443 . 2090

262

DTLM F

55.6049

AVERAGE U BTU/HR-SQFT-R 149.6937

VAL VE, COMPRESSOR AND PUMPS ITEM: V-SOl

BLOCK:

B2

MODEL: VALVE

INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID: ***

3

DFEED NRTL-RK HC-l

RENON (NRTL)

/ REDLICH-KWONG



2598.04 105380. -0.389504E+09 ***

VALVE OUTLET PRESSURE VALVE FLOW COEF CALC.

INPUT DATA PSI

***

OUT

RELATIVE DIFF.

2598.01 105380. -0.389505E+09

o .111286E-04 0.838604E-05 0.371189E-05

***

43.5113

NO

FLASH SPECIFICATIONS: NPHASE MAX NUMBER OF ITERATIONS CONVERGENCE TOLERANCE ***

VALVE PRESSURE DROP

RESULTS PSI

2

30 0.00010000

***

186.389

ITEM: CP-4l0

BLOCK:

COMP

MODEL : COMPR


8

7

NRTL-RK HC-l

RENON (NRTL)

/ REDLICH-KWONG



4235.72 20404.3 -0.343117E+08 ***

INPUT DATA

ISENTROPIC CENTRIFUGAL COMPRESSOR

OUTLET PRESSURE PSI ISENTROPIC EFFICIENCY MECHANICAL EFFICIENCY ***

***

OUT

RELATIVE DIFF.

4235.67 20402.4 -0.327405E+08

0.971472E-05 0.926774E-04 -0 . 457894E-Ol

***

262.816

0.72000

1.00000

RESULTS ***

INDICATED HORSEPOWER REQUIREMENT BRAKE HORSEPOWER REQUIREMENT NET WORK REQUIRED ISENTROPIC HORSEPOWER REQUIREMENT CALCULATED OUTLET TEMP F ISENTROPIC TEMPERATURE F EFFICIENCY (POLYTR/ISENTR) USED OUTLET VAPOR FRACTION HEAD DEVELOPED, FT-LBF/LB

HP HP HP HP

263

616.427

616.427

616.427

443.828

202.604

188.534

0.72000

1.00000

43,033.1

VALVE, COMPRESSOR AND PUMPS ITEM: CP-4l0 (CONTINUED) INLET HEAT CAPACITY RATIO INLET VOLUMETRIC FLOW RATE , CUFT/HR OUTLET VOLUMETRIC FLOW RATE, CUFT/HR INLET COMPRESSIBILITY FACTOR OUTLET COMPRESSIBILITY FACTOR AV. ISENT . VOL. EXPONENT AV. ISENT. TEMP EXPONENT AV. ACTUAL VOL. EXPONENT AV. ACTUAL TEMP EXPONENT

1.37282 131,634. 115,460. 1.00658 1.00800 1.38721 1.37402 1.61390 1.59665

ITEM: P-110 BLOCK: HOACPUMP MODEL: PUMP INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID: ***

HOACMIX 2

NRTL-RK HC-1

RENON (NRTL)

/ REDLICH-KWONG



723.090 42571.9 -0.138556E+09 ***

INPUT DATA

***

OUT

RELATIVE DIFF.

723.090 42571.9 -0.138493E+09

O.OOOOOOE+OO O.OOOOOOE+OO

-0.457815E-03

***

263.000 1.00000

OUTLET PRESSURE PSI DRIVER EFFICIENCY FLASH SPECIFICATIONS: LIQUID PHASE CALCULATION NO FLASH PERFORMED MAXIMUM NUMBER OF ITERATIONS TOLERANCE

30 0 . 00010000

*** RESULTS VOLUMETRIC FLOW RATE CUFT/HR PRESSURE CHANGE PSI NPSH AVAILABLE FT-LBF/LB FLUID POWER HP BRAKE POWER HP ELECTRICITY KW PUMP EFFICIENCY USED NET WORK REQUIRED HP

***

719.600 248.300 1.90509 12.9947 24.9302 18.5904 0.52124 24.9302

ITEM: P-540 BLOCK: SOLVPUMP MODEL: PUMP INLET STREAM: OUTLET STREAM: PROPERTY OPTION SET: HENRY-COMPS ID: ***


SOLVCOOL SOLVENT NRTL-RK HC-1

RENON (NRTL)

/ REDLICH-KWONG

MASS AND ENERGY BALANCE IN 1550.00 62277.9 -0.245489E+09

264

***

OUT

RELATIVE DIFF.

1550 . 00 62277.9 -0.245420E+09

O.OOOOOOE+OO O . OOOOOOE+OO

- 0.283578E-03

VAL VE, COMPRESSOR AND PUMPS ITEM: P-540

(CONTINUED)

*** INPUT DATA OUTLET PRESSURE PSI DRIVER EFFICIENCY FLASH SPECIFICATIONS: LIQUID PHASE CALCULATION NO FLASH PERFORMED MAXIMUM NUMBER OF ITERATIONS TOLERANCE *** RESULTS VOLUMETRIC FLOW RATE CUFT/HR PRESSURE CHANGE PSI NPSH AVAILABLE FT-LBF/LB FLUID POWER HP BRAKE POWER HP ELECTRICITY KW PUMP EFFICIENCY USED NET WORK REQUIRED HP

***

235.000 1.00000

30 0.00010000 * **

1,055.61 203.200 64.8476 15.6000 27 . 3599 20 . 4023 0.57018 27.3599

ITEM: P-600

BLOCK:

ACOHPUMP MODEL : PUMP


ACOH ACOHFEED NRTL-RK HC-1

MASS AND ENERGY BALANCE TOTAL BALANCE MOLE (LBMOL/HR) ) MASS (LB/HR ENTHALPY (BTU/HR ***

RENON (NRTL)

***

IN

OUT

RELATIVE DIFF.

743.209 29861.6 -0.116257E+09

743.209 29861.6 -0.116244E+09

O.OOOOOOE+OO O.OOOOOOE+OO -0 . 112453E-03

INPUT DATA

***

OUTLET PRESSURE PSI DRIVER EFFICIENCY

100.000 1.00000

FLASH SPECIFICATIONS: LIQUID PHASE CALCULATION NO FLASH PERFORMED MAXIMUM NUMBER OF ITERATIONS TOLERANCE

30 0.00010000

*** RESULTS VOLUMETRIC FLOW RATE CUFT/HR PRESSURE CHANGE PSI NPSH AVAILABLE FT-LBF/LB FLUID POWER HP BRAKE POWER HP ELECTRICITY KW PUMP EFFICIENCY USED NET WORK REQUIRED HP ITEM: P-620

BLOCK:

ETACPUMP MODEL: PUMP

INLET STREAM: OUTLET STREAM:

/ REDLICH-KWONG

ETACREC ETACREC2

265

***

550 . 937 62 . 2000 0.0 2.49224 5.13808 3.83147 0.48505 5.13808

YALYE, COMPRESSOR AND PUMPS ITEM: P-620 (CONTINUED) PROPERTY OPTION SET: HENRY-COMPS ID: ***

NRTL-RK HC-1

RENON (NRTL)

/ REDLICH-KWONG


TOTAL BALANCE MOLE (LBMOL/HR) ) MASS (LB/HR ENTHALPY (BTU/HR

350.000 22326.3 -0.601971E+08 ***

INPUT DATA

***

OUT

RELATIVE DIFF.

350.000 22326.3 -0.601865E+08


***

98.0000 1.00000

OUTLET PRESSURE PSI DRIVER EFFICIENCY FLASH SPECIFICATIONS: LIQUID PHASE CALCULATION NO FLASH PERFORMED MAXIMUM NUMBER OF ITERATIONS TOLERANCE

30 0.00010000

*** RESULTS VOLUMETRIC FLOW RATE CUFT/HR PRESSURE CHANGE PSI FT-LBF/LB NPSH AVAILABLE FLUID POWER HP BRAKE POWER HP ELECTRICITY KW PUMP EFFICIENCY USED NET WORK REQUIRED HP

***

399.522 63.0000 74.7222 1 . 83054 4.16750 3.10771 0.43924 4.16750

ITEM: P-730 BLOCK: RECYPUMP MODEL: PUMP



21 20 NRTL-RK HC-1

RENON (NRTL)

/ REDLICH-KWONG

MASS AND ENERGY BALANCE IN 85.1205 5111.13 -0.137821E+08

*** INPUT DATA *** OUTLET PRESSURE PSI DRIVER EFFICIENCY FLASH SPECIFICATIONS: LIQUID PHASE CALCULATION NO FLASH PERFORMED MAXIMUM NUMBER OF ITERATIONS TOLERANCE *** RESULTS *** VOLUMETRIC FLOW RATE CUFT/HR PRESSURE CHANGE PSI NPSH AVAILABLE FT-LBF/LB FLUID POWER HP BRAKE POWER HP

266

***

OUT

RELATIVE DIFF.

85.1205 5111.13 -0.137811E+08


40.0000 1.00000

30 0.00010000 98.1015 15.3000 1.29537 0.10916 0.36921

VAL VE, COMPRESSOR AND PUMPS

(CONTINUED) ELECTRICITY KW PUMP EFFICIENCY USED NET WORK REQUIRED HP

ITEM: P-730

0 .2 7532 0.29566 0.36921

267

268

69Z

.IN3:W3:.I V.IS W3:1ROlId

:U XIUN3:ddV

270

Acetaldehyde from Acetic Acid Acetaldehyde is a versatile chemical intennediate. It is commercially made via the Wacker process, the partial oxidation of ethylene. That process is very corrOSlve, requmng expensive materials of construction. And like all oxidations, over-oxidation of the ingredient and the product reduce the yield, and convert expensive ethylene into carbon oxides. Acetic Acid, produced from inexpensive methanol, would be a good feedstock, if a selective route to acetaldehyde could be found. Because of the possible legislation of MTBE out of gasoline, there may be a worldwide glut of methanol, so any chemicals that use methanol may become much more economically attractive. But the reduction of acetic acid to acetaldehyde is notoriously difficult, because aldehydes are easier than acids to reduce. However, Eastman Chemical has developed a selective palladium catalyst that glves acetaldehyde with selectivity of up to 86% at 46% conversion. Byproducts fonned include ethanol, acetone and ethyl acetate, all of which can be sold after puri fication . Main reaction:

CH 3 -COOH + H2

Side reactions:

(1)

CH 3-COOH + H2 ~ CH 3 CH 20H + H 20

(2)

CH 3-COOH + CH 3-CH 20H

(3)

2 CH 3-COOH + 2 H2

~

CH 3 -CHO + H 20

~

~~

CH r COO-CH 2-CH 3 + H 20

CH3-CO-CH3 + CH 4 +H 20

Distillation of the product will be complicated by the existence of azeotropes between ethanol and ethyl acetate, water and ethanol, and water and ethyl acetate. And the acetic acid water and acetone-water mixtures are famous for their tangent pinches. Rigorous distillation simulations with thennodynamics that accurately predict each of these azeotropes and pinches will be required to have confidence in the design.

271

Your company has asked your group to detennine whether this new technology should be used in your Gulf Coast plant. Your job is to design a process and plant to produce 100 MM lb/yr of acetaldehyde from acetic acid, which is available on the site. Based on past experience, you know that you will have to defend any decisions you have made throughout the design, and the best defense is the economic justification. Assume a U.S. Gulf Coast location on the same site as a large chemical plant. Acetaldehyde can be sold for $0.18/Ib. However, ifMTVE is legislated out of gasoline, that price might drop to $0.12/Ib. Test your economics with both prices, and make appropriate recommendations. Hydrogen can be purchased over the plant fence for %0.50/Ib at 200 psig. Ethanol, if99.95% pure, can be sold (on an excise tax-free basis) for $2.50/gal; however, the ethanol-water azeotrope can also be sold into the fuel market for $1.60/gal. You may sell either or both grades of ethanol, depending on which is most economical to produce. Ethyl acetate can be sold for $0.60/Ib. Acetone can be sold for $0.20/Ib. You will need storage tanks, truck or railcar loading stations, etc., for each byproduct that you sell, or you may burn them in the boiler for fuel value. Byproducts sold much also meet nonnal purity specs for that chemical. All prices listed are in 2002 dollars. The plant design should be as environmentally friendly as possible. Recover and recycle process materials to the maximum economic extent. Also, energy consumption should be minimized, to the extent economically justified. The plant design must also be controllable and safe to operate. Remember that you will be there for the start-up and will have to live with whatever design decisions you have made.

References: US Patent 6,121,498 to Eastman Chemical

272

tLZ

86.,'IZI'9 -LN3-LVd S3-LV-LS G3-LINfl

:3XIGN3ddV

274

Ijllllllllill IIUII IIml

111111 11111111 lI!

United States Patent

[11]

[19]

Thstun et at )

[45J

US006121498A

6,121,498 Sep.19,2000

Patent Number: Date of Patent:

--',.,

'.

[54] . METHOD FOR PRODUCING ACETALDEHYDE F ROM ACETIC ACID

R. Pestman et al., "The formation of ketones and aldehydes from carboxylic acids, structure-activity relationship for two competitive reactions",Journal ofMolecular Catalysis, pp. 175-180, (1995).

[75] Inventors: Gerald C. Tustin; Leslie S. Depew, both of Kingsport; Nick A. Collins, Fall Branch, all of Tenn.

Z.E Pei et aI., "On the intermediates of the acetic acid reactions on oxides: an IR Study", Applied Surface Science, 103, pp. 171-182, (1996).

Assignee: Eastman Chemical Company, Kingsport, Tenn.

[73]

(List continued on next page.)

"[21]

Appl. No.: 09/069,953

[22]

Filed:

Primary Examiner-Howard C. Lee Assistant Examiner-Everett White Attorney, Agent, or Firm-Harry J. Gwinel1; Matthew W.

Apr. 30, 1998

[51] Int. CI.7 ........................... C07C 47/00; C07C 45/00; BOU 23/00; BOll 23/42 [52] U.S. Cl........................... 568/420; 568/401; 502/300;

502/326; 502/339 [58] Field of Search ..................................... 568/420, 401; 502/300, 325, 339 [56]

Smith

A method of producing acetaldehyde hydrogenates acetic

acid in the presence of an iron oxide catalyst containing between 2.5 and 90 wt % Pd, more preferably 10 and 80 wi % Pd and most preferably 20 and 60 wt % Pd. The catalyst has a specific surface area of less than 150 m 2 /g. Hydrogen and acetic acid are fed to a reactor in a hydrogen to acetic acid ratio of 2:1 to 25:1, more preferably in a hydrogen to acetic acid ratio of 3:1 to 15:1 and most preferably in a hydrogen to acetic acid ratio of 4:1 to 12:1. The hydroge nation is performed at a temperature of about 250° C. to 400° C., more preferably about 270· C. to 350° C. and most preferably about 280° C. to 325° C. The hydrogenation of acetic acid produces a partially gaseous product, and acetal dehyde is absorbed from the partially gaseous product with a solvent containing acetic acid. The gas remaining after the absorption step contains hydrogen, and tbis gas is recycled for the hydrogenation of acetic acid. .T he absorbed acetal dehyde is distilled to isolate same. After acetaldehyde is isolated. from uoreacted acetic acid and the either products via distillation, the unreacted acetic acid is separated from

the other products using azeotropic distillation. Water is

contained in the other products, and the azeotrope is an

azeotrope of ethyl acetate and water. The unreacted acetic

acid is separated in a column, and the column is controlled

to contain an ethyl acetate rich azeotrope of ethyl acetate and

wa teI.

References Cited U.S. PATENT DOCUMENTS

4,237,073 12/1980 Steppich el al. ........................ 568/401

4,268,362 5/1981 Ogawa et al. ............................ 203/28

5,059,716 10/1991 Joentgen el aL ........................ 568/426

5,306,845 4/1994 Yokohama el aI ...................... 568/449

5,336,810 8/1994 Van Geem et al. .................... 568/435

FOREIGN PATENT DOCUMENTS 0539274A1 4/1993 0700890Al 11/1996 WO 96/18458 6/1996

ABSTRACT

[57]

European PaL Off.. European PaL Off. . WlPO.

OlliER PUBLICATIONS

J. Kondo e'l al., "Infrared Study of Hydrogenation of Ben zoic Acid to Benzaldehyde on Zro z Catalysts", Bull. Chem. Soc., Jpn, pp. 3085-3090, (1993). R. Pestrnan et al., "Selective hydrogenation of acetic acid, towards acetaldehyde", Reel. Trav. Chim. Pays-Bas, 113, pp. 426-430, (1994). EJ. Groolendorst et al., "Selective Reauction of Acetic Acid to Acetaldehyde on Iron Oxides", Journal of Catalysis, 148,

pp. 261-269, (1994).

27 Claims, 2 Drawing Sheets

10

9

18

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275

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6,121,498 Page 2

OlliER PUBLICAl"10NS Pestrnan, et aI., "Identification of the Active Sites in .tbe Selective Hydorgenation of Acetic Acid to Acetaldehyde on Iron Oxide Catalysts", Journal of Catalysis, vol. 174, 1998, pp. 142-152. Pestman, et ai., "Reactions of Carboxylic Acids on Oxides", Journal of Catalysis, vol. 168, 1997, pp. 255-264.

Pavlova, et aI., "Low-Temperature Co Oxidation on Iron

Oxide Supported Palladium", React.Kinet.Catal.Lett, vol.

59, No.1, 1996, pp. 103-110.

Abstract of Japanese Patent Publication No. 9-100254A,

Apr. 15, 1997.

Chemical Abstracts, vol. 113, No.8, Aug. 20, 1990, p . 136,

Abstract No. 61684.

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METHOD FOR PRODUCING ACETALDEHYDE FROM ACETIC ACro

reaction (1) (300-400° C.). The above discussed reactions related to hydrogen and acetic acid in the vapor phase are summarized below:

BACKGROUND OF THE INVENTION 5 1. Field of the Invention The present invention relates in general to producing acetaldehyde. More specifically, the present invention relates to producing acet3.Jdehyde by hydrogenating acetic acid. 10 2. Description of the Related Art Acetaldehyde is an important industrial chemical. It has been used as a starting material for the commercial manu facture of acetic acid, acetic anhydride, cellulose acetate, other acetate esters, vinyl acetate resins, synthetic pyridine 15 derivatives, terephthalic acid, peracetic acid and pentaeryth ritol. Historically, acetaldehyde has been used to produce acetic acid, but improvements in technology have resulted in more economical acetic acid production from synthesis gas (a mixture of carbon monoxide and hydrogen). This devel 20 opment implies that it may be more economically attractive to produce acetaldehyde from acetic acid ratber than to produce acetic acid from acetaldehyde if a technically viable route existed. Acetaldehyde has been produced commercially by the 25 reaction of ethanol with air at 480° C. in the presence of a silver catalyst This process has been replaced by the current process, the Wacker oxidation of ethylene. Both of these processes start with ethylene, and the Wacker route is more direct and efficient than the ethanol oxidation route. Acetal-' 30 dehyde bas also been produced by the hydration of acety lene. This process uses mercury salts as a catalyst, and mercury handling can cause environmental and safety prob lems. The use of acetylene causes safety concerns, and the high cost of acetylene relative to ethylene has rendered this 35 process obsolete, Acetaldehyde can also be produced by reacting synthesis gas over a rhodium on silica catalyst at elevated temperature and pressure, but the selectivity to acetaldehyde is poor, and the process has never been prac ticed commercially. Acetaldehyde has also been produced 40 from tbe reaction of methanol witb synthesis gas at elevated temperature and pressure using a cobalt iodide catalyst with a group 15 promoter, but this process also has never been, practiced commercially. Although the Wacker process is the preferred commercial process at this time, it also has many 45 undesirable aspects. These include the special safety and handling problems associated witb reacting ethylene with oxygen and the very corrosive nature of the aqueous acidic cbloride-containing reaction mixtures which necessitates very expensive materials of construction. Thus a need exists 50 for an acetaldehyde synthesis that is an improvement over the existing known processes. A potentially attractive means to synthesize acetaldehyde is by the hydrogenation of acetic acid. See reaction (1) below. However the carboxylic acid group is generally 55 considered to be among the most difficult functional groups to reduce by catalytic hydrogenation. Aldehyde groups, conversely, are easily reduced by catalytic hydrogenation to alcohols. See reaction (II) below. Thus, under the conditions required to reduce a carboxylic acid, the aldehyde is often 60 not isolated in good yield because the aldehyde is further reduced to an alcohol. Furthermore, when the cart)Qxylic acid contains an a-hydrogen, conversion to a ketone, water and carbon dioxide can occur. See reaction (III) below. This reaction becomes more prevalent as the number of 65 a-hydrogens increases. Thus, aCetone can be readily formed from acetic acid at the temperatures typically used for

(I) CR,C0 2 H + H 2

....

CH,CHO +

H 20

(II) CHJCHO + H, .... CR,CR,OH

lIG 3 OO" 'c. ~ +0, 8 kcal/mole lIG4OO" c. ~ -0 ,04 kca l/mole lIG3 OO" c. ~ -0.4 kcal/mole AG 4 OO" c, ¥ +2.5 kcal/mole

(ill) 2 CH3 C02 H -. CH,COCH, + CO2 + Hp.

The hydrogenation of acetic acid to acetaldehyde and water (reaction (I) is a mildly endothermic reaction. So, the thermodynamics of this reaction improve as the temperature is increased. The subsequent reaction (II), the hydrogenation of acetaldehyde to ethanol, is exothermic, and this reaction becomes less favorable as the temperature increases. Since the equilibrium of the acetic acid hydrogenation is poor, the reaction must be run with an excess of hydrogen to achieve appreciable acetic acid conversion. Thus, on a thermody namic basis, ethanol formation will be favored at tempera tures of 300-400° C. Reaction (III), the formation of acetone, is essentially irreversible at all temperatures above 0° C. and becomes very favorable thermodynamically as the temperature is increased. Increasing the temperature signifi cantly above 400° C. will not likely improve the selectivity to tbe desired acetaldehyde product because of increasing acetone production. Other reactions, sucb as the formation of methane, carbon oxides and C2 hydrocarbons also are relevant in acetic acid hydrogenation chemistry, but are of less importance than the three reactions described above unless excessively high temperatures are used. In some circumstances, the formation of ethyl acetate presumably through ethanol as an intermediate can also lower the selectivity to the desired acetaldehyde. Thus, it appears that a IDajor challenge in producing acetaldehyde via acetic acid hydrogenation is catalyst desigIh The ideal catalyst should facilitate the initial hydro genation of acetic acid to acetaldehyde but have essentiaUy no activity for the subsequent hydrogenation to ethanol nor for the dimerization reaction producing acetone. If a catalyst has even a small activity for conversion of acetaldehyde to ethanol or for the conversion of acetic acid into acetone, tben extreme losses in acetaldehyde selectivity may occur if the reaction is operated beyond the equilibrium conversion level allowed for converting acetic acid and hydrogen into acetal dehyde and water. A need exists for a caialyst that selectively hydrogenates acetic acid to acetaldehyde. Catalyst selectivity is only one requirement for a viable acetaldehyde synthesis. The synthesis must also be operated in a manner that will allow for the facile recovery of the very volatile acetaldehyde product, the recovery of byproducts and the recycle of unconverted reactants. GeneraUy pro cesses that hydrogenate carboxylic acids to aldehydes do so under conditions of about 1 bar pressure (all pressures given berein are in terms of absolute pressures) and hydrogen to carboxylic acid ratios approaching 50/1. Although these conditions may be sufficient for nonvolatile aldehydes, they are impractical for acetaldehyde which boils at 19-20° C. Thus, a need also exists for a process that converts acetic acid into acetaldehyde in a manner that is selective and provides for the economical recovery of the acetaldehyde. In spite of the thermodynamic limitations surrOllDding the hydrogenation of carboxylic acids to aldehydes, several

27~

6,121,498

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examples of this reaction appear in the prior art. Generally these reactions are performed at about 1 bar pressure in the vapor phase in a large excess of hydrogen at temperatures ranging between 200 and 500 0 c., and the reaction is most successful with aromatic carboxylic acids or aliphatic acids containing few a-hydrogens. Van Geem et aI., in U.S. Pal. No. ~,336,81O, describe a Mn/Zn/Al oxide catalyst that converts benzoic acid to benzaldehyde in the vapor phase at 3300 C. in a large excess of hydrogen in 88.3% selectivity at 98.9% conversion . Joentgen et aI., in U.s. Pat. No. 5,059,716, describe catalyst system based on titanium or vanadium oxides in conjunction with one or more metals selected from Cr, Mo, Co, Ni, Zn, Cd and Cu for the hydrogenation of aromatic and aliphatic carboxylic acids contai.ning not more than one a-hydrogen at 325-425 0 C. at 1 bar in the presence of a large excess of hydrogen. Yokoyama et aI., in Stud. In Surf. Sci. and Cat. 1994, 90, 47-58 and in Bull Chern. Soc. Jpn. 1993, 66, 3085-3090, describe the use of zirconium oxide and modified zirconium oxide catalysts for the hydrogenation of aromatic carboxylic acids to aldehydes under similar reaction conditions. Yokoyama et al., in U.S. Pat. No. 5,306,845, also describe the use of a purified chromium oxide catalyst for the hydrogenation of both aromatic and aliphatic carboxylic acids under similar reaction conditions. This patent gives several examples of the hydrogenation of high molecular weight acids, such as stearic acid . Acetic acid is also stated to be as a suitable acid, but no examples are given. Yokoyama et al. stress that the reason for the high purity' requirement in the chromium oxide is to prevent the ketone formation reaction. Welguny et aI., in European Patent Application EP 0 700 890 (1996), describe the use of oxide-supported tin catalysts for hydrogenation of a wide variety of carboxylic acids to aldehydes under the typical high-temperature, high-hydrogen, low-pressure conditions described previously. Although acetic acid is included in the c1ainIs of tbis patent application, the only examples are for aromatic carboxylic acids and for pivalic acid. Ferrero et aI., in Europe.an Patent Application No. EP 539,274 (1993), descnbe Ru-Sn-B on alumina catalysts for hydrogena tion of a wide variety of carboxylic acids to aldehydes under the typical high-temperature high-hydrogen low-pressure conditions described previously. Although the Ferrero patent, application gives no examples for acetic acid hydrogenation, it is mentioned in the claims. Most of the Ferrero reference concerns the reduction of senecioic·· acid to prenal or the reduction of aromat ic carboxylic acids to the corresponding aldehydes. The most definitive work on the acetic acid hydrogenation to acetaldehyde is described by Ponec and coworkers in Reel. Trav. Chim. Pays-Bas 1994, 426--430, in J. Cata!' 1994,148,261-269, inJ. Molecular Catalysis A: Chemical 1995, 103, 175-180, in Applied Surface Science 1996, 103, 171-182, and in J. Cala/. 1997, 168, 255-264. These workers have proposed a working mechanism for the reac tion and have reported several examples of the conversion of acetic acid to acetaldehyde in good selectivity. The base catalysts for these reductions are partially reduced metal oxides having an intermediate metal-oxygen bond strength. Partially reduced iron oxide is the most selective metal oxide, and acetaldehyde selectivities almost as high as 80% could be obtained at 1.2 bar pressure and using a hydrogen/ acetic acid ratio=50/1 at 321 0 C. Addition of 5 wt. % Pt to this catalyst furtber increases the selectivity to acetaldehyde to over 80%. With tin oxide, the addition of the Pt about doubles the selectivity, increasing it from about 40% to about 80%. Ponec mentions inJ. Cala/. 1997,168,255-264

4 that there is an optimum Pt level, and tbat increasing the Pt level above 1.25 atomic % actually decreases the selectivity. Although the acetic acid hydrogenation process studied by Ponec and coworkers is very selective to acetaldehyde, it 5 is impractical as a commerciaiway to produce acetaldehyde. The impracticality stems from the need to isolate and collect acetaldehyde (normal boiling point-19-20° C.) from a vapor stream where it is present in maximum concentrations of 2-3% (or less, depending on tbe conversion) at about 1 10 bar pressure. Water and byproducts must be removed from the mixture, and bydrogen and unconverted acetic acid must be recycled to the reactor. These operations require that the temperature be lowered considerably from the 300--4000 C. reaction temperature. A practical process requires much 15 lower hydrogen/acetic acid ratios and much higher reaction pressures than used by Po nee. SUMMARY OF mE INVENTION 20

25

30

35

40

45

50

55

60

Accordingly, it is an object of the present invention to provide a method of producing acetaldehyde that avoids dangers associated with mercury and acetylene. It is a further object of the present invention to provide a method of producing acetaldehyde tbat avoids handling problems associated with reacting ethylene and oxygen. It is a still further object of tbe present invention to provide a method of producing acetaldehyde that avoids corrosive aqueous acidic acid chloride-containing reaction mixtures. It is another object of the present invention to provide a method for hydrogenating acetic acid with good selectivity for producing acetaldehyde . It is still another object of the present invention to provide a method for hydrogenating acetic acid that allows for easy recovery of volatile acetaldehyde. These and other objects are accomplished by a method of producing acetaldehyde that hydrogenates acetic acid in the presence of an iron oxide catalyst containing between 2.5 and 90 WI % Pd, more preferably 10 and 80 wt % Pd and most preferably 20 and 60 wt % Pd. The catalyst has a specifrc surface area of less than 150 m 2 /g. Hydrogen and acetic acid are fed to a reactor in a hydrogen to acetic acid ratio of 2:1 to 25 :1, more preferably in a hydrogen to acetic acid ratio of 3:1 to 15:1 and most preferably in a hydrogen to acetic acid ratio of 4:1 to 12:1. The hydrogenation is performed at a temperature of about 2500 C. to 400° C., more preferably about 270 0 C. to 3500 C. and most prefer ably about 2800 C. to 325 0 C. The hydrogenation of acetic acid produces a partially gaseous prod1.1ct, and acetaldehyde is absorbed from the partially gaseous product with a solvent containing acetic acid. The gas remaining after tbe absorp tion step contains hydrogen, and ,this gas is recycled for the hydrogenation of acetic acid . The absorbed acetaldehyde is distilled to isolate same. After acetaldehyde is isolated from uoreacted acetic acid and the other products via distillation, the uoreacted acetic acid is separated from the other prod ucts using azeotropic distillation. Water is contained in the other products, and the azeotrope is an azeotrope of ethyl acetate and water. The uoreacted acetic acid is separated in a column, and the column is controlled to contain an ethyl acetate rich azeotrope of ethyl acetate and water. BRIEF DESCRIPTION OF THE DRAWINGS

The invention will be readily understood by reference to 65 the following description of the specific embodiments described by way of example only, with reference to the accompanying drawings, wherein:

280

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FIG. 1 is a schematic representation of components used to produce acetaldehyde; and . · . FIG. 2 is an schematic representation of components used to recover acetic acid. DETAILED DESCRIPTION OF TIlE PREFERRED EMBODIMENTS The present invention will now be described with pre ferred embodiments and examples which are given by way of example only, not limitation. A specific embodiment of the process of the invention consists of two main sections: a reaction section and a recovery section shown schematically in FIGS. 1 and 2, respectively. Acetic acid is converted to acetaldehyde and water with excess hydrogen in the reaction section over a catalyst containing iron and palladium in a fiXed-bed reactor RX. The acetaldehyde product is recovered via distillation D after absorption A using the acetic acid-rich distillation bottoms as a solvent after cooling S. Referring to FIG. 1, stream 3 is a feed to the reactor RX containing acetic and hydrogen. Although a 1-to-1 molar ratio is stoichiometrically sufficient for producing acetaldehyde, an excess of hydrogen is supplied in feed 3. The reactor RX contains an iron oxide/palladium catalysl. Before the feed is supplied to the reactor, it is heated with furnace F and reactor preheater PH. The product of reactor RX is fed to an absorber A This product is hot and is cooled in feed effluent exchanger FE. Feed effluent exchanger FE also serves to preheat the feed 3 to the reactor. The product of reactor RX is substantially gaseous. Absorber A is used to liquify the acetaldehyde and other prodUCts. Cooled product 4 supplied to the absorber A and acetic acid feed 7 is also supplied. Acetic acid from feed 7 captures the products and allows hydrogen to pass via stream 6. A portion of the hydrogen is recycled via stream 10, recycle compressor RC and stream 13. Another portion of the hydrogen is purged via stream 9, and tbis maintains the purity of hydrogen. Recycle compressor RC compresses the hydrogen. Reactor RX and absorber A operate under pressure. The pressure in absorber A is from pressurized product in stream 4 and from pump

10

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30

35

40

PU.

,)

The liquid coming off of absorber A as stream 8 is sent to, distillation column D to recover acetaldehyde. The overhead from distillation column D is cooled via condenser C to condense same. A portion of the condensed liquid is sent back to the distillation column D as a reflux. Offgas 18 is not condensed and leaves the system shown in FIGS. 1 and 2. Acetaldehyde product comes from stream 19, and tbis also leaves apparatus shown in FIGS. 1 and 2. From the bottom of the distillation column, are-boiler RB is provided to supply the more volatile compounds back to the distillation column D. Stream 23 is acetic acid rich and is partially recycled to the absorber A. As mentioned previously, the absorption in absorber A works best at lower temperatures, and solvent cooler S is provided for this purpose. Stream 30 may contain ethyl acetate, water, acetic acid and acetone. To separate these compounds, the recovery apparatus shown schematically in FIG. 2 is employed. First, acetic acid column AC is used to separate out acetic acid. The boiling point of acetic acid is very close to that of water, and it would normally be difficult to separate these two components via distillation. To address tbis problem, ethyl acetate is fed to acetic acid column AC via stream 35. Ethyl acetate forms an azeotrope with water. The azeotrope has a boiling point significantly lower than either water or ethyl acetate. This enables separation. After acetic acid reboiler

45

50

55

60

65

281

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acetic acid is recovered from stream 33. This acetic acid may be mixed with hydrogen and fed to reactor RX via stream 3. The overhead from acetic acid column AC contains ethyl acetate, water and other products. Because water is difficult to separate from acetic acid as mentioned above·, it is important that excess water not be supplied via stream 35. For this purpose, stream 32 is condensed in decanter cooler DC and then decanted in decanter DE. The aqueous phase leaves decanter DE in stream 38, and the organic phase leaves in stream 37. A portion of stream 37 is supplied back to the acetic acid column Ae. Another portion of stream 37 is fed to azeotrope column Z via stream 39 to distill a "near" ethyl acetate-water azeotrope. The mixture is a "near" azeotrope because it does not contain the exact azeotropic ratio of ethyl acetate to water. As mentioned above, the azeotrope has a low boiling point and therefore can be removed as an overhead from azeotrope column Z. After azeo column condenser ZC, the azeotrope is indirectly recycled back to acetic acid column AC via stream 43. From the bottom of azeotrope column Z, stream 42 is supplied to ethyl acetate column E after azco column reboiler ZR. As mentioned above, excess hydrogenation of acetic acid produces ethanol. The ethanol can react with the acetic acid and produce ethyl acetate in an esterification process. This reaction occurs throughout the apparatus, whenever ethanol and acetic acid are present together. The reaction may be especially prominent when both reactants are in the liquid phase. Ethyl acetate column E separates ethyl acetate as an overhead. After ethyl acetate column condenser EC, stream 54 contains ethyl acetate which can be sold as a finished product. From the bottom of ethyl acetate column E, a somewhat small stream 55 of acetic acid is produced after ethyl acetate column reboiler ER. As mentioned above, decanter DE separates aqueous products from organic products. The aqueous stream 38 is supplied to steam stripper SS. Steam stripper SS is a distillation column heated by steam 46. Lighter organics come off the top of steam stripper SS in stream 45 and waste water comes off the bottom as stream 47. The organics in streanr45 are supplied to waste acetone column W. Acetone has a very low boiling point, even lower than the azeotrope. Thus, a waste acetone stream 51 is produced after acetone column condenser We. From the. bottom of the waste acetone column W, a near ethyl acetate-water azeotrope stream 50 is recycled after acetone column reboiler WR. The two azeotrope recycle streams 50 and 43 are not supplied directly back to the acetic acid columnAC. Instead, they are fed to decanter cooler DC . ~nd decanter DE to remove water. The processes depicted in FIGS. 1 and 2 are designed for optimum operation at the following conditions: 1) as/I molar ratio of hydrogen to acetic acid in the reactor RX feed 3, 2) byproduct ethanol is converted to ethyl acetate as dictated by chemical equilibrium at of conditions present in the bottom of the acetaldehyde recovery column D, and 3) the reactor operates at 300 0 e., 17.2 bar, and 45% acetic acid conversion with a selectivity of 89% to acetaldehyde, 5% to ethanol, 4% to acetone (and COJ, and 2% to methane and C2 hydrocarbons (ethylene plus ethane). If the degree of ethyl acetate formation from ethanol and unconverted acetic acid in the reactor RX is low, the reaction may be simply catalyzed by adding sulfuric acid to the HOAc-rich solvent before recovery. The recovery scheme shown in FIG. 2 is bigbly dependent on this conversion of byproduct ethanol to ethyl acetate and is a significant part of the present inven tion.

6,121,498

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Mass-separating agents other than ethyl acetate are pos 90 wt % Pd with the balance of the weigbt calculated as sible. Such agents may be selected from those 'organic Fe Z0 3 (the actual chemical nature of the iron mayor may not compounds that from a minimum-boiling azeotrope with be Fe2 0 3 depending on the specific method of catalyst water and separate into water-rich and organic-rich liquid synthesis used). More preferred catalysts contain between phases upon condensation. Those skilled in the art ofsepa 5 10 and 80 wt % Pd based on Fe Z0 3 • The most preferred rations may select such an alternate to ethyl acetate and catalysts contain between 20 and 60 wt % Pd based on modify the process depicted in FIG. 2 appropriately. Fe2 0 3 . Catalysts containing low amounts of palladium per However, as ethyl acetate is a coproduct of the process its form well under low-pressure high-hydrogen conditions, but use as an azeotroping agent avoids introducing another 10 may not perform well under the high-pressure low-hydrogen compound to the process and as such is used in the preferred conditions preferred in the invention. Catalysts containing embodiment. low amounts of palladium may rapidly lose their activity and selectivity under the high-pressure low-hydrogen conditions In the preferred embodiment the azeotroping agent both preferred in the invention. Excessively high amounts of forms a minimum boiling azeotrope with water and forms two liquid phases upon condensation. Potential azeotroping 15 palladium are uneconomical and may produce excessive amounts of hydrocarbons. The active components of the agents include, but are not limited to, acrylonitrile, allyl catalyst of the invention can be supported, but the support acetate, allyl acetone, allyl cyanide, benzene, I-butanol, should be unreactive for the conversion of acetic acid to l-butenylethyl ether, l-butoxy-2-propanol, butyl acetate, butyl acetoacetate, butyl acrylate, n-butyl aniline, butyl 20 acetone. The catalyst should have a surface area below 150 mZ/g. Catalysts with excessively high surface areas can benzoate, butyl butyrate, butyl chloride, butyl ether, butyl exhibit reduced selectivity to the desired acetaldehyde. The isopropenyl ether, 2-butyl octanol, butyraldehyde, catalysts of the invention may be reduced in hydrogen prior butyronitrile, carbon disulfide, carbon tetrachloride, to their use in the reaction of hydrogen and acetic acid by 2-chloroethyl ether, chloroform, chloroisopropyl ether, crotonaldehyde, cyclohexane, cyc!ohexanone, 25 contacting the catalysts with hydrogen at about between 50 and 500· C. and at about 1-50 bar pressure. More preferred cyclopentanone, diallyl acetal, diallyl amine, dibutyl acetal, pre reduction conditions are between 200 and 400 0 C. and dibutyl amine, dibutyl ethanolamine, 2,3-dichloropropanol, 1-20 bar pressure, and the most preferred pre reduction dicyclopentadiene, diethyl acetal, diethyl butyral, 0 diisobutylene, diisobutyl ketone, dimethyl butyral, 2,5 30 conditions are between 250 and 350 C. and 1-5 bar pressure. dimethyl furan, 2,6-dimethyl-4-heptanol, dimethylisobutyral, dipropyl acetal, dipropyl ketone, It is rather important that the catalyst be in a correct oxidation state, and the correct oxidation state should be epichlorohydrin, ethyl acetate, ethyl acrylate, n-ethyl aniline, ethylbenzene, 2-ethylbutanol, 2-ethylbutyl acetate, readily regenerated under the reaction conditions. If tbe 2-ethylbutyl butyrate, ethylbutyl ether, ethylbutyl ketone, 35 catalyst is in an over oxidized state, then acetone becomes 2-ethylbutyraldehyde, ethylcrotonate, ethylene dichloride, the predominant product. The selective catalysts contain a mixture of zero valent metal and metal oxide phases. If tbe ethyl formate, 2-ethylhexanol, 2-ethylhexyl acetate, catalyst is in an over reduced state, methane becomes the 2-ethythexyl amine, 2-ethylhexyl chloride, 2-ethylhexyl predominant product. Addition of Pd to the catalyst facili crotonate;2-ethylhexyl ether, ethylidene acetone, 40 tates tQe formation and maintenance of the desired oxida tion 4-ethyloctanol, ethyl propionate, heptane, 2-heptyl acetate, 3-heptyl acetate, hexaldehyde, hexane, hexanol, 2-hexenal, state. hexyl acetate, hexyl chloride, isobutyl alcohol, isophorone, The catalysts of the invention are reactive and selective isopropyl acetate, isopropylbenzene, isopropyl chloride, iso-' under a wide variety of conditions. Temperatures can range propyl ether, mesityl oxide, methacrylaldehyde, l-methoxy 45 from about 250 to 400° C. More preferred temperatures l,3-butadiene, 3-methoxybutyl acetaie, methylamyl ketone, range from 270 to 3500 c., and the most preferred tempera methylene chloride, 2-methyl-5-ethyl pyridine, 5-methyl-2 ture range is from 280 to 325 0 C. At low temperatures the hexanone, methylisobutyl ketone, methylisopropenyl rate may be low and, if the mixture is low in hydrogen, the ketone, n-methylmorpholine, 2-methyl pentanal, 2-methyl reaction can also be limited by the equilibrium restrictions pentanol, 4-methyl-2-pentanol, 4-methyl-2-pentene, 50 dictated by the thermodynamics of the reaction. Excessively 4-methyl-2-pentyl acetate, 2-methylpropyl acetate, methyl high temperature can lead to lower acetaldehyde selectivity propyl ketone, nonane, paraldebyde, pentane, 2,4 due to the formation of acetone and hydrocarbons. Pressures pentanedione, 3-pentanol, propionitrile, propyl chloride, can range from less than 1 bar to greater than 50 bars, and propylene dichloride, styrene, tetrachloroethylene, 1,4 55 the catalysts will still have excellent rates and acetaldehyde thioxane, toluene, triallyl amine, l,l,2-trichloroethane, 1,1, selectivities provided the right temperatures and hydrogen to 2-trichloroethylene, valeraldehyde, valeric acid, vinyl acetic acid ratios are used. At pressures of about 1 bar at acetate, vinylallyl ether, vinylbutyl ether, vinyl butyrate, 300 0 C. and at hydrogen to acetic acid ratio of about 40, vinyl crotonate, vinylethyl ether, vinyl-2-ethylhexyl ether, excellent rates and conversion are seen even with Fe 2 0 3 vinylisobutyl ether, vinyl isobutyrate, vinyl isopropyl ether, 60 containing no Pd. The rate and selectivity under these vinyl-2-methyl pentanoate, vinyl propionate, vinylpropyl conditions are even higher if Pd is added to the Fe Z0 3 in the ether, and m-xylene. Among these, ethyl acetate is preferred levels preferred in the present invention. However the recov since, as mentioned above, it is a coproduct and its use does ery and recycle portions of the process of the invention not introduce anotber component to the separation. 65 become impractical at these low-pressure high-hydrogen conditions. Lowering the hydrogen to acetic acid ratio at low The catalyst (in reactor RX) of the invention contains iron pressure lowers the rate and conversion to impractical levels and palladium. Catalysts can contain between about 2.5 and

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9

10

and places the catalyst in an unfavorable oxidati?o state than acetaldehyde (boiling po~nt 19-20~ C.) using a so~vent causing increased selectivity to acetone. Generally an rich in acetic acid . The conditions used III absorber A will be largely dictated by the temperature, press~re, and composJ increase in hydrogen plus acetic acid pressure increases the tion of the reactor effluent and tbe desIred aceta~dehyde rate and degree of acetic acid conversion if other conditions remain unchanged. Selectivity can also change as the pres 5 recovery. Acetaldehyde recoveries over 50% are desIred and sure is increased. Ethyl acetate, which normally is not a may be obtained by proper choice of conditions. Generally, recovery improves with decreasing temperature, increasing signillcant product at low. pressure, becomes a significant pressure, and increasing solvent feed rate. This is why the product as the pressure increases. Acetone, which can be a significant product under low-pressure low-hydrogen 10 temperature of the reactor effluent is decreased via a reactor conditions, is not a significant product at high-pressure feed-effiuent heat exchanger FE as depicted in FIG. 1. Preferably, the temperature of the effiuent will be reduced low-hydrogen conditions provided the catalyst contains below 250 0 C. prior to absorption. More preferred are about 20 wt % Pd based on Fe2 0 3 · If the catalyst contains significantly less than about 20 wt % Pd based on Fez0 3 , temperatures below 2000 C. with temperatures below 1500 then the activity and acetaldehyde selectivity of the catalyst 15 C. most preferred. rapidly deteriorate with time on stream, and acetone and ethyl acetate selectivity increase under ~igh-~ressure lowhydrogen conditions. Pressures from. acellc aCId and. h!dro gen greater than SO bars can cause Increased selectiVity to ethanol and ethyl acetate. However the use of di~uen~s ~o increase the pressure significantly above SO. bars IS Wlt~n the spirit of tbe invention. and can be done WIthout ha:mmg the selectivity. In view of the above-mentIOned considerations, the preferred pressure of acetic acid plus hydrogen for the process of the invention is between abOut 5 and 50 bars. A more preferred pressure of hydrogep plus

The pressure in absorber A is important to acetaldehyde recovery and should be as high as practically possible. This pressure should be close to that used in the reactor after taking into account pressure drops and placement of the 20 gaseous recycle compressor RC. As noted previously, cata lyst selectivity to acetaldehyde suffers when the combined . partial pressure of hydrogen and acetic acid exceeds 50 bars which effectively limits the absorber pressure to below 60 25 bar after accounting for diluents. So, a broad range of absorber pressure is S to 60 bar with pressures of 6 to 25 bars preferred.

The composition of the absorber solvent in stream 7 will acetic acid is betw~en about 5 and 30 bars, and the most . 30 depend on catalyst selectivity and .acetic acid conversion in preferred pressure IS be~een ~bout 6 an~ 20 bars. The catalysts of the lllvention are acllve under a WIde the reactor. It should contain mostly unconverted acetic acid, range of hydrogen to acetic acid ratios. The rate of the however with at least 50 wt % acetic acid ranging up to 9S wt % at' low conversion levels. Preferably the acetic acid reaction increases as the amount of hydrogen increases. The rate of reaction first increases as the amount of acetic acid content of stream 7 will be between 60 and 85 wt %. Solvent increases then decreases as the amount of acetic acid 35 rates will be dictated by the desired acetaldehyde recovery in absorber A but should range between a solvent to absorber increases further. As mentioned above excessive amounts of acetic acid at low pressure can place the. catalyst in the feed (stream 4) ratio of 0.1 to 20 wt/WI and preferably wrong oxidation state giving low rates and lllcreased selec between 1 and 10 wt/wt. . The gaseous product of stream 6 from the absorber will tivity to acetone. Acetal~ehyde can be produced at hyd~ogen 40 to acetic acid ratios rangmg from about 2:1 to SO:l.or higher. contain mostly unconverted bydrogen and light gases However, in view of the recovery and rec~cle ~0I11~ns of the formed as reaction byproducts. This stream will be largely invention, the preferred hydrogen to acellc aCid raho rangc:s, recycled to the reactor with a purge rate set to maintain a desired hydrogen purity. While none of these light gases from about 2:1 to 2S:1. More preferred hydrogen to acetic acid ratio ranges from about 3:1 to lS:l, and the most 45 have been shown to have a deleterious effect on catalyst preferred ratio ranges from 4:1 to 12:1. performance, it is expected that the hydrogen content oftbe gaseous recycle 13 should exceed SO mol % with purities The gas hourly space velocity (GHSY, vo.lumes o~ ~eactants contacting the catalyst per hour at reactIOn condilions) between 60 and 9S mol % preferred.

~

,.

depends on the other p~r~eters descnbed p~eviously. ~enerally ~e space veloc.lt~ IS chosen to proVlde the deSired converSIon. The selecuvlty to acetal~ehyde decreases as the acetic acid cODversion increases. This effect can be. ~re~ter at very .low hydr.ogen levels because once ~he equilibnum conversIOn level IS reached any further reachon converts the acetaldehyde into ethanol and ethyl acetate. Under th~ mo~t preferred conditions of temperature, hydrogen to acetic aCid " aCId pressure It..IS pre £erre d t0 ratio and hydrogen plus acehc keep the acetic acid conversion below SO% if acetaldehyde is the main product desired. If greater amounts of ethyl acetate are desired, then it is possible to operate the reaction so that the acetic acid conversion approaches 100%. Separation of the reactor eflluent into product and uncon verted reactant streams requires a number of steps. In the preferred embodiment, the firSt step is the absorption in absorber A of acetaldehyde and compounds boiling higher

The second major separation step · is recovery of the acetaldehyde via distillation in distillation column D. Col umn pressure is important for producing liquid stream 19 from this relatively low-boiling acetaldehyde component (19-200 C.) and should be as high as possible to minimize 55 refrigeration requirements in the overhead condenser. Mini mum column pressure is 1 bar with preferred pressures from 5 20 b

to ar.

50

EXAMPLES 60

The examples that follow are intended to illustrate the process of the invention and are not intended to limit the scope of tbe invention. General Experimental Methods

65

Acetic acid hydrogenations at one bar pressure were performed using a reactor system equipped with on-line gas

283

6,121,498

11

12

chromatography. Metered gas flows were provided .by six Tylan Model FC-260 mass flow controllers. Electric tem perature control and monitoring were provided by a Dow Camile® control system interfaced with a Gateway Model 2000 486DXJ33 computer. All gas delivery lines were teed into pressure relief columns containing water to prevent . accidental over pressurization. Acetic acid was fed by meter ing hydrogen or nitrogen through a temperature-controlled vaporizer containing the acetic acid. The temperature of the vaporizer was maintained by a circulating water/ethylene glycol bath. Product analysis was performed by on-line gas chromatography utilizing a Hewlett-Packard Model 3790A gas chromatograph fitted with a 6 fLxlfs inch stainless steel column containing 80/120 Carbopack B/6.6% CarbowaX® 20M. Products were analyzed by this on-line gas chromato graph with the column programmed for 80° C. for 0 minutes, 4° C./minute to 150 0 C. and 1500 C. for 0 minute using a flame ionization detector. A4-port Valco Industries sampling valve was used to send the feed mixture to the reactor or to the gas chromatograph for analysis. Two six-port Valco Industries gas chromatographic sampling valves containing 1 mL volume sample loops were used to sample the reactant stream or the product stream. All tubing lines connecting the exit of the acetic acid vaporizer, bypass valve, reactor, six-port sampling valves and the gas chromatograph.. were constructed of Ifs-inch stainless steel and were heated with temperature-controlled heating tapes to 1500 C. The three ' sampling valves were heated to 1500 using valve ovens. The reactor was constructed of main section of 8-inch longx8 mm 0.0. borosilicate glass fused to a lower section con sisting of 6-inch longx7.5 mm 0.0.-3 mm 1.0. capillary tubing. The reactor had a I-inch longx8 mm 0.0. borosili 0 cate side arm situated at 90 and 1 inch down from the top of the 8 mm 0.0. glass portion of the main reactor section. The three openings to the reactor were fitted with 2-inch long ¥.-incb 0.0. kovar metal tubing sealed to the end of the glass. Accurately weighed catalyst charges (typically 0.2 g) were loaded into the reactor by first inserting a glass or quartz wool plug from the top of the reactor into the top part, of the capillary section and then placing the catalyst charge on top of the glass or quartz wool plug. A thermocouple was inserted through the top of the reacto·r into the catalyst bed and sealed to the kovar tube with Swagelok® fittings. The reactant mixture was fed through the side arm, and the product exited at the base of the reactor. The kovar portions of the reactor inlet and outlet were connected to the stainless steel transfer lines using Swagelok® fittings. The reactor was heated with a vertically-mounied single element electric furnace containing a 12-inch long heat zone. The apparatus allowed for additional hydrogen or inert gas to be metered into the vapor stream exiting the temperature-controlled vaporizer. The acetic acid partial pressure could be con trolled by altering the temperature of the vaporizer or by adding hydrogen or inert gas to the vapor stream exiting the temperature-controlled vaporizer. The apparatus could also easily be configured to allow inert gas to be metered to the temperature-controlled vaporizer. This flexibility in setting the feed composition facilitated the study of the reaction kinetics. Normally catalysts were reduced in hydrogen (22.4 standard cubic centimeters per minute, SCeM) overnight at 3000 C. before feeding the acetic acid and hydrogen mixture.

In some cases a higher temperature was used for the reduc tion. When the reactor was idle between acetic acid hydro genation experiments with the same catalyst charge, hydro gen flow (22.4 SCCM) was maintained at 3000 C. High pressure acetic acid hydrogenation reactioIlS were performed in a reactor constructed from a 12 inch length of Hastelloy C tubing having an outer diameter of ¥. inch. All gas flow, pressure and temperature control devices were controlled by a Camile® Model 3300 process monitoring and control system interfaced with an IBM Model 750-P90 computer. Hydrogen flow was provided by a Brooks mass flow controller, and acetic acid was fed using dual ISCO high pressure syringe pumps. The device was fitted with a relief valve set for 35 bar. Pressure was controlled by a modified Research Control Valve with a pressure transducer located between the flow controller and the reactor. A 2-micron filter was placed between the reactor and the Research Control Valve. The product exiting the Research Control Valve was fed to a Valco Industries 6-port gas chromatographic sampling valve containing a 1 mL sample loop. The gas chromatographic sampling valve was inter faced to a Hewlett-Packard Model 3790A gas chroma tograph fitted with a 6 ft.XI/S inch stainless steel column containing 80/120 Carbopack B/6.6% Carbowax® 20M. Products were analyzed by this on-line gas chromatograph with the column programmed for 80 0 C. for 0 minutes, 4° C./minute to 1500 C. and 1500 C. for 0 minute using a flame ionization detector. The transfer lines, filter and Research Control Valve connecting the reactor to the gas chroma tographic sampling valve were heated to 200 0 C. by a temperature-controlled heating tape. The gas Chromato graphic sampling valve and the transfer line connecting it to the gas chromatograph were maintained at 150° C. The reactor tube was loaded to position the accurately weighed catalyst charge (typically 0.2 g) in the middle of the reactor. Quartz fines (1 inch layer), 12x20 mesh quartz chips (35 inches-layer) and quartz or glass wool plugs were placed on both sides of the catalyst charge. The entire length of the reactor was heated with a temperature-controlled heating tape. The acetic acid was delivered to the reactor via a line passing concentrically through the reactor head and about an inch into the upper portion of the heated portion of the reactor. The hydrogen delivery line and the relief valve were also fitted to the reactor head. Thus the upper portion of the heated reactor acted as an acetic acid vaporization and vapor mixing zone. Catalysts were reduced in hydrogen (25 SCCM) at 1.7 bar at 300° C. in the reactor over night or longer before feeding hydrogen and acetic acid. Reactions were started by setting the bydrogen and acetic acid feeds to the desired rates at the 1.7 bar setting and then selling the pressure to tbe desired amount. When the reactor was idle between acetic acid hydrogenation experiments with the same catalyst charge, hydrogen flow (22.4 secM) at 1.7 bar was maintained at 300° C. The following definitions apply to the specific examples: Space velocity (SV or GHSV)=volumes of gas per vol ume of catalyst per hour under reaction conditions, Space time yield (STY)agrams of product produced per liter of catalyst per hour, % acetic acid conversion=100(mmoles acetic acid reacted)/(mmoles acetic acid fed),

5

10

15

20

25

30

35

40

45

50

55

60

65

284

6,121,498

14

13

% acetic acid accountability=100(mmoles aceti>; acid Catalyst No.8: Pd sponge. Pd sponge (20 mesh, Alfa lot #00777) was used as received. recovered+mmoles acetate equivalents in products)/ (=oles aceticacid fed); Example 1 % normalized selectivity=100(mmoles product)/(total This example illustrates the effect of changing the weight mmoles all products). percentage of Pd on Fe 20 3 by large amollDts under a Catalysts stand ard set of feed conditions at one bar pressure. The The catalysts used in the examples were obtained by the example illustrates that acetic acid conversion is low when methods that follow. . the catalyst contains 0 or 100% Pd and that the selectivity to Catalyst No . 1: Fe 2 0 3 . Fe 2 03 (Aldrich, lot #DQ15808DQ, 99.98% purity) was used as received. 10 methane is high . The example also illustrates that, of tbose catalysts converting over 90% of the acetic acid, the catalyst Catalyst No. 2: 2.5% Pd on Fe20 3. A solution was containing 10 wt % Pd produces acetaldebyde at the higbest prepared from Pd(N03)2xHz0 (442 mg, Alfa lot rate and selectivity with the lowest methane selectivity. The #120982,39.9% Pd) and water (10 mL). This solution example further shows that althougb the catalyst containing was added to 20x40 mesh Catalyst No.1 (7_1607 g) 15 no Pd had the highest acetaldehyde selectivity, it also had the contained in an evaporating dish. The mixture was lowest acetic acid conversion. The relationship between dried on the steam bath and calcined in a muffle furnace acetaldehyde selectivity and conversion will become more for 4 hours at 400° C. apparent in subsequent examples. Tbe data for Example 1 were collected at a point in time when the catalyst activity Catalyst No.3: 5% Pd on Fe 20 3. A solution was prepared from Pd(N0:J2xHz0 (127 mg, Alia lot #120982, 20 was high and are presented in Table 1. 39.9% Pd) and water (2 mL). This solution was added Example 2 . to Catalyst No.1 (1.0294 g) contained in an evaporat This. example compares the performance of catalysts ing dish. The mixture was dried on the steam bath and 25 containlD~ 2.5. and 5 wt.% Pd under conditions ?~ compa calcined in a muffie furnace for 5 hours at 400° C. rable acelic aCid conversIOn. The same feed condllions used Pd F A I . .' Ca ta Iyst N0.: 4 lO ot -;0 on ez 3' so ution was pre . ' , ill Example 2 were used as lD Ex:rn:ple 1, and the data were pared from Pd(N0 )2 xH 20 (251 mg,Alfa lot #120982, 3 39.9% Pd), Fe(N03)3. 9Hz O (5.06 g, MallincJ.aOdt lot colle~ted after the catalyst a~t!Vlty had moder~ted thus L) 'T' h' I t' Vll'T'J) d t (10 allowmg for the lower conversIOns. The example illustrates #5032 n.n~. an wa er m. JO t 15 so u IOn was· th b a l " 5 m Pd' I ' th . d fr .. 'd 30 at t e cat yst contammg wt -/0 15 more se ectJve an added a separate soI utlOn prepare om cltnc aCI .. ' I C I 'al) that contalmng 2.5 wt % Pd when run at the same level of (2 .59 g, E astman Ch emlca ompany pant maten "d . Th I fu b ill h acelic aCI conversIOn. . d th e examp e rt er ustrates t at and water (5 m). L The mIxture was evaporate on e . . . . . much higher acetaldehyde selectIVIty at much hlgber acetic · d ' fIl . . steam bath to a sea Iy mass and th en calClDe ill a mu e .. . . c 5 h 4000 C aCid conversIOn can be achieved With catalysts contalDillg fu mace lor ours a t . 35 Pd than the Fe 20 3 catalyst of Example 1. The data for . Catalyst No.5: 20% Pd on Fez 0 3' A solutIOn was pre E xamp Ie 2 are presente d'ill T able 2 . pared from Pd(N03hxH 20 (501 mg, Alfa lot #120982, Example 3 39.9% Pd), Fe(N03)3.9Hz0 (5,06 g, Mallinckrodt lot #5032"KHTJ) and water (10 mL). To this solution was This example compares the performance of catalysts added a separate solution prepared from citric acid 40 conta:iJ)ing 5 and 10 wt % Pd IlDder conditions of comparable (2.23 g, Eastman Cbemical Company plant material) acetic acid conversion. The same feed conditions used in Example 3 were used as in Example 1, and the data were and water (5 mL). The mixture was evaporated on the steam bath to a scaly mass and then calcined in a muffle' collected while the catalyst activity was higbest thus allow 45 ing for the higher conversions. The example illustrates that furnace for 5 hours at 400° C. the catalyst containing 10 wt % Pd is more selective than Catalyst No.6: 40% Pd on Fe20~. A solution was pre pared from Pd(N03)2xH20 (Alpha lot #120982, 39.9% that containing 5 wt % Pd when run at the same level of acetic acid conversion. The example further illustrates tbat, Pd), Fe(N03hx9H20 (Mallinckrodt lot #5032 KJITJ) and water (10 mL). To this solution was added a at one bar pressure, the optimum performance is achieved separate solution prepared from cilric acid (Eastman 50 when the Pd level of 10 wt %. The data for Example 3 are Cbemical Company plant material) and water (5 mL). presented in Table 3. The mixture was evaporated on the steam bath to a Example 4 scaly mass and then calcined in a muffle furnace for 5 This example illustrates the effects of changing the mole hours at 400° C. The amount of Pd(N03hxH20 used in 55 fraction of acetic acid in hydrogen (XHOAJ at various space Catalyst No.5 was approximately doubled to achieve velocities on tbe performance of the 5 wt % Pd on FeZ0 3 at 40% Pd. one bar pressure. The example illustrates that high acetal Catalyst No. 7: 80% Pd on Fe20 3. A solution was pre dehyde selectivity can be achieved at higb acetic acid mole pared from Pd(N03)2xH20 (2.005 g, Alfa 101#120982, 60 fraction, but that it is difficult to obtain higber conversions 39.9% Pd), Fe(N03)3.9H20 (1.01 g, Mallinckrodt lot by lowering the space velocity when tbe acetic acid mole #5032 KHTJ) and water (lOmL). To this solution was fraction is high at one bar pressure. The data for Example 4 added a separate solution prepared from citric acid are presented in Table 4. (1.93 g, Eastman Chemical Company plant material) Example 5 and water (5 mL). The mixture was evaporated on the 65

°

steam bath to a scaly mass and then calcined in a muffle furnace for 5 hours at 400° C.

This example illustrates tbe performance of tbe 10 wI. % Pd on Fe 20 3 at 250 psig pressure and at a 5/1 bydrogenJ

285

6,121,498

15

16

acetic acid ratio as a function of time on stream. The example illustrates that good rate and acetaldehyde selec TABLE 1 tivity can be achieved, but that the rate, conversion and

Effect of a to 100 wt %Pd 00 tlle Performance of Fop, Olt21ysIS

acetaldehyde selectivity decrease after a certain time on stream. The example also illustrates that the selectivity to Wt%Pd 80 1()0

0 10 20 40 hydrocarbons is very low under the high-pressure low Calalyst /'10 . 4 7 8 5 . hydrogen conditions. The · example further illustrates that 19 96 99 % HOAc Conv. 26

98 81 ethyl acetate is a significant product under the high-pressure 280 499 157 79 45

low-hydrogen conditions. The performance data for 10 G/(l-hr) HAc 80 56 % HAc sel.' 15 4 38 35 Example 5 are presented in Table 5. 0.6 %acetone sel. 3.1 0.2 0.3 2.7 1.1 %EtOH sel. 7 38 22 50 0.4 55 Example 6 %CH., set. 10.5 2.7 8.5 62.9 95.4 8.6 0.1 0.7 3.1 % C, H. C. sel.'· 0.3 0 0.1 This example illustrates the performance of the 40 wt % 15 % HOAc acct.··· 100 100 108 107 105 100 Pd on Fe2 0 3 at 17.2 bar gauge pressure at 7/1 and 5/1 Conditions: 90 SCCM H2 containing 2 mol % HOAc, 0.2 g catalyst, 300· hydrogen/acetic acid ratios with time on stream. 1bis e. example also iliustrates that the performance of this catalyst 'Selectivities are normalized. does not deteriorate in the manner exhibited by the 10 wt % 20 "c, HydrocarlJOllS - ethylene + ethane. Pd catalyst of Example 5. The performance data for "'Acetic acid accountability. Example 6 are presented in Table 6. TABLE 2 Effect

of % Pd on tbe Performance of Fe 2 0, CatalysIS

Wt%Pd %HOAc Conv. G/(l-lu:) HAc % HAc sel.· %acetone sel. % EtOH seL %CH., sel. % C2 H. e. sel." %HOAc accl'"

25 54 597 78 0.8 15 4 .6 1.0 91

50 621 79 0.8 15 4.1 0.9 107

52 656 77 0.9 17 4.4 0.9 103

50 698 80 0.8 14 3.8 0.8 103

Cooditions: 90 SCCM H2 containing 2 mol % HOAc, 'Selectivities are normalized.

"c, Hydrocarbons - etbylene + ethane.

...Acetic acid accoun~bility.

45 59 51 48 45 674 748 694 527 662 82 84 84 73 84 0.7 0.6 0.6 1.6 0.7 12 10 9 9 18 6.1 5.2 5.7 5.9 5.9 1.6 0.7 0.6 0.7 0.6 97 101 101 102 105 0.2

g catalyst,

300'

e.

Example 7

I

J

TABLE 3 This example illustrales the integx.ated process of the 45

invention. The processing steps of the invention are depicted

Effect of % Pd 00 the Performance of Fe20, Catalysts: in FIGS. 1 and 2. The reactor (a) is loaded with a Pd/Fe2 0 3 Comparison at the 5 and 10 WI. % Levels catalyst of the invention and operated at 300° C. with a 5/1

molar hydrogen to acetic acid ratio at 17.2 bar pressure, and 50

5 10 Wt%Pd the reaction is 89% selective to acetaldehyde, 5% selective to ethanol lethyl acetate, 4% selective to acetone and C02, 98 92 97 91 % HOAc Coov. and 2% selective to hydrocarbons at 45% acetic acid con 773 994 642 779 G/(l-br) HAc version. Ethanol is converted to ethyl acetate as dictated by 52 47 68 % HAcsel." 36 the chemical equilibrium conditions in the bottom of the 55 1.0 1.0 1.1 0.9 %acetone scI. acetaldehyde recovery column (1). Optional sulfuric acid 27 44 40 39 % EtOH sel. catalyst can be used 10 facilitate the attainment of the 3.4 14 5.4 11 % CH. scI. ethanol-acetic acid-water-ethyl acetate equilibrium. The 2.6 0.6 3.7 1.0 % C, B.C. sel.·· heat and material balances for the process of the invention 60 103 103 98 98 % HOAc aeel.··· operating in this mode are provided in Tables 7 and 8. Conditions: 90 SCCM H2 conlaining 2 mol % HOAc, 0.2 g catalyst, JOO· While the invention has been descnbed in connection with the preferred embodiments and examples, it will be c. understood that modifications within the principle outlined 'Selectivities are normalized. above will be evident to those skilled in the art. Thus, the 65 "c, Hydrocarbons ~ ethylene + ethane. invention is not limited to the ·preferred embodiments and "'Acetic acid accountability. examples, but is intended to encompass such modifications.

286

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6,121,498

17

18

"

TABLE 4 Effect of Cbanging tbe Mole Fraction of Acetic Acid in Hydrogen

on the Performance of 5 wt. % Pd/Fe203

at Different Space Velocities.

5350 90 73000 0.057 38 1003 S7 1.1 8.0 3.2 0.6 86

TfOS,}nin."' SCCM H2 GHSV, hr- '

X HOAC % HOAc conv. Gf(l-br) HAc % HAc sel.·· % Acetone sel. % EtOH sel. % CH. sel. % C, R C. sel.··· % HOAc acct.····

7033 30 24000 0.095 31 283 87 1.1 6.8 4.8 0.8 82

7141 90 73000 0.095 16 497 89 0.9 5.3 3.9 0.5 91

8134 90 73000 0.026 66 740 79 0.9 15.8 3.7 0.7 92

9291 90 73000 0.20 16 899 90 1.8 5.8 1.8 0.4 95

8886 90 73000 0.20 23 523 87 2.5 7.5 2.7 0.2 81

9328 25 20000 0.20 17 338 89 3.9 4.6 1.9 0.3 96

9396 25 20000 0.20 ' ,~. ,: 26 407 89 3.0 5.4 2.2 0.6 89

Conditions: 0.2 g catalyst, 300° C. *TfOS total time on stream under hydrogen and acetic acid feed. • ·Selectivities are normalized '''c, Hydrocarbons ~ elbylene + ethane. ....Acetic acid accountability.

TABLE 5

TABLE 6 25

Effect of Tune on Stream on the Perfomance of 10 WI %

Effects of Hydrogen/Acetic Acid Ratio and Tinte on Stream on the

Pd/F~03

Performance of 40 WI % Pd/Fe203 at 250 psig.

at 250 psig aDd 5/1 Hydrogen/Acetic Acid Ratio.

TIOS min J

1739

2089

22

10

3350

970

TrOSt min

512

% HOAcConv. Gf(l-hr) HAc

2318

7

5

3530

2600

46

42

38

1530

2125

2175

H,fHOAc ;>,(

534

30

. GHSV, hr-l % HOAc Conv.

2600

% HAc sel.··

77.9

62.7

% acetone sel.

1.5

4.6

% HAc sel."

86.4

77.1

% EtOHoel.

15.0

16.2

% acetone sei.

1.7

1.3

1.5

% EtOAc sel.

4.6

15.5

% EtOH sel.

9.6

15.9

J5 .2

0.7

0.7

% EtOAc sel.

2.1

5.6

6.3

0.1

% CH. sel.

0.1

<0..1

<0.1

% C:zll C. 8el.···

0

<0.1

<0.1

ca.

% sel. % C, RC. sel.···

0.2

Gf(l-hr) HAc 35

40

ConditiollS : GHSV 12200, 300° C.

Conditions: 300° C.

'TIOS total time on stream under hydrogen and acetic acid feed. "Selectivities are normalized

"'c, Hydrocarbons -

77.0

"!TOS - total time on stream under bydrogen and acetic acid feed 45 •• Selectivities are normalized.

• "Cz

etbylene + ethane.

Hydrocarbons - ethylene + ethane.

TABLE 7 HOAc Hydrogenation Reaction Section Balance Stream

. J

11

Temperature C Pressure BAR Vapor Frnction Mole Flow KGMOUHR Mass Flow KGIHR \blume Flow M3/HR Enthalpy MJIHR Mole Flow KGMOUHR

67.3 19.0 0.848 4982 63088 6348 -3888JO

HOAC H2 HAC METHANE ACETONE ETHANOL

742.54 3742.14 33.21 358.78 2.59 0.23

18

19

23

30

31

33

36

77.6 19.0 1.000 3845 18807 5914 -57092

37.8 6.9 1.000 22 510 84 -2J48

37.8 6.9 0.000 318 13455 18 -61647

167.8 6.6 0.010 4466 183638 465 -1624722

167.8 6.6 0.010 737 30312 77 -268188

167.8 6.6 0.010 3729 153325 389 -1356535

37.8 2.8 0.000 3729 153325 155 -1397118

66.7 19.0 0.847 4982 63086 6333 -388610

15.63 3332.30 33.21 356.76 2.59 0.23

0.00 5.28 5.94 8.40 0.00 0.00

0.00 0.05 293.39 2.95 0.06 0.00

2265.66 0 .00 0.30 0.00 26.65 6.11

373.98 0.00 0.05 0.00 4.40 1.01

1891.67 0.00 0.25 0.00 22.25 5.10

1891.67 0.00 0.25 0.00 22.25 5.10

748.43 3742.14 33.21 358.76 2.59 6.12

13

287

•

6,121,498

19

20

,-.-- "

TABLE 7-continued

------ 1

HOAc Hydrogenation Reaction Section Balance Stream

ETIIEI'!£ H2O CO2 ITOAC Mass Fraction HOAC H2 HAC METHANE ACErONE ETHANOL

ETIIENE H2O CO2 ETOAC

11

13

18

19

28.43 28.98 39.37 5.89

28.43 28.98 39.37 5.89

1.28 0.11 1.49 0.00

2.18 16.85 2.61 0.00

0.7070 0.1200 0.0230 0.0910 0.0020 0.0002 0.0130 0.0080 0.0270 0.0080

0.0500 0.3610 0.0790 0.3090 0.0080 0.0008 0.0430 0.0280 0.0930 0.0280

0.0000 0.0210 0.5130 0.2840 0.0000 0.0000 0.0700 0.0040 0.1280 0.0000

23 0.00 2071.76 0.00 95.49

0.7410 0.0000 0.0001 0.0000 0.0080 0.0020 0.0000 0.2030 0.0000 0.0460

36

33

0.00 1729.78 0.00 79.73

0.00 341.98 0.00 15.76

0.7410 0.0000 0.0001 0.0000 0.0080 0.0020 0.0000 0.2030 0.0000 0.0460

0.0000 0.0000 0.9610 0.0040 0.0003 0.0000 0.0050 0.0230 0.0090 0.0000

31 .

30

0.00 1729.78 0.00 79.73

0.7410 0.0000 0.0001 0.0000 0.0080 0.0020 0.0000 0.2030 0.0000 0.0460

28.43 23.09 39.37 0.00

0.7410 0.0000 0.0001 0 .0000 0.0080 0.0020 0.0000 0.2030 0.0000 0.0460

0.7120 0.1200 0.0230 0.0910 0.0020 0.0040 0.0130 0.0070 0.0270 0.0000

TABLE 8 HOAc

Hydro~nation

Recovery Section Balance

1

2

3

5

7

8

9

12

Temperarue C Pressure BAR Vapor Fraction Mole Flow KGMOllHR Mass Flow KG/HR \-blum. Flow M3/HR Enlhalpy MJ/HR Mole Flow KGMOllHR

167.8 8.8 0.006 737.5 3032.3 61.4 -268378

96.8 2.1 1.000 1490.7 87620 22170.6 -515645

141.5 2.1 0.000 382.8 22466 24.8 -169455

43.3 . 2.1 0.000 1136.1 79762 89.5 -473168

43.3 2.1 0.000 1198.6 84156 94.4 -499232

43.3 2.1 0.000 353.3 7270 7.6 -102244

43.3 2.1 0.000 62.6 4394 4.9 -26065

102.2 2.1 0.000 16.9 1445 1.B -7813

HOAC ACETONE ETHANOL H2O ETOAC HAC Mass Fraction

374.10 4.40 1.01 342.15 15.77 0.05

25.00 82.96 9.91 238.03 779.28 0.87

26.38 87.53 10.46 251.14 822.21 0.92

2.41 4.96 1.60 336.28 798 0.05

1.38 4.57 0.55 13.11 42.93 0.05

Saeam

HOAC ACErONE ETHANOL H2O ITOAC HAC

0.7410 0.0080 0.0020 0.2030 0.0460 0.0001

28.74 8736 10.92 587.71 795.05 0.92

0.0200 0.0580 0.0060 0,1170 0.'7990 0.0005

370.36 0.00 0.00 12.47 0.00 0.00

0.9900 0.0000 0.0000 0.0100 0.0000 0.0000

0.0190 0.0600 0.0060 0.0540 0.8610 0.0005

50 What is clainled is: 1. A method of producii:Jg acetaldehyde, comprising the steps of: (a) hydrogenating acetic acid at a pressure between about 5 and 50 bars in the presence of an iron oxide catalyst containing between 20 and 90 WI % palladium to 55 produce a gaseous product; and (b) absorbing acetaldehyde from the gaseous product with a solvent containing acetic acid. 2. The method according to claim 1, wherein the catalyst contains between 20 and 80 WI % palladium. 3. The method according to claim 1, wherein the catalyst 60 contains between 20 and 60 wt % palladium. 4. The method according to claim 1, further comprising the step of supplying bydrogen and acetic acid to a reactor in a hydrogen to acetic acid ratio of 2:1 to 25:1. S.The method according to claim 1, further comprising 65 the step of supplying bydrogen and acetic acid to a reactor in a hydrogen to acetic acid ratio of 3: 1 to 15: 1.

0.0190 0.0600 0.0060 0.0540 0.8610 0.0005

0.0200 0.0400 0.0100 0.8330 0.0970 0.0003

0.0190 0.0600 0.0060 0.0540 0.8610 0.0005

1.3 6 0.09 0.01

am 15.41 0.00

0.0570 0.0040 0.0004 0.0001 0.9390 0.0000

6. The method according to claim 1, further comprising the step of supplying hydrogen and acetic acid to a reactor in a hydrogen to acetic acid ratio of 4:1 to 12: 1. 7. The method accordiIig to clainl 1, wherein the iron oxide is Fe2 0 3 • 8. The method according to claim 1, wherein the bydro genation is performed at a temperature of about 2500 C. to 400 0 C. 9. The method according to claim 1, wherein the hydro genation is performed at a temperature of about 2700 C. to 3500 C. 10. The method according to clain11, wherein the hydro 0 genation is performed at a temperature of about 280 C. to 325° C. 11. The method according to claim 1, wherein the catalyst has a specific surface area of less than 150 m2 /g. 12. The method according to claim 1, wherein the step of absorbing acetaldehyde is run at a temperature below 250 0 C.

288

6,121,498

21 .\

.(

13. The method according to claim 1, wherein tbe step of absorbing acetaldehyde is run at a iemperature below 2000 C. 14. The method according to claim 1, wherein the step of absorbing acetaldehyde is run at a temperature below 1500 C. 15.- The method according to claim 1, wherein step (b) produces a gaseous remainder containing hydrogen, the gaseous remainder being recycled to step (a) for the hydro genation of acetic acid. 16. The method according to claim 1, further comprising the step of (c) distilling the absorbed acetaldehyde from the solvent containing acetic acid. 17. The method according to claim 16, wherein step (c) is performed at a pressure of 1 bar or greater. 18. The method according to claim 16, wherein step (c) is performed at a pressure from 5 to 20 bar. 19. The method according to claim 16, wherein step (c) produces acetaldehyde product and a mixture of ethyl acetate, water, acetic acid and acetone, the method further comprising the step of (d) recovering the acetic acid from the mixture of ethyl acetate, water, acetic acid and acetone using an azeotropic distillation. 20. The method according to claim 19, wherein a hetero geneous water azeotrope is used for the azeotropic distilla tion. 21. The method according to claim 19, wherein an azeo trope of ethyl acetate and water is used for the azeotropic distillation. 22. The method according to claim 21, wherein the unreacted acetic acid is separated in a column, and the column is controlled to contain an ethyl acetate rich azeo trope of ethyl acetate and water. 23. The method according to claim 19, wherein step (a) is conducted in a reactor zone, the method further comprising the step of returning acetic acid recovered in step (d) to the reactor zone. 24. The method according to claim 19, further comprising the step of (e) recovering ethyl acetate, water and acetone

22 from tbe mixture of ethyl acetate, water, acetic acid and acetone using decantation, steam stripping and distillation . 25. Tile method according to claim 16, wherein step (c) produces acetaldehyde product and a mixture containing acetic acid, a portion of the nllxture containing acetic acid being used in step (b) as the solvent for absorbing acetal dehyde. 26. A process for the preparation and recovery of acetal dehyde comprising the steps of: 10 (a) contacting within a reactor zone hydrogen and acetic acid with a hydrogen to acetic acid molar ratio of less than 25 in the presence of an iron oxide catalyst containing between 20 and 90 wt. % palladium at temperatures between 250 and 400 0 C. and pressures 15 between 5 and 50 bar; (b) absorbing the reaction product in acetic acid-rich solvent and returning a major portion of the uncon densed gases to the reactor zone; (c) distilling the acetaldehyde from the acetic acid-rich 20 solvent; (d) recovering unconverted acetic acid by azeotropic distillation; (e) returning the recovered acetic acid to the reactor zone; 25 and (f) recovering the coproducts water, acetone and ethyl acetate by decantation, steam stripping and distillation. 27. A method of producing .acetaldehyde, comprising the steps of: 30 (a) supplying hydrogen and acetic acid to a reactor in a hydrogen to acetic acid ratio of 2:1 to 25:1; and (b) hydrogenating acetic acid in the reactor at a pressure between about 5 and 50 bars and a temperature of about 250 0 C. to 400° c., the hydrogenation being conducted 35 in the presence of an iron oxide catalyst containing between 20 and 60 WI. % palladium.

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289

Production of Acetaldehyde From Acetic Acid

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