MassTr ansf erI
CLB20804
Experiment 1
PACKED PACKED COLUMN COL UMN DISTILLAT DIS TILLATION ION PROCESS PROC ESS 1.0
OBJECTIVES •
To operate vapor – liquid separation proess usin! a Pa"ed Colu#n Distillation Unit$
2.0
•
To anal%&e anal%&e t'e e((et o( re(lu) r e(lu) ratio on separation o( et'anol*+ater s%ste#$
•
To deter#ine deter#ine t'e nu#,er o( sta!es ,% usin! MCa,e T'iele #et'od
OVERVIEW
Distillation is one o( t'e i#portant unit operations in #an% 'e#ial industries and 'as ,een used (ro# t'e ineption o( 'e#ial and proess industr%$ industr%$ Distillation is used (or t'e separation o( o#ponents in a liquid #i)ture #i)ture o( volatile onstituents$ T'e Distillation Distillation Colu#n is usuall% a vertial olu#n +'ere t'e liquid and vapor p'ases o( t'e #i)ture are #ade to #i) and approa' equili,riu#$ equili,riu#$
T'e t+o t%pes t%pes o( distil distillat lation ionss utili utili&ed &ed in indust industr% r% are ,at' ,at' and ontin ontinuou uous$ s$ -at' -at' distillation is desira,le +'en s#all quantities o( 'i!' valued 'e#ials need to ,e separated$ In a ,at' s%ste#. t'e olu#n an 'andle di((erent #i)tures ,% si#pl% 'an!in! its operatin! onditions$ In t'is la,. t'e pa"in! in t'e olu#n is ra'i! ri! !lass$ T'e distillation olu#n also ontains a ondenser. +'i' ools and ondenses t'e vapor leavin! t'e top o( t'e olu#n$ A re,oiler is onneted to t'e ,otto# o( t'e distillation distillation apparatus and it provides t'e re,oil 'eat t'at is neessar% (or distillation$
/
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
0i!ure 1 s'o+s t'e s'e#ati dia!ra# o( t'e apparatus in t'is e)peri#ent$
0i!ure 12 Pa"ed distillation olu#n
1
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
3.0
EXPERIMENTAL PROCE!RES
3.1
C"emi#$%& $n' An#i%%$r( E)*ipment& Re)*ire'2
PART A+ C$%i,r$ti-n #*re -/ et"$n-%$ter mixt*re&
C'e#ials required2 Et'anol industrial !rade$ • Deioni&ed*3ater$ • Anillar% equip#ents required2 Test Tu,e4 15 test tu,e per !roup6 • -ea"ers 475 #l6$ • Dropper • 8lass rod • Re(rato#eter •
PART A+ C$%i,r$ti-n #*re -/ Et"$n-%W$ter mixt*re&
/$ O,tain 1/ test tu,es9 la,el t'e test tu,es +it' A/ until A1/$ Total volu#e in ea' test tu,e is 15 #l$ 1$ Prepare t'e #i)ture o( et'anol and deioni&ed +ater to ea' test tu,e aordin! to volu#e indiate ,% Ta,le /$ :$ Note t'at. Stir t'e #i)ture o( solution 4A/ until A1/6 +it' !lass rod$ ;$ O,tain t'e re(rative inde) readin! (or solution in ea' tu,e usin! re(rato#eter$ 7$ Reord t'e re(rative inde) readin! (or ea' tu,e tests usin! Ta,le /$
:
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
Ta,le /2 T'e volu#e o( 'e#ial needed in ea' test tu,e Te&t t*,e
V-%*me -/ Et"$n-%m%
V-%*me -/ ei-ni4e' W$term%
A/
5
15
A1
/
/<
A:
1
/=
A;
:
/>
A7
;
/?
A?
7
/7
A>
?
/;
A=
>
/:
A<
=
/1
A/5
<
//
A//
/5
/5
A/1
//
<
A/:
/1
=
A/;
/:
>
A/7
/;
?
A/?
/7
7
A/>
/?
;
A/=
/>
:
A/<
/=
1
A15
/<
/
A1/
15
5
;
Re/r$#tie In'exRI
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
PART B+ Oper$te $p-r %i)*i' &ep$r$ti-n pr-#e&& *&in5 $ P$#6e' C-%*mn i&ti%%$ti-n !nit *n'er re/%*x r$ti-.
C'e#ials required2 Et'anol industrial !rade$ • Deioni&ed*3ater$ • Anillar% equip#ents required2 Dropper • -ea"ers 475 #l6 • Tissue • Re(rato#eter •
:$1 7ener$% &t$rt*p pr-#e'*re&. /$ Prepare 30 %itre& #i)ture o( et'anol*deioni&ed +ater ,% addin! 10 8 -/ et"$n-% (ro# total volu#e o( t'e #i)ture$ 1$ Ensure valves V39 V: $n' V; are losed$ :$ Ensure valves V29 V< and V10 are open$ ;$ Ensure t'at t'e -otto# Produt sa#plin! valve V; and Top Produt sa#plin! valve V: are losed$
7$ Slo+l% turn on t'e Coolin! 3ater CW suppl% to t'e Condenser$ Ma"e sure +ater is indeed (lo+in! t'rou!' it ,% #a"esure +ater (lo+s to t'e drain (ro# t'e Coolin! 3ater outlets$ Do not start t'e e)peri#ent until t'e Coolin! 3ater (lo+ is visi,le in t'e outlets to t'e drain$ ?$ Set +ater (lo+rate o( Coolin! 3ater CW to = L>min ,% ad@ustin! +ater (lo+ ontrol ?CV2. >$ Open valve V=. (ill t'e re,oiler vessel B1 +it' t'e :5 L Et'anol*3ater #i)tures$ =$ Close t'e valve V= and open valve V2 a(ter (inis' (ill re,oiler vessel +it' t'e :5 L Et'anol*3ater #i)tures$ <$ C'e" t'at t'e liquid level in Re,oiler vessel is satis(ator% 4Re(er to instrutor te'niian6$Ot'er+ise top up +it' t'e Et'anol – 3ater #i)ture t'rou!' t'e C'ar!e Port 4Re(er to instrutor te'niian6$ /5 Turn on t'e #ain po+er ontrol s+it'$ // Turn on t'e po+er s+it' o( t'e 'eater$ 12
S+it' on eletrial suppl% 4!reen B'eater on B,utton6$
/: Set 'eater ontroller C; to #a)i#u# settin! 4a,out 1:5 :5A6$
7
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
/; Allo+ a period o( /7 #inutes (or t'e equip#ent to #aintain t'er#al equili,riu# +it' surroundin!s$ /7 T'e unit is no+ read% to ,e used (or an e)peri#ent$
Experiment+ Oper$ti-n *n'er re/%*x r$ti- #-n'iti-n
/$ 3'en #i)ture is start to ,oil. lose valves V2$ 1$ 3'en distillate liquid is seen to (lo+ t'rou!' R1.1C. ad@ust ,ot' valve (or Re(lu) Ratio RCV1 so t'at ,ot' readin!s on R/ and R1 provide a re(lu) ratio o( /$5 (or t'e operation$ :$ Ensure t'at t'e Re(lu) Ratio is #aintained at /$5$ ;$ Collet sa#ples (or ,otto# produt (ro# valve V; and t'e over'ead produt (ro# valve V: (or ever% 7 #inutes$ 7$ O,serve t'e te#perature o( t'e re,oiler T/;$I( t'e te#perature is alread% <5 OC. redue t'e urrent o( t'e re,oiler to ,et+een 15A$ ?$ Conentration o( t'e sa#ples dra+n is #easure usin! t'e re(rative inde) #et'od >$ Reord all data o,tained in appendi) A$ =$ Repeat t'e e)peri#ent 4steps 1 to ?6.(or re(lu) ratio o( /$7 and 1$5
:$:
7ener$% &"*t @ '-n pr-#e'*re&.
/$ Ad@ust 'eater ontroller C$; to #ini#u# settin!$ 1$ S+it' o(( eletrial suppl% 4red B'eater o((F ,utton6$ :$ Turn o(( t'e po+er s+it' o( t'e re,oiler$ ;$
Turn o(( t'e Main po+er ontrol s+it'$
7$ Do not drain t'e 'ot liquid (ro# t'e Re,oiler$ I( neessar%. t'e liquid +it'in t'e s%ste# ould ,e drained onl% +'en t'e liquid is alread% ooled$ ?$ Allo+ t'e oolin! +ater to run (or so#e ti#e$
?
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
:.0 ANALSIS AN ISC!SSION
Discuss all your results. The questions below only serve as a guideline. Your discussion should not only
limit to these questions.
/$ Ma"e a #$%i,r$ti-n 5r$p" ,ased on %our data o,tained (ro# Experiment A ,% plottin! Re(rative inde) 4RI6 on t'e %*a)is a!ainst #ole (ration o( et'anol on t'e )* a)is$ 1$ Deter#ine t'e #ole (ration o( et'anol (or t'e top and ,otto# produt (or ea' re(lu) ,% re(er to ali,ration !rap'$ :$ Calulate t'e o#plete overall and o#ponent #ass ,alane o( t'e proess$ ;$ Deter#ine t'e nu#,er o( sta!es t'at our in t'e proesses (or ea' re(lu) ,% onstrut t'e !rap' MCa,e T'iele Met'od$ Equili,riu# data (or et'anol*+ater s%ste# is !iven in Appendi) A$ 7$ Disuss t'e results o,tained and e((et o( re(lu) ratio (or et'anol*+ater #i)ture separation ?$ Disuss an% possi,le errors in t'e e)peri#ent and state an% reo##endation to i#prove t'e proess$
;.0
RE?ERENCES
/$ Tre%,al. R$E$. Mass Transfer Operations, 3 rd ed., M*8ra+*ill. /<=/ 1$ MCa,e G S#it'. nit Operations of !hemical "ngineering, # th ed, M*8ra+*ill. /<<: :$ 8ean"oplis.C$ H$ $. Mass Transport $henomena, % th "d., Rine art 3inston. Ne+ Jor"$ ;$ Coulson G Ri'ardson. !hemical "ngineering. ol$ 1 Per!a#on Press. O)(ord$
>
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
APPENIX A T$,%e -/ Re&*%t&
Re/%*x r$ti-
1.0
Rota#eter readin! R/ 4L'r6
Rota#eter readin! R1 4L'r6
Te#perature T; 4oC6
Te#perature T1 4oC6
Ti#e. t 4#in6
TOP PRODUCT Re(rative inde) Mole (ration 4RI6
-OTTOM PRODUCT Re(rative inde) Mole (ration 4RI6
5 7 /5 /7 15 17 :5
Re/%*x r$ti-
1.;
Rota#eter readin! R/ 4L'r6
Rota#eter readin! R1 4L'r6
Te#perature T; 4oC6
Te#perature T1 4oC6
Ti#e. t 4#in6
TOP PRODUCT Re(rative inde) Mole (ration 4RI6
-OTTOM PRODUCT Re(rative inde) Mole (ration 4RI6
5 7 /5 /7 15 17 :5
=
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
Re/%*x r$ti-
2.0
Rota#eter readin! R/ 4L'r6
Rota#eter readin! R1 4L'r6
Te#perature T; 4oC6
Te#perature T1 4oC6
Ti#e. t 4#in6
TOP PRODUCT Re(rative inde) Mole (ration 4RI6
-OTTOM PRODUCT Re(rative inde) Mole (ration 4RI6
5 7 /5 /7 15 17 :5
<
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
APPENIX B E)*i%i,ri*m $t$ /-r Et"$n-%W$ter Mixt*re& M-%e /r$#ti-n -/ et"$n-% in %i)*i'9 x
M-%e /r$#ti-n -/ et"$n-% in $p-r9 (
5$55
5$55
5$57
5$:=
5$/5
5$7:
5$;5
5$>7
5$?5
5$><
5$=5
5$=?
5$<;
5$<;
5$<5
5$
5$<;
5$<;
5$
5$
5$<=
5$<<
/5
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
STEP B STEP TO CONSTR!CT 7RAP MCCABE TIELE METO 1.
Dra+ t'e equili,riu# urve ,ased on data !iven in Appendi) -. ,% plottin! #ole (ration o( et'anol in vapor on t'e %*a)is a!ainst #ole (ration o( et'anol in liquid on t'e )*a)is$
1$ Dra+ t'e ;7*de!ree line4 % )6 :$ Indiate distillate 4)D6. ,otto# 4)-6 and (eed 4)06 o#position on t'e !rap' ,ased on data o,tained (ro# e)peri#ent$4re(er to appendi) A6$ ;$ Dra+ t'e (eed line 4q line6$ 0or saturated liquid. t'is is a vertial line runnin! (ro# t'e (eed o#position 4)06 t'rou!' t'e equili,riu# urve$ 7$ 0or a spei(ied re(lu) ratio. r. dra+ t'e reti(%in! line 4ROL6$ T'is reti(%in! line ,e!ins at t'e point ) D on t'e ;7*de!ree line and 'as interept on %*a)is$
ROL equation2
?$ Dra+ t'e strippin! line 4SOL6 ,% onnetin! t'e intersetion o( t'e (eed line and t'e reti(%in! line and t'e point ) - on t'e ;7*de!ree line$ >$ -e!innin! at t'e point ) D on t'e reti(%in! line. dra+ a 'ori&ontal line to t'e equili,riu# urve and t'en a vertial line to t'e operatin! 4reti(%in! or strippin!6 line$ =$ Repeat step > (or#in! a stairase until %ou rea' or pass t'e point ) - on t'e ;7*de!ree line$ <$ Ea' point +'ere t'e stairase intersets t'e equili,riu# urve denotes one sta!e in t'e olu#n$
//
NA/Exp1/SEPT2014
MassTr ansf erI
CLB20804
S$mp%e 7r$p" -/ M#C$,e T"ie%e Met"-'
/1
NA/Exp1/SEPT2014
