Chemical Engineering Laboratory Manual

Multistage Distillation

EXPERIMENTNO.51
MULTISTAGEDISTILLATION
OBJECTIVES:
1. Compareobservedcolumntemperatureandcompositionprofileswiththose
predictedbyMcCabeThiele/RADFRAC.
2. Determinetheoverallcolumnefficiencyandcomparewithtypicalefficiencies
fortrayedbubblecapcolumns.
3. Checkmaterialandenergybalancesforthecolumnoperatingatsteadystate.
4. Determinetheoptimumfeedstageforthissystem.
NOTATION:
B

liquidmolarflowrateoftheproductleavingthereboiler(moles/time)

liquidmolarflowrateoftheproductleavingthecondenser(moles/time)

liquidmolarflowratedescendingwithintherectifyingsectionofthetower
(moles/time)

L/

liquidmolarflowratedescendingwithinthestrippingsectionofthetower
(moles/time)

thestrippingsectiontraynumber,wheretraynumberoneisatthetopofthe
tower

thetraynumber,wheretraynumberoneisatthetopofthetower

heatrequiredtoconvert1moleoffeedfromitsconditionasitentersthe
towertoasaturatedvapordividedbythemolallatentheatofthefeed

refluxratio,molepertimeofliquidfromthecondenserreturnedtothetop
trayofthetowerdividedbythemolespertimeofdistillate

molefractionofAintheliquidphase

xB

molefractionofAintheliquidleavingthereboiler

xD

molefractionofAintheliquid(thedistillate,D)leavingthecondensernot
returnedtothetower

xF

molefractionofAinthefeedstream

molefractionofAinthevaporphaseenrichingsection

THEORY:
Distillationisamethodofseparatingthecomponentsofasolution.Itdependsuponthe
distributionofthesubstancesbetweenagasandaliquidphase,appliedtocaseswhere
allcomponentsarepresentinbothphases(2).Itisacommon"unitoperation"found,
forexample,inthepetroleumandchemicalindustries.

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Distillationisbasedontheprinciplethatwhensufficientenergyistransmittedtoa
mixturecontainingcomponentsofdifferingvolatilities;themorevolatilecomponents
(i.e.havingahighervaporpressure)willvaporizepreferentiallywithrespecttotheless
volatilecomponents.
Indistillationonlyafractionoftheliquidisvaporized;withrespecttotheoriginal
liquidthevaporisricherinthemorevolatilecomponentsandtheresidualliquidis
richerinthelessvolatilecomponents.Thevaporiscondensedandthenpartially
vaporized,thisprocessisrepeateduntilthevaporhasthedesiredcomposition.The
remainingliquidfromeachpartialvaporizationiscountercurrentlyandintimately
contactedwiththevapor,whichisleanerinthemorevolatilecomponentfromthe
precedingpartialvaporizationstage.Thepointinadistillationtowerwheretheliquid
andvaporcontactiscalledastage.Thecontactingisdonetypicallybyintimatemixing
onsievetrays,inpackedsections,orbybubblecaps,asinthisexperiment.
Whenthestagesarearrangedinaverticalfashionsothatthevaporsevolvingfromone
stagecontactthedescendingliquidfromthestageabove,wehaveadistillation
"column"or"tower",seeFigure188(1),orFigure11.41(6).
Thesectionabovethepointwherethefeedentersthetowerisreferredtoasthe
enrichingorrectifyingsection.Intheenrichingsectionthefallingliquid"washes"the
lessvolatilecomponentsfromtherisingvapor.Thesectionbelowthefeedisreferred
toasthestrippingsection.Inthestrippingsectiontheliquidinthebottomofthetower
ispartiallyvaporized,thevaporthenrisesstrippingthedescendingliquidofthemore
volatilecomponents.
Forliquidtobeprovidedtothetopstage,someofthecondensedvaporsfromthisstage
arereturnedasreflux.Forvaporstobesuppliedtotheloweststage,someliquidfrom
theloweststageisvaporizedinthe"reboiler".
Twocommonmethodsusedtocalculatetherelationshipbetweenthenumberoftrays,
liquid/vaporratios,andproductcompositionforabinarymixture(AandB)arethe
PonchonandSavaritmethodandtheMcCabeandThielemethod.Theformerrequires
detailedenthalpydatawhilethelatterdoesnotandisthereforealsolessaccurate.Often
theMcCabeThielemethodisadequatebecausetheenthalpyeffectsarenotlarge.
McCabeThieleMethod
Theprimaryassumptionisthattheoperatinglinesinaxycoordinatesystemplotare
straightforeachtowersection.Thiswillbetrueifenthalpyeffectsarenegligible.

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Theoperatinglinefortheenrichingsectioncanbeobtainedfromamaterialbalance
aroundtheenrichingsectionincludingthecondenser,seeFigure188(1).Ifthe
condenserisatotalcondenserthentheoperatinglineequationis

y n 1

L
D
xn
xD
LD
LD

Amaterialbalancearoundthestrippingsectionincludingthereboileryieldsthe
operatinglineforthestrippingsection
y m 1

L/
B
xm /
xB
/
L B
L B

Theoperatinglineforthefeed,theqline,isestablishedfromamaterialandanenthalpy
(energy)balancearoundthefeedstage,yielding
y

q
x
x F
q 1
q 1

Ifthefeedcompositionandthermodynamicstate,xD,xB,andtherefluxratioare
specified,theoperatinglinescanbedrawnonaxycoordinatesystemplot.Fromthe
graphthenumberoftheoreticalstagesforthedesiredseparationcanbedetermined.
Notethatfiveoftheabovementionedvariablesneedtobeknowntodeterminethe
sixth,graphically.
EQUIPMENT:
Asimpleschematicarrangementofadistillationcolumnwithaccessoriesisshownin
Figure188(1).Thedistillationequipmentinthelaboratoryismoreelaborate.Itwas
madebytheBrightonCorporationofCincinnati,Ohio.Thereisasetofdrawings
providedtoaidinunderstandingitsconstructionandarrangement.Thepipingdiagrams
aredrawingsBD20194EL,BC80841ELandBC80842EL(6).Thedistillation
columnitselfcontains20bubblecapplates.Eachplatehas3bubblecaps.Thecolumn
ismadeupof18coppersections,each6incheshigh,eachflangedatbothendsand
boltedtogetherwithaplatebetweeneachpairofadjacentsections.Thetwotop
sections,19&20,areofglass,sobubblecapactionmaybeobserved.The
downcomershaveaninsidediameterofabout1inch(eyeballestimate).Thecolumn
sectionshaveadiameterof8inches;flangediameteris11inches;9l/2inchboltcircle
with12boltspercircle.
Thecolumnisuninsulated;therefore,itwillnotoperateadiabatically.

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Akettleisprovidedtofurnishheatedfeed.Afeedpumpisprovided.Acalandria
reboilerislocatedinthebottomofthecolumn.Threewatercooledoverhead
condensersoperateinseriesfortotalcondensationoftheoverheadvapors.Pipingis
suchthatfeedmaybeintroducedtoanyofthelower18platesortothetopofthe
column.Tanksareprovidedforoverheadandbottomproductcollection,butthese
streamsshouldbesampledusingthelinetaps.Instrumentationisprovidedfor
measuringtemperaturesandpressureswithinthesystemandformeasuringflowrates
onthevariousstreams.Samplingcontainersarearrangedalongthecolumntoobtain
liquidsamplesfromalternateplates.
PREPARATION:
Beforecomingtothelaboratorypreparethefollowingaids:
1. Avaporliquidequilibriumdiagram(TxyandXYdiagrams)fortheethanolwater
systemat13.25psia.ASPENPluscanbeusedtogeneratethesediagramsusingthe
properphysicalpropertyset.Youshouldverifytheaccuracyofthegenerated
diagramswithliteraturedata;Perrys6theditiongivesanenthalpyconcentration
diagramfortheethanolwatersystem.
2. Youwillbefeedinga~0.12molfractionethanolinwaterstreamtoa20stage
distillationcolumnataflowrateof0.2gpmandatemperatureof60C.Your
targetproductconcentrationis0.70molfractionethanolinthedistillateand97%
recoveryofethanolinthedistillate.UseMcCabeTheile/ASPENRADFRACto
estimatetherefluxratiorequiredandoptimalfeedstageforthisseparationwhenthe
Murphreestageefficiency(Emv)is0.50.Assumethatthereboilerdoesnotcountas
anadditionalequilibriumstage.Useanoverallcolumnmaterialbalanceto
determinethedistillateproductflowrateingallonsperminute.FromASPENusing
NRTL,themolardensityof12mol%ethanolat60Cis2.63lbmol/ft3,andthe
molardensityof70mol%ethanolatthebubblepointis1.26lbmol/ft3.
PROCEDURE:
1. Safety:Hardhatandsafetyglassesrequired.Thesteamlines,feedkettle,
reboiler,andcolumnalloperateatelevatedtemperatures.
2. Familiarizeyourselfwiththedistillationcolumnsystem.KnowtheFeedsystem,
ReboilerCondensate(Bottoms)system,Refluxsystem,UtilitiesPumpsystem,and
Steamsystem.
3. Ensurethatfeedcompositioninkettleisatleast0.12molfractionofethanol.
4. Turn on cooling water supply to the kettle condenser and the top product condensers.
Confirm that condenser vent line to atmosphere is open; this allows non-condensable
gas to exit the column during startup.
5. Open feed valve on desired feed tray, and verify that all other tray valves are closed.

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6. Open gate valve for steam coming from header (located on east wall). Make sure ball
valve for the steam condensate is open (going towards the absorber).
7. Verify level in feed kettle and reboiler. Collect a feed sample for GC analysis.
8. Turn on the power supply to the control panel.
9. Startup the computer. On the Desktop, open Distillation Control Strategy. Click
Debug, and then Start Strategy.
10. Put feed kettle temperature control loop in AUTO in PAC Display Runtime Basic
(setpoint at 140 F).
11. With valves open from kettle to pump and then to column, start the feed pump.
Adjust the feed flow rate with the rotameter to achieve 0.1 gpm.
12. Set reboiler temperature in AUTO at 215 F in PAC Display Runtime Basic.
13. Set the Bottoms level to be 80% in PAC Display Runtime Basic.
14. Temperatures for each stage of the column can be viewed in PAC Display Runtime
Basic by opening the Unit Display.
15. Once the overhead temperature reaches 70 C, increase the feed flow rate to 0.2
gpm.
16. Monitor reflux flow rate on display panel. Once the reflux flow rate exceeds 0.1
gpm, start the product flow rate at a value corresponding to your desired reflux ratio.
17. Visually observe the top two stages through the glass wall. Look for flow patterns
that could lower tray efficiency, such as weeping, entrainment, and liquid splashing
down the downcomer.
18. Carefully touch the atmospheric vent line to see if it is hot. If it is hot, increase the
condenser cooling water flow rate and notify the instructor.
19. If level gets too high in Bottoms, Reflux, or Distillate tanks, open valves to drain
tanks and start the Utility Pump to drain tanks into the Kettle.
20. Monitor column temperatures and flow rates (including reflux rotameter) to verify
steady state operation. Verify that all sample jars are empty.
21. Write down all temperatures and flow rates.
22. Sample the overheads distillate and the bottoms product using the needle sample
valves. Open the bottoms sample valve slowly and carefully this sample will
be hot. The person collecting samples should wear rubber gloves.
23. Manually actuate the sample valves with instrument air. Once all the sample jars are
at least half filled, bleed instrument air pressure to close the sample valves.
24. Transfer samples to sample bottles and allow cooling to room temperature.
25. Measure reboiler condensate flow on the display panel labeled Bottoms flow rate.
Whenyouhavecompletedthedistillationrun,observethefollowingproceduresin
shuttingdown.
1. Turn off steam supply manual valves at the column and at the main supply header.
2. Turn off the feed pump.
3. Close out of PAC Display Runtime Basic. In PAC Control Basic, click Stop
Strategy and close out.
4. Turn off power supply to display.
5. Turn off the cooling water after the temperature at the top of the column has

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dropped to 40 C.
6. Analyze samples for mole fraction ethanol using GC or refractive index.

REPORTING:
Inreportingthisexperimentyoushould:
1. Plottemperatureversusstagenumber.Compareyourmeasuredtemperatureswith
thosepredictedfromyourmeasuredcompositionsviayourTxydiagram.Also
compareyourmeasuredtemperatureprofilewithyourRADFRACgenerated
profile.
2. Plotliquidethanolmolefractionversusstagenumber.Compareyourmeasured
compositionprofilewithprofilesgeneratedbyMcCabeThiele/RADFRAC.
3. Calculatethemolalflowratesofvaporandliquidatthetop.Checkyouroverall
columnmaterialbalance.
4. DetermineyourexperimentalreboilerandcondenserdutiesinBtu/hr.Checkyour
overallcolumnenergybalance.
5. Showthedeterminationoftheoreticalstages(plates)neededtoachievethe
observedseparationbyMcCabeThieleandRADFRAC.
6. Computetheoverallcolumnefficiencyfromyourdata.Comparethiswithtypical
efficienciesreportedintheliteraturefortrayedbubblecapcolumns.
7. Estimatethechangeinmolalvaporflowfromtoptobottomduetocolumnheat
losses.Howwouldthisaffectyourcalculatedcolumnefficiency?
REFERENCES:
1. McCabe,SmithandHarriott,UnitOperationsofChemicalEngineering,Fifth
Edition,McGrawHillBookCo.(1993).
2. Treybal,MassTransferOperations,ThirdEdition,pp.185,342357,371419,
McGrawHillBookCo.(1968).
3. Perry,GreenandMaloney,ChemicalEngineers'Handbook,SixthEdition,pp.18
37to1819,McGrawHillBookCo.(1984).
4.

Perry,Ibid,FourthEdition,pp.132to1310,1817,McGrawHillBookCo.
(1963).

5.

Perry,Ibid,ThirdEdition,p.575(1950).

6.

C.J.Geankoplis,TransportProcessesandUnitOperations,ThirdEdition,
PrenticeHallPTR(1993).

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7.

OperatingInstructionsforCompleteModel"A",LaboratoryDistillationUnit,
SDSM&T,SerialNo.4269,BrightonCorporation(1961).

8.

InternationalCriticalTables,Vol.3,p.310.

FORADDITIONALINFORMATION:
9.

Chu,JuChin,etal.,DistillationEquilibriumData,ReinholdPublishingCorp.
(1950).

10.

Chu,JuChin,etal.,VaporLiquidEquilibriumData,J.W.Edwards,Publisher
(1956).

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