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Separation Technology: Draw Insights on Distillation

Residuecurvemappingisapowerfultooltobetterunderstandthedesignandoperationofdistillation
columns.Thisarticledescribeshowtouseresiduecurvemapstocheckthefeasibilityofseparationof
homogeneousmixturesandfordevelopingtheconceptualdesignoftowers.
ByRaymondE.Rooks,TheDowChemicalCo.
May15,2006

Residuecurvemappingisapowerfultooltobetterunderstandthedesignandoperationofdistillationcolumns,
especiallywhenthemixtureisazeotropic[1].ApreviousarticleinChemicalProcessing[2]introducedthe
approachandfocusedonthefeasibilityofapplicationsinvolvingmixturesthatformtwoliquidphases.Thatarticle
showedhowtoexploittwoliquidphasebehaviortofacilitateadesiredseparation.Thisarticlewilldescribeusing
residuecurvemapstocheckthefeasibilityofseparationofhomogeneousmixturesandfordevelopingthe
conceptualdesignoftowers.

Astandardresiduecurvemapisacompositionplotofthekettleresidueliquidasthemixtureiscontinuallyboiled
withnoreflux.Asyoucanimagine,themixturewillgetheavierovertime,asthelightercomponentsareboiledoff.
Thisisimportantbecauseresiduecurvemapsareanapproximationtotheliquidcompositionprofileina
distillationcolumnoperatedattotalreflux.

Key advantages
Residuecurvescanbeusedtodeterminewhatseparationsarepossiblewithadistillationcolumnindependentof
howmanystagesarerequiredandhowmuchenergyisconsumed.Moreover,comparedtostagetostage
columncompositionprofilecalculations,residuecurvesaremathematicallymucheasiertoworkwithandcan
provideagreatamountofinsightintotheseparationofamixture.

Forinstance,considerthemixtureofmethanol,ethanolandnpropanol.Thismixturedoesnotformazeotropes
andisreasonablyideal.Theresiduecurvesforthemixture(Figure1)havetwoendpoints:oneatthemethanol
vertexandtheotheratthenpropanolvertex.Ifyoupickedanypointalongaresiduecurveasaninitial
compositionfortheboilingkettle,then,asthelightermaterialisboiledoff,thekettlecompositionwouldstayon
thesamecurveandeventuallyconvergeonthenpropanolvertex.

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Figure 1. Separation of a mixture of methanol, ethanol and 1-propanol follows the appropriate residue
curve. (Click to enlarge)
Astagetostagecompositionmapforacolumnoperatedattotalreflux(Figure2)has16equilibriumstagesto
producetheindicatedbottomsanddistillatecompositionsfromthefeed.Aresiduecurvepassingthroughoneof
theequilibriumstagesisalsoshownitcloselyresemblesthecolumnliquidcompositionprofile.Generally,asthe
mixturebecomesmoredifficulttoseparate,thesecurveswillbemoresimilar.

Figure 2. Producing the overhead and bottoms products indicated requires sixteen equilibrium stages.
(Click to enlarge)
Alsonoticethatthefeed,distillateandbottomscompositionsareallonaline.Thisisrequiredviamassbalance
forasinglefeed,twoproductcolumn.Fromamassbalance,weknowthat:

F B
http://www.chemicalprocessing.com/articles/2006/071/ 2/6
5/28/2017 ProcessEngineering|Drawinsightsondistillation|ChemicalProcessing

whereDisthedistillateflow,Bisthebottomsflow,ziFisthefeed(massormole)fraction,ziBisthebottoms
fractionandziDisthedistillatefractionofagivencomponentinthemixture.Thisequationprovidesthecolinear
relationshippreviouslydescribedandalsoisanexcellentwaytocheckmassbalancesfromplantsamples.
Pluggingintotheequationtheresultsofafeed,distillateandbottomscompositionanalysisforeverycomponent
inthemixtureshouldresultinthesameD/Bratio.Thisequationalsocanbeusedtoverifytheresultsofflow
meters.

Acolumnmassbalanceandresiduecurvemapscansignificantlyhelpdeterminewhatseparationsarepossible.
Forexample,consideramixtureofacetone,isopropanolandwater.Thismixtureformsasinglehomogeneous
azeotropebetweenisopropanolandwater.

Theresiduecurvemapforthismixtureshowsallofthecurvesstartingatacetonebutsomeendingat
isopropanolandsomeatwater(Figure3).So,dependingontheinitialstartingconcentrationinthepot,thelast
dropofliquidinthekettlewillbewaterorisopropanol.Thisistheeffectoftheazeotropebetweenwaterand
isopropanol.Themixtureissplitintotwozonesordistillationregionsbyacurvebetweenacetoneandthe
isopropanol/waterazeotrope.Thiscurveistermedadistillationboundaryasitseparatesthetwodistillation
regions.Thedistillationboundaryindicatesthatifthefeedcompositiontothecolumnisinonedistillationregion,
thenacolumnoperatingattotalrefluxwouldbeunabletoseparatethemixtureintothethreedistinctcompounds.
Italsoshowsthatwater,althoughapotentialpureproductfromamixturelyinginthelowerregion,cannotbe
completelyrecoveredfromisopropanolandacetone.

Figure 3. Acetone/isopropanol/water mixture can form an isopropanol/water azeotrope. (Click to enlarge)

Column at less-than-total reux

EngineersusethewellknownMcCabeThielediagramtoevaluatedistillationdesignsformixtureswithtwokey
componentswhenthefeedcomposition,feedquality(liquid,vapor,degreeofsuperheat,etc.)anddesired
productcompositionsareknown.Steppingoffstagesbetweentheoperatinglineandtheequilibriumcurvegives
thenumberofequilibriumstagesnecessary.Contrastthistohowsimulationsareperformedinastandard
processsimulator:thenumberofstagesisguessedandthecolumncompositionsareiterativelysolvedandthe
stagecountupdateduntilthedesiredsolutionisfound.McCabeThielediagramsareparticularlyusefulbecause
theyprovideinstantvisualfeedbackyoucanquicklydetermineiftherefluxratioistoolow,ifapinchpoint
arisesorifthereisaninfeasiblesetofspecificationsduetothepresenceofanazeotrope.

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