SEPARATION PROCESSES I LABORATORY

TABLE OF CONTENTS

1.

Introduction

2.

Rules and safety precautions in laboratory

3.

Report and evaluation

4.

Experiment 1: Packed distillation column

Experiment 2: !ubble cap distillation column

".

Experiment 3: Packed absorption column # Rasc$i% rin%

&.

Experiment 4: Packed absorption column # Intalox saddle

'.

Experiment : Parallel#flo( plate $eat exc$an%er

).

Experiment ": *i+uid#li+uid Extraction

1,. Experiment &: Packed reactor column for acetone#(ater separation system

1.

INTRODUCTION

-nit .peration 1 laboratory syllabus contains six experimental e+uipments. /ll t$e e+uipments are prepared to instill a clear understandin% of t$e concepts and principles learnt in -nit .peration 1 course. /ll t$e related t$eories (ill be fully utili0ed in t$is laboratory.

1tudents (ill be exposed to t$e application of t$e semi#industry scale e+uipments as a preparation before t$ey (ork in t$e actual process. !esides2 t$is sub3ect (ill also %ive t$em practical and informative exposure about operational mec$anisms of a separation system2 ($ic$ is also a basis in c$emical en%ineerin% based industries.

4$e ot$er important element t$at (ill be emp$asi0ed in t$is sub3ect is team (orkin%. !esides promotin% communications and positive interactions amon% students and (it$ t$e tec$nicians2 t$e laboratory5s environment is also conducive and suitable in trainin% t$e students to $ave %ood leaders$ip and time mana%ement skills2 as (ell as in s$apin% t$em to be a responsible and disciplined person in any %iven situation. 6it$ t$ese proactive attitudes2 t$e aim of creatin% professionalism at (ork can be ac$ieved.

In order to be a successful process en%ineer2 a student s$ould $ave a clear vision and make t$e best use of t$is sub3ect to %ain as muc$ kno(led%e and experience as possible.

2.

RULES AND SAFETY PRECAUTIONS IN LABORATORY

General rules

1. 2. 3.

Every student must (ear a lab coat and s$oes 7slippers or sandals are totally pro$ibited8 and al(ays be in a %ood manner. 4ables and experimental surroundin%s must al(ays be in a clean and or%ani0ed condition and s$ould be placed in order before leavin% t$e laboratory. /ll t$e specific safety precautions in t$e laboratory must be obeyed.
4

4. . ". &.

1tudents s$ould be responsible on t$e e+uipments t$at t$ey use. /ll students are pro$ibited from smokin%2 drinkin% or eatin% in t$e laboratory. Pay attention and be careful ($en runnin% t$e experiment to %overn t$e accuracy of t$e results and to avoid accidents. 1tudents are not allo(ed to run experiment after t$e sc$eduled time except for cases ($ere it is ordered by t$e supervisor and t$e student is monitored by lecturer9supervisor9laboratory assistant9tec$nician. /ll litters and (astes from t$e experiment must be t$ro(n a(ay in a dust bin or a special desi%nated area. :o not t$ro( litters and (astes in (as$bin or urinal. :o not make noise in t$e laboratory. 4$e students must familiari0e t$emselves (it$ t$e location of emer%ency aids e.%. fire extin%uis$er2 emer%ency s$o(er etc. /ny accident must be reported immediately and verbally to lecturer9supervisor9laboratory assistant9tec$nician. Experimental data must be endorsed by lecturer9supervisor9laboratory assistant9tec$nician after t$e experiment.

'. ). 1,. 11. 12.

Safety attire

1.

;ake sure t$at you (ear proper safety e+uipment9measure ($en runnin% t$e experiment. ;ost of t$e experiments t$at you (ill be dealin% (it$ involve c$emicals2 $i%$ temperature and pressure. 4$erefore2 %o%%le must be put on to protect your eyes. 1afety $elmet must be used if you need to climb e.%. distillation column to collect data and record your observation.

2.

Laboratory equipments

1.

1tudents are pro$ibited from usin% t$e experimental e+uipments before receivin% a compre$ensive explanation from lecturer9laboratory assistant. 4$is is not only
5

dan%erous to t$e student $imself9$erself or ot$ers in t$e laboratory2 but can also dama%e t$e e+uipments. 2. 3. 4. . !efore usin% t$e e+uipments2 make sure of t$e appropriate9correct po(er source and plu% for t$e e+uipments. 1ensitive e+uipments cannot be moved. -se t$e e+uipments in t$e desi%nated area. /ny dama%e to t$e e+uipment ($ile usin% it must be reported immediately to t$e responsible laboratory assistant9tec$nician. :o not try to repair it yourself. 1tudents are forbidden from usin% dama%ed e+uipments.

Disposal of laboratorys wastes

1. 2.

1tudents are $eld responsible for cleanin% t$e table area2 e+uipments t$at t$ey used as (ell as t$e surroundin%s to avoid $a0ards to ot$er users. 6astes must be properly labeled and disposed in a desi%nated area.

Electricity, gas and others

1.

/ll sources of %as2 fuel and %as flo( valve must be turned off ti%$tly before leavin% t$e laboratory and ($en t$ey are not in use. 4$e cover of a fume c$amber must be lo(ered to t$e lo(est level. ;ake sure t$e ri%$t po(er source is used (it$ t$e e+uipment to be en%a%ed. E+uipments ($ic$ are not in use must be s(itc$ed off. If you intend to leave an operatin% e+uipment2 make sure t$e e+uipment can operate safely. 1tudents also need to inform t$eir absence to t$e laboratory assistant or tec$nician.

2. 3.

Attendance

1.

1tudents are mandatory to participate in all t$e outlined experiments. 1tudents (ill be failed if t$ey do not attend even one experiment. 1tudents are also re+uired to si%n an attendance record. 1tudents must come to t$e laboratory 1, minutes earlier before t$e experiments starts2 (ell prepared and or%ani0ed. Eac$ experiment (ill take around 2 $ours. 1tudents (ill be divided into several %roups. / supervisor (ill conduct t$e class and (ill be assisted by tec$nician or laboratory assistant. 4$e time allocation for t$e experiment is as follo(s:

2. 3.

a8 4$e first 1, minutes 1tudents briefly read t$e experimental procedure and t$eory as (ell as identifyin% t$e e+uipments needed. b8 4$e next 1. $ours 1tudents run t$e experiment. c8 4$e last 2, minutes 1tudents clean up t$e (orkin% area and t$e e+uipments used.

4.

4o ensure t$e experiment %oes smoot$ly2 students are re+uired to read and understand t$e (ork procedure and experimental t$eory before t$e class.

Report e aluation

i)

Report evaluatio !"#e$e

Eac$ student or %roup must prepare a report (it$in 1 (eek from t$e date of t$e experiment. / report submitted later t$an 3 days (ill not be accepted or (ill be penali0ed.

4$e overall mark of t$e report is ',< and anot$er 2,< comes from t$e final examination. 4$e date2 time and venue of t$e examination (ill be announced once after all t$e experiments are completed.

ii)

For$at o% t#e report $ar&i '

=ormat of t$e report >over pa%e /bstract Introduction *iterature study9t$eory ;et$odolo%y9procedure Results and discussions >onclusions Recommendations References Professionalism 4otal

< # 1, 1, 1,

3, 1

1, 1,,

(.

REPORT AND E)ALUATION

1cientific report (ritin% is an important mode of communication for all en%ineers and scientists. In researc$2 an effective report enables ot$ers to be exposed to t$e experiments t$at $ave been conducted and t$e related ne( findin%s. In en%ineerin%2 documentation is a must for furt$er advanced studies and as a support for t$e ne( experiment besides providin% information to be disseminated. It is t$erefore vital for a student to (rite a report ($ic$ is clear2 simple2 based on format and usin% t$e ri%$t %rammars.

/ll reports must be prepared usin% 6ord Processin% soft(are suc$ as ;icrosoft 6ord2 *otus or ot$er computer soft(are e.%. ;icrosoft Excel2 Po(erPoint. ;atematica2 ;atlab2 1tatistica2 /uto>ad and ot$ers can also be used to dra( tables2 %rap$s and dia%rams.

4$e purpose of report (ritin% is to prepare a summary of met$ods2 to evaluate and to interpret t$e experimental results as (ell as to compare t$em (it$ t$e t$eoretical results.

4$e report must not be less t$an 1, pa%es 7font: 4imes ?e( Roman2 12 pt2 spacin%: 1. lines8. 4$e number of pa%es is not includin% t$e abstract2 table of content2 list of dia%rams2 references and appendices. 4$e format of t$e report is as follo(s:

1.

Cover pa'e. 4$e pa%e includes title of t$e experiment2 dates of t$e experiment and report submission2 name of t$e laboratory5s supervisor and tec$nician on duty2 section and %roup number2 and name of t$e %roup5s leader and t$e members. A*!tra"t. 4$e purpose of (ritin% an abstract is to summari0e t$e overall report in 1,,#2,, (ords. It contains description of t$e experiment and t$e results obtained. /n abstract must be clear2 simple and statin% t$e +uantitative value7s8 obtained from t$e experiment. /n abstract is t$e last part prepared ($en (ritin% a report. Ta*le o% "o te t. It indicates t$e pa%e of eac$ main section of t$e report as (ell as list of dia%rams and tables. I tro+u"tio . Introduction serves to describe t$e ob3ective and scope of experiment as (ell as t$e previous (orks done. It must be (ritten in an or%ani0ed (ay to ease t$e readers to follo( t$e experiment to be done. T#eor, or Literature Stu+,. 4$e t$eoretical part describes briefly t$e desi%n of t$e experiment2 t$e function of t$e e+uipment and t$e e+uations involved in data analysis as (ell as t$e related assumptions. /ll t$e e+uations must be numbered in order
9

2.

3. 4.

e.%@..718 etc. 4$e variables2 e+uation derivation and calculation steps must be included in t$e appendix. ". -et#o+olo',. 4$is section describes t$e procedure of t$e experiment clearly but in a simple (ay. Aou only $ave to mention t$e important points e.%. 7weigh mass ! g of "a"#$ and the white filter paper before putting them into%s$ould be (ritten as: ! g of "a"#$ is used%8 Re!ult!. 4$is section consists of important data to be discussed and t$e data is usually presented in table2 %rap$ and dia%ram forms. Eac$ %rap$ic must be numbered and annotated clearly. >omparison of t$e results (it$ t$e t$eoretical and literature data can be included in t$is section. Di!"u!!io !. 4$is section interprets t$e results obtained ($ic$ covers also error and uncertainty analysis of t$e experiment. In t$e discussion2 you must explain t$e causes of t$e error and standard deviation of t$e results.

&.

'.

&'ote( Results and discussions can be combined)

). 1,.

Co "lu!io !. 4$is part includes summary of t$e results and discussions. It also briefly discusses t$e application and adaptation of t$e experiment conducted. Re"o$$e +atio !. 4$is part presents t$e ideas or recommendations2 ($ic$ are based on t$eory and lo%ic t$at can be applied to reduce t$e errors and to improve t$e results of t$e experiment. Re%ere "e!. References from 3ournals2 books2 standards and laboratory manual must be cited in t$e main text and listed accordin%ly in t$is section. 4$e format of t$e reference is based on t$e -4; t$esis (ritin% format. Aou $ave to include at least 3 main references t$at are related to t$e experiment conducted. Appe +i"e!. 4$is is a part ($ere detailed data analysis2 error analysis2 material p$ysical properties2 example of calculation and additional dia%rams are included to clarify t$e main text of your report. 4$e ori%inal experimental data t$at $as been stamped and si%ned by t$e supervisor must also be attac$ed in t$is section.

11.

12.

10

Su$$ar, o% t#e report %or$at

Cover Pa'e A*!tra"t Ta*le o% Co te t .i "lu+i ' li!t o% 'rap#!/ ta*le! a + !,$*ol!) 1.0 I tro+u"tio 1.1 1.2 1.3 2.0 (.0 Experimental back%round .b3ective Experimental scope

T#eor,1Literature Stu+, -et#o+olo', 3.1 3.2 E+uipment and materials Experimental procedure9met$odolo%y

2.0

Re!ult! a + Di!"u!!io ! 4.1 4.2 4.3 Experimental data :ata analysis and discussion /ns(ers to t$e +uestions in t$e experiment module

3.0 4.0

Co "lu!io ! Re"o$$e +atio !

Re%ere "e! Appe +i"e!

11

12

E5PERI-ENT 16 PAC7ED DISTILLATION COLU-N

#b*ecti e(

1. 2.

4o study t$e effect of operational time on t$e composition and volume of t$e product distillate. 4o study t$e correlation bet(een t$e volume of t$e product distillate and t$e composition of t$e product distillate.

+heory(

:istillation process is a process of separatin% li%$t components from ot$er components based on volatility differences. 4$e components (it$ lo(er boilin% points (ill vapori0e first and t$erefore (ill be collected as distillate (it$ $i%$ purity. Packin% materials are used to increase t$e surface area for en$ancin% contact bet(een t$e vapori0ed components (it$ t$e reflux so t$at purity of t$e product distillate can be furt$er improved.

Equipment,-aterials(

1. 2. 3. 4. . ". &. '. ).

Packed distillation column Refractometer 1yrin%e !eaker ;easurement cylinder Rea%ent bottle 1top (atc$ 6ater ;et$anol

13

.rocedure( 1. Prepare & met$anol#(ater mixtures usin% pipette. .btain t$e refractive index of t$e mixtures usin% t$e refractometer.
Bolume of met$anol 7ml8 Bolume of (ater 7ml8 Refractive index , 2, 2 1' 1 1, 1, 1 1' 2 2, ,

2. 3. 4.

Prepare 32 liters of met$anol#(ater feed mixture (it$ composition of met$anol 3,< and (ater &,<. ;ake sure all e+uipment is in place and in %ood conditions before startin% t$e experiment. /d3ust t$e valves position as follo(s: .pen valve: B2 >lose valve: R>B12 B32 B4

. ".

4urn on t$e electric $eater simultaneously (it$ t$e coolant flo( pump. 1et t$e reflux ratio at 2., or 3., by slo(ly opennin% reflux control valve R>B1 and t$e product distillate (ill flo( to RI 1!. 4$e rest of t$e product distillate (ill flo( t$rou%$ RI 1/ and return to t$e reboiler vessel. 4o collect product distillate ($ic$ does not return to t$e reboiler vessel2 ad3ust t$e position of t$e valves as follo(s: >lose valve B2 .pen valve B3 7>lose valve B3 if B4 is opened8 .pen valve B4 7to collect sample8

&.

'. ). 1,.

;easure t$e volume and refractive index of t$e collected product distillate. Repeat steps & and ' for every minutes and fill in t$e table %iven.

Reminder: ;ake sure samples of t$e standard material and t$e product distillate are kept in t$e container %iven.

/uestions(

14

1. 2. 3. 4. . ". &.

Plot %rap$ refractive index vs. <#mole met$anol for benc$mark mixture of met$anol# (ater. :iscuss t$e resulted %rap$. >alculate t$e met$anol mole fraction from t$e refractive index. Plot %rap$ mole fraction and volume of product distillate vs. time. :iscuss t$e advanta%es of packed distillation column. :iscuss t$e data and results obtained. *ist all t$e safety re%ulations and precautions t$at need to be considered ($en conductin% t$e experiment.

References(

1. 2. 3.

Ceankoplis2 >. D.2 0+ransport .rocesses 1 2nit #perations32 3rd Edition2 Prentice# Eall2 1)) . ;c >abe2 6. *.2 1mit$2 D. >. F Earriot2 P.2 02nit #peration of "hemical Engineering32 4t$ Edition2 ;c Cra(#Eill2 1)' . >oulson F Ric$ardson2 0"hemical Engineering32 Bolume 22 Per%amon2 1)'3.

E!perimental data(

4I;E 4E;PER/4-RE I? P*/4E 4I 1 4I 1! 4I 2 4I 2/ 4I 2! 4I 2> 4I 2: 4I 2=

1,

2,

3,

4,

",

15

4I 3 4emp. ori%inal solution 4emp. coolin% (ater Reflux 4I 4

4I 4I " RI 1/ RI 1!

Reflux ratio Bolume distillate Refractive index Bolta%e >urrent

16

E!perimental Setup

Packed :istillation >olumn

17

E5PERI-ENT 26 BUBBLE CAP DISTILLATION COLU-N

#b*ecti e(

1. 2.

4o study t$e effect of operational time on t$e composition and volume of t$e product distillate. 4o study t$e correlation bet(een t$e volume of t$e product distillate and t$e composition of t$e product distillate.

+heory(

:istillation process is a process of separatin% li%$t components from ot$er components based on volatility differences. 4$e components (it$ lo(er boilin% points (ill vapori0e first and t$erefore (ill be collected as distillate (it$ $i%$ purity. Packin% materials are used to increase t$e surface area for en$ancin% contact bet(een t$e vapori0ed components (it$ t$e reflux so t$at purity of t$e product distillate can be furt$er improved.

Equipment,-aterials(

1. 2. 3. 4. . ". &. '. ).

!ubble cap distillation column Refractometer 1yrin%e !eaker ;easurement cylinder Rea%ent bottle 1top (atc$ 6ater Et$anol

18

.rocedure( 1. Prepare & et$anol#(ater mixture usin% pipette. .btain t$e refractive index of t$e mixtures usin% refractometer.
Bolume of met$anol 7ml8 Bolume of (ater 7ml8 Refractive index , 2, 2 1' 1 1, 1, 1 1' 2 2, ,

2. 3. 4.

Prepare 32 liters of met$anol#(ater feed mixture (it$ composition of met$anol 3,< and (ater &,<. ;ake sure all e+uipment is in place and in %ood conditions before startin% t$e experiment. /d3ust t$e valves position as follo(s: .pen valve: B2 >lose valve: R>B12 B32 B4

. ".

4urn on t$e electric $eater simultaneously (it$ t$e coolant flo( pump. 1et t$e reflux ratio at 2., or 3., by slo(ly opennin% reflux control valve R>B1 and t$e product distillate (ill flo( to RI 1!. 4$e rest of t$e product distillate (ill flo( t$rou%$ RI 1/ and return to t$e reboiler vessel. 4o collect product distillate ($ic$ does not return to t$e reboiler vessel2 ad3ust t$e position of t$e valves as follo(s: >lose valve B2 .pen valve B3 7>lose valve B3 if B4 is opened8 .pen valve B4 7to collect sample8

&.

'. ). 1,.

;easure t$e volume and refractive index of t$e collected product distillate. Repeat steps & and ' for every minutes and fill in t$e table %iven.

Reminder: ;ake sure samples of t$e standard material and t$e product distillate are kept in t$e container %iven.

/uestions(

19

1. 2. 3. 4. . ". &.

Plot %rap$ refractive index vs. <#mole et$anol for benc$mark mixture of et$anol# (ater. :iscuss t$e resulted %rap$. >alculate t$e et$anol mole fraction from t$e refractive index. Plot %rap$ mole fraction and volume of product distillate vs. time. :iscuss t$e advanta%es of bubble cap distillation column. :iscuss t$e data and results obtained. *ist all t$e safety re%ulations and precautions t$at need to be considered ($en conductin% t$e experiment.

References(

1. 2. 3.

Ceankoplis2 >. D.2 0+ransport .rocesses 1 2nit #perations32 3rd Edition2 Prentice# Eall2 1)) . ;c >abe2 6. *.2 1mit$2 D. >. F Earriot2 P.2 02nit #peration of "hemical Engineering32 4t$ Edition2 ;c Cra(#Eill2 1)' . >oulson F Ric$ardson2 0"hemical Engineering32 Bolume 22 Per%amon2 1)'3.

E!perimental data(

4I;E 4E;PER/4-RE I? P*/4E 4I 1 4I 1! 4I 2 4I 2/ 4I 2! 4I 2> 4I 2: 4I 2=

1,

2,

3,

4,

",

20

4I 3 4emp. ori%inal solution 4emp. coolin% (ater Reflux 4I 4

4I 4I " RI 1/ RI 1!

Reflux ratio Bolume distillate Refractive index Bolta%e >urrent

21

E!perimental setup6

!ubble >ap :istillation >olumn

22

E5PERI-ENT (6 PAC7ED ABSORPTION COLU-N 8 RASC9I: RIN:

#b*ecti e(

1. 2.

4o study t$e effect of manipulated air flo( rate and (ater flo( rate on floodin% in t$e absorber. 4o study t$e correlation and t$e effect of (ater and air flo( rates on pressure difference2 GP.

+heory(

/bsorption process is one of t$e separation tec$ni+ues ($ic$ involves %as and li+uid. .ne or more components in %as mixture can be separated ($en a certain li+uid is flo(in% t$rou%$ it in cross#flo( or counter#currently. 4$e li+uid (ill absorb t$e component and mass transfer (ill take place to separate t$e component from t$e %as mixture. Packin% materials are used to increase t$e contact surface area for t$e absorption process so t$at t$e process (ill become faster and more efficient.

Equipment,-aterials(

1. 2. 3. 4. .

Packed absorption column # Rasc$i% rin% 7,.& mm8 /ir compressor 1top (atc$ 6ater /ir

.rocedure(

1.

>$eck and make sure all valves and components are in place and in %ood conditions before startin% t$e experiment.
23

2. 3. 4. . ". &. '.

1et (ater flo( rate at 2., *9min. /d3ust air flo( rate at 3, *9min. /t t$e same time2 start t$e stop (atc$ and continue for minutes. ;ake sure t$e (ater and air flo( rates are at t$e settin% value. /fter minutes2 record t$e pressure difference2 GP. minutes until

Repeat steps 3 and 4 for 1,*9min increment of air flo( rate for every floodin% occurs.

6$en floodin% occurs2 record t$e GP and reduce t$e air flo( rate back to 3,*9min. Repeat steps 3#& for (ater flo( rates of 2. 2 3., and 3. *9min. ?ext2 set air flo( rate at ,*9min and for every 2 minutes2 record t$e pressure difference at (ater flo( rate 2., to 3. *9min (it$ eac$ increment of ,. *9min.

E!perimental data(
6ater flo( rate2 6 7*9min8 /ir flo( rate2 C 7*9min8 Pressure drop2 GP 7cm E2.8 4ime 7every minutes8

2.,

2.

24

3.,

3.

/ir flo( rate2 C 7*9min8

6ater flo( rate2 6 7*9min8

Pressure drop2 GP 7cm E2.8

4ime 7every 2 minutes8

2., 2. 3., 3.

/uestions(

1. 2. 3. 4. .

Plot a %rap$ of lo% GP vs. lo% air flo( rate for eac$ (ater flo( rate t$at $as been set. :etermine t$e correlation bet(een GP and t$e flo( rate. Plot a %rap$ of lo% GP vs. (ater flo( rate for t$e air flo( rate t$at $as been set 7in procedure '8. :etermine t$e correlation bet(een GP and t$e flo( rate. :escribe t$e definition of floodin%2 floodin% velocity2 visual floodin% and load point. :iscuss t$e data and t$e results obtained. >ompare t$e operation and t$e efficiency of t$e absorption column usin% packin% materials of Intalox saddle and Rasc$i% rin%.

References(

1. 2.

Ceankoplis2 >. D.2 0+ransport .rocesses 1 2nit #perations32 3rd Edition2 Prentice# Eall2 1)) . ;c >abe2 6. *.2 1mit$2 D. >. F Earriot2 P.2 02nit #peration of "hemical Engineering32 4t$ Edition2 ;c Cra(#Eill2 1)' .
25

3.

4reybal2 R.E.2 0-ass +ransfer #perations32 3rd Edition2 ;c Cra(#Eill2 1)',.

26

E!perimental Setup(

Packed /bsorption >olumn 7Ras$i% Rin% and Intalox 1addle

27

E5PERI-ENT 26 PAC7ED ABSORPTION COLU-N 8 INTALO5 SADDLE

#b*ecti e(

1. 2.

4o study t$e effect of manipulated air flo( rate and (ater flo( rate on floodin% in absorber. 4o study t$e correlation and t$e effect of (ater and air flo( rates on pressure difference2 GP.

+heory(

/bsorption process is one of t$e separation tec$ni+ues ($ic$ involves %as and li+uid. .ne or more components in %as mixture can be separated ($en a certain li+uid is flo(in% t$rou%$ it in cross#flo( or counter#currently. 4$e li+uid (ill absorb t$e component and mass transfer (ill take place to separate t$e component from t$e %as mixture. Packin% materials are used to increase t$e contact surface area for t$e absorption process so t$at t$e process (ill become faster and more efficient.

Equipment,-aterials(

1. 2. 3. 4. .

Packed absorption column # Intalox saddle 7,.& mm8 /ir compressor 1top (atc$ 6ater /ir

.rocedure(

1.

>$eck and make sure all valves and components are in place and in %ood conditions before startin% t$e experiment.
28

2. 3. 4. . ". &. '.

1et (ater flo( rate at 2., *9min. /d3ust air flo( rate at 3, *9min. /t t$e same time2 start t$e stop (atc$ and continue for minutes. ;ake sure t$e (ater and air flo( rates are at t$e settin% value. /fter minutes2 record t$e pressure difference2 GP. minutes until

Repeat steps 3 and 4 for 1,*9min increment of air flo( rate for every floodin% occurs.

6$en floodin% occurs2 record t$e GP and reduce t$e air flo( rate back to 3,*9min. Repeat steps 3#& for (ater flo( rates of 2. 2 3., and 3. *9min. ?ext2 set air flo( rate at ,*9min and for every 2 minutes2 record t$e pressure difference at (ater flo( rate 2., to 3. *9min (it$ eac$ increment of ,. *9min.

E!perimental data(

6ater flo( rate2 6 7*9min8

/ir flo( rate2 C 7*9min8

Pressure drop2 GP 7cm E2.8

4ime 7every

minutes8

2.,

2.

29

3.,

3.

/ir flo( rate2 C 7*9min8

6ater flo( rate2 6 7*9min8

Pressure drop2 GP 7cm E2.8

4ime 7every 2 minutes8

2., 2. 3., 3.

/uestions(

1. 2. 3. 4. .

Plot a %rap$ of lo% GP vs. lo% air flo( rate for eac$ (ater flo( rate t$at $as been set. :etermine t$e correlation bet(een GP and t$e flo( rate. Plot a %rap$ of lo% GP vs. (ater flo( rate for t$e air flo( rate t$at $as been set 7in procedure '8. :etermine t$e correlation bet(een GP and t$e flo( rate. :escribe t$e definition of floodin%2 floodin% velocity2 visual floodin% and load point. :iscuss t$e data and t$e results obtained. >ompare t$e operation and t$e efficiency of t$e absorption column usin% packin% materials of Intalox saddle and Rasc$i% rin%.

References(

1.

Ceankoplis2 >. D.2 0+ransport .rocesses 1 2nit #perations32 3rd Edition2 Prentice# Eall2 1)) .

30

2. 3.

;c >abe2 6. *.2 1mit$2 D. >. F Earriot2 P.2 02nit #peration of "hemical Engineering32 4t$ Edition2 ;c Cra(#Eill2 1)' . 4reybal2 R.E.2 0-ass +ransfer #perations32 3rd Edition2 ;c Cra(#Eill2 1)',.

31

E5PERI-ENT 36 PARALLEL8FLO; PLATE 9EAT E5C9AN:ER

#b*ecti e(

4o determine t$e $eat transfer coefficient 7-8 for a parallel#flo( plate $eat exc$an%er.

+heory(

4$e operational principle of plate $eat exc$an%er is based on $eat transfer from $ot stream to cold stream2 ($ic$ conse+uently causes temperature c$an%es in bot$ streams.

4$e $eat transferred from t$e $ot to cold streams is e+ual to t$e $eat received by t$e cold stream.

/ 4 m"p &+567+58) 4 m"p &+"87+"6)

H m >p 4E1 4E2 4>1 4>2

I Eeat transfer I =luid mass I =luid $eat capacity I Eot stream inlet temperature I Eot stream outlet temperature I >old stream inlet temperature I >old stream outlet temperature

/ 4 2A9+lm / G4lm I Eeat transfer coefficient I Plate surface area I *o% mean temperature difference2 ($ic$ is described by:
32

+lm =

7+5 2 +" 2 8 7+5 1 +"1 8 + +" 2 ln 5 2 +5 1 +"1

4$e standard $eat transfer coefficient for t$is experiment is bet(een ,, # &,, 69m2.J>.

Equipment,-aterials(

1. 2. 3. 4. .

Parallel#flo( plate $eat exc$an%er 1,* capacity plastic container 1top (atc$ 6ater pump 6ater

33

.rocedure(

1. 2. 3. 4. . ". &. '. ).

1(itc$ on t$e $eater and stirrer to $eat up t$e fluid in t$e stora%e tank. 4urn $ot stream pump on to recycle $ot (ater in t$e tank. *et t$e (ater flo( until t$e (ater temperature in t$e tank reac$es ", J>. ;ake sure $ot stream temperature 74E28 is e+ual to t$e temperature in t$e tank 74E18. 6$en t$e temperatures are even2 make preparation to record t$e inlet and outlet temperatures for eac$ $ot stream and cold stream simultaneously. .pen t$e cold stream valve slo(ly. /t t$e same time2 start t$e stop (atc$ and record all t$e related temperatures as in procedure 748. 1top t$e stop (atc$ ($en t$e time is up. >lose t$e cold stream valve. Repeat steps 3#' for t$ree 738 subse+uent sets of data readin%. >alculate t$e avera%e readin% for all t$e data recorded.

E!periment data(

Experimental information for parallel#flo( plate $eat exc$an%er *en%t$ of t$e plate 6idt$ of t$e plate 4$ickness of t$e plate 4otal number of plate 42, 12 4" 1 mm mm mm pieces

Exp.

/vera%e

34

4emp. 7J>8 4E1 4E2 4>1 4>2 Bolume (ater 4ime 7s8

Initial readin%

=inal readin%

Initial readin%

=inal readin%

Initial readin%

=inal readin%

Initial readin%

=inal readin%

35

/uestions(

1. 2. 3. 4. .

!ased on t$e recorded data2 plot a %rap$ of temperature vs. time for $ot stream and cold stream. :ra( a temperature profile vs. plate t$ickness for parallel#flo( plate $eat exc$an%er. :etermine t$e overall $eat transfer coefficient for t$is $eat exc$an%er. :iscuss ($y t$e calculated value differs from t$e standard value. :escribe t$e advanta%es of plate $eat exc$an%er. :iscuss all t$e results obtained.

References(

1. 2. 3.

Eolman2 D. P.2 05eat +ransfer32 't$ edition2 ;c Cra(#Eill Inc.2 -.1./2 1))&. ;c >abe2 6. *.2 1mit$2 D. >. F Earriot2 P.2 02nit #peration of "hemical Engineering32 4t$ Edition2 ;c Cra(#Eill2 1)' . Ceankoplis2 >. D.2 0+ransport .rocesses 1 2nit #perations32 3rd Edition2 Prentice# Eall2 1)) .

36

E5PERI-ENT 46 LI<UID8LI<UID E5TRACTION

.b3ective: 4o observe t$e effect of c$an%e in flo(rate to(ards t$e performance of t$e extraction process

4$eory: *i+uid#li+uid extraction is a separation tec$ni+ue t$at involves components $avin% different p$ysical and c$emical properties. 4$e process is carried out by $avin% t$e $eavy p$ase li+uid 7solvent8 flo(in% counter#currently (it$ t$e li%$t#p$ase li+uid 7feed9diluent8. /t t$e end of t$e process2 t$e $eavy p$ase containin% solutes bein% transferred from t$e li%$t p$ase is kno(n as Extract and t$e more pure li%$t p$ase is called Raffinate.

Experimental Procedure 1. !efore be%innin% t$e experiment2 determine t$e iodine concentration in t$e li%$t p$ase li+uid usin% titration tec$ni+ue. 2. 4urn on t$e feedin% pump follo(ed by t$e pulsatin% pump 3. 1et t$ese parameters: Pulsatin% pump at ,< 71,8 =eedin% pump for $eavy p$ase ,< 71,8 and li%$t p$ase & < 71 8 4. *et t$e system operate for 1 minutes. . .bserve t$e interface level. ;ake sure t$e level is less t$an 2,cm from t$e feedin% point of t$e li%$t p$ase. If necessary2 use t$e balancin% le% to ad3ust t$e level. ". 6$en t$e interface level is stable2 start t$e timin% and collect sample every from t$e raffinate t$rou%$ valve B1&. &. /nalyse t$e solute content 7iodine8 in t$e sample usin% titration tec$ni+ue. '. Repeat t$e sample collection process until t$e iodine content in t$e sample is stable. ). 6$en t$e iodine content is constant2 collect sample from valve B) by closin% valve B&. /nalyse t$e iodine content in t$e sample also usin% titration tec$ni+ue. 1,. Repeat steps 3 to )2 but (it$ t$e follo(in% flo( rate:
37

minutes

Eeavy P$ase 71 8 *i%$t P$ase 71 8

Eeavy P$ase 72,8 *i%$t P$ase 71 8

11. 4itration tec$ni+ue: a. Pipette 3,cm3 of sample into t$e conical flask. b. /dd a fe( drops of starc$ indicator. c. 4itrate t$e sample usin% sodium t$iosulp$ate solution 7,.,1;8 %radually. d. 1top t$e titration once t$e blue#black colour turns becomes clear.

Experimental :ata: Raffinate >omposition 7%9*8 Eeavy P$ase flo( rate: 1, *9min *i%$t P$ase flo( rate: 1 *9min 4ime 7min8

Extract >omposition 7%9*8

4ime 7min8

Raffinate >omposition 7%9*8 Eeavy P$ase flo( rate: 1 *9min *i%$t P$ase flo( rate: 1 *9min

4ime 7min8

Extract >omposition 7%9*8

4ime 7min8

Raffinate >omposition 7%9*8 Eeavy P$ase flo( rate: 2, *9min *i%$t P$ase flo( rate: 1 *9min

4ime 7min8

Extract >omposition 7%9*8

4ime 7min8
38

/uestions(

1. 1tate ($ic$ component is t$e $eavy p$ase2 li%$t p$ase2 solvent2 solute and diluents. 2. 1tate t$e dispersed p$ase and t$e continuous p$ase in t$is experiment. 3. 6$at is t$e meanin% of e+uilibrium contactK 4. :iscuss t$e effect of flo(rate to(ards t$e extraction performance. . 1tate ot$ers steps and measures to be taken to increase t$e performance of t$is extraction process. ". :escribe t$e importance of li+uid#li+uid extraction processes in c$emical en%ineerin%.

References(

1. 2. 3.

Ceankoplis2 >. D.2 0+ransport .rocesses 1 2nit #perations32 3rd Edition2 Prentice# Eall2 1)) . ;c >abe2 6. *.2 1mit$2 D. >. F Earriot2 P.2 02nit #peration of "hemical Engineering32 4t$ Edition2 ;c Cra(#Eill2 1)' . 4reybal2 R.E.2 0-ass +ransfer #perations32 3rd Edition2 ;c Cra(#Eill2 1)',.

39

E!perimental Setup(

*i+uid#*i+uid extraction

40

E5PERI-ENT =6 PAC7ED REACTOR COLU-N FOR ACETONE8;ATER SEPARATION SYSTE-

#b*ecti e(

1. 2.

4o study and determine t$e efficiency of packed column in acetone#(ater separation system. 4o determine boilin% point of eac$ component.

+heory(

Reactor column in -nit .peration 1 laboratory is used to separate acetone from acetone# (ater mixture based on a simple principle of distillation. 4$is is a batc$ system in ($ic$ t$ere (ill be no continuous feed to t$e system t$rou%$out t$e operation.

Equipment,-aterials(

1. 2. 3. 4. . ". &. '.

Pilot plant packed reactor column !eaker Class rod 1yrin%e Refractometer 1top (atc$ /cetone 6ater

.rocedure(

41

1.

Prepare & acetone#(ater mixture usin% pipette. .btain t$e refractive index of t$e mixtures usin% refractometer.
Bolume of acetone 7ml8 Bolume of (ater 7ml8 Refractive index , 2, 2 1' 1 1, 1, 1 1' 2 2, ,

2. 3. 4. . ". &. '. ). 1,. 11.

Pour 1"* mixture of ',< (ater and 2,< acetone carefully into t$e reboiler t$rou%$ feed funnel. ;ake sure all valves and components are in place and in %ood conditions before startin% t$e experiment. 4urn on t$e (ater tap and s(itc$ on centrifu%al pump to start t$e coolin% system. 1(itc$ on reboiler and stirrer and set t$e temperature at certain $eatin% rate. .bserve t$e reactor until e+uilibrium is reac$ed 7t$at is ($en t$e +uantity of vapor leavin% t$e reactor e+uals to t$e +uantity of li+uid returned to t$e reboiler8. .pen valve B1 to allo( li+uid acetone to flo( t$rou%$ condenser in order to be cooled do(n. /t t$e same time2 open valves B2 and B3 and close valve B4. *et acetone flo( t$rou%$ valves B2 and B32 and subse+uently to t$e back of collector 1 and flask 2. 1imultaneously2 start t$e stop (atc$. /fter minutes2 close valve B3 and open valve B4 to collect product distillate. /t t$e same time2 record t$e temperatures of t$e mixture and t$e distillate. ;easure t$e volume and t$e refractive index of t$e product. Repeat steps ' # ) for every minutes for a total of ", minutes.

Reminder: ;ake sure samples of t$e standard material and t$e product distillate are kept in t$e container %iven.

E!perimental data(

4ime 7s8 4emperature mixture 7J>8 4emperature distillate 7J>8

1,

2,

3,

4,

",

42

Bolume distillate 7m*8 Refractive index 7n:8

/uestions(

1. 2. 3. 4. . ". &.

Plot %rap$ refractive index vs. <#mole acetone for benc$mark mixture of acetone# (ater. :iscuss t$e resulted %rap$. >alculate t$e acetone mole fraction from t$e refractive index. Plot %rap$ mole fraction2 volume of product distillate and temperature of distillate vs. time. Plot %rap$ composition of t$e product distillate vs. volume. :iscuss t$e results obtained. !ased on t$e %rap$2 explain t$e efficiency of t$e packed reactor column for acetone#(ater separation system. *ist all t$e safety re%ulations and precautions t$at need to be considered ($en conductin% t$e experiment.

References(

1. 2. 3.

Ceankoplis2 >. D.2 0+ransport .rocesses 1 2nit #perations32 3rd Edition2 Prentice# Eall2 1)) . ;c >abe2 6. *.2 1mit$2 D. >. F Earriot2 P.2 02nit #peration of "hemical Engineering32 4t$ Edition2 ;c Cra(#Eill2 1)' . >oulson F Ric$ardson2 0"hemical Engineering32 Bolume 22 Per%amon2 1)'3.

43

E!perimental Setup(

Packed Reactor >olumn

44