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PACKEDBEDFLUIDDYNAMICSANDAMMONIAABSORPTION
INSTRUCTIONSFORSTUDENTS
Safety
Overview
Scenario
Apparatus
Procedure
AmmoniaRotameterCalibration
Report
NotesonGasAbsorption
ResidenceTimeDistributionTheory
SampleCalculationofPressureDrop
References
Comments
A.SAFETY
1.AMMONIAISBOTHTOXICANDCOMBUSTIBLE.Ifamajorammonialeakdevelops,evacuatethe
laboratoryimmediately,withoutattemptingtoshutoffthecylindervalve.Openthemaincylindervalveonly
aboutonehalfturn,topreventdischargeathighrates.
2.Wearsafetyglassesatalltimes.Besurethelabventilationsystem(inRoom171)isoperatingbeforeusing
ammonia.Besuretheammoniacylindervalveisclosedbeforeendingtheexperiment.Knowthesafety
showerandeyewashstationlocations.
3.Wearjeansorslacks,alongsleevedshirt,andsturdyshoesthatgivegoodtractiononpossiblywetfloors.
4.Guardagainstelectricalhazardsbymakingsurethatallequipmentiswellgroundedusingthreewireplugs
andothermeans.
5.Handlewithgreatcareanysolventsorotherpotentiallyvolatile,flammable,toxic,orotherwisedangerous
chemicals.Inthisexperimentair,water,ammonia,andasolutionofpotassiumchlorideareused.Potassium
chlorideistoxicifingestedinlargeamounts.Ammoniaistoxicinhigherconcentrations.
6.Guardagainstfalls,burns,cuts,andotherphysicalhazards.Useheavyglovestoopenorclosehotsteam
orcondensatevalves.
7.THINKFIRSTOFSAFETYINANYACTIONYOUTAKE.Ifnotcertain,asktheTAorafaculty
memberbeforeyouact.
B.OVERVIEW
Thepackedbedabsorberusedinthisexperimentmaybeoperatedinthreemodes:
(a)Thepressuredropacrossthecolumnisdeterminedasafunctionofairandwaterflowrates.
(b)Theresponsetoimpulseinjectionofaninerttracerisusedtodeterminethewaterholduponthepacking.
(c)Thecolumnisoperatedatthesteadystateasanammoniaabsorber,andtheheightofatheoreticalplateis
determinedasafunctionofairandwaterflowrates.
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Ingeneral,severallabsessionsareneededtoexploreallofthesemodes.
C.SCENARIO
Packedcolumnsarecommonlyemployedtocarryoutabsorptionandscrubbingoperations.Theyprovidea
mediuminwhichcountercurrenttwophaseflowoccurs,andinwhicharelativelylargegasfluidinterface
perunitvolumeofcolumnvolumeexists.Becauseofthenatureofthepackingmaterial(oftenaceramic)a
packedcolumncanoperateusingstronglycorrosivefluids.Packedcolumnsareoftenmoreeconomicalto
buildandoperatethantheirplateorbubblecapcolumncounterparts,althoughpressuredropscanbehigh,
whichrequireslargergasblowerswithhighenergyconsumption.
Thepackedbedabsorberinthisexperimentistobeusedeventuallytoremoveammoniafromawasteair
stream.Beforerunningammonia,however,itisnecessarytodeterminewhatwaterandairflowratescanbe
accommodated,tomeasurethepressuredropacrossthebedsothattheairblowercanbespecified,andto
testanoninvasivemethodformeasuringtheamountofwaterhelduponthepacking,sothatincipient
floodingcanbedetected.
Anairstreamfromadriercontainsroughly0.10%byweight(1000ppm)ammonia.Environmental
regulationsprohibitdischargeoftheammoniaintotheair,andthusasmallpackedbedscrubberhasbeenset
uptopilottheammoniaremovalprocess.Yourjobistorunthescrubberatvariousairflowandwaterflow
rates,andcollectdatafromwhichcanbecalculatedtheheightofatransferunitforthepackingusedinthe
scrubber.Theresultswillbepassedtoadesigngroupwhichwilldesignafullscalescrubber,basedontheair
flowratefromthedrierandthemaximumallowableammoniacontentoftheeffluentair.
Yourjob,asagroup,istosetforthandcarryoutaseriesofpressuredrop,tracerresponse,andammonia
absorptionexperimentsthatwillprovidedata,andresultsderivedfromthedata,thatserveasagoodbasisfor
thedesignofafullscalescrubber.
D.APPARATUS
Thepackedcolumn(seeFig.1)consistsofa4"IDby36"longsectionofborosilicatepipesittingona4"by
2"borosilicatewell.Stainlesssteeltop,bottomandsideplatesaresealedwithTeflongasketsandprovided
withair,water,sampleandpressuretapconnections.About30inchesofceramic3/8"Raschigringpacking
issupportedabovetheairentrypoint.Thewatereffluentlineis1/2"stainlesstubingwithSwagelockfittings
thatpermittheleveloftheexitline,andthusthelevelofthewaterinthecolumnbottom,tobeadjusted.
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Waterenteringthetopofthecolumnisdistributedevenlyoverthepackingbya4armdistributor.Theair,
water,andammoniafeedratesaresetmanuallyandmeasuredbyrotameters.Awatermanometerisusedto
measurethepressuredropacrossthepacking.Aninfraredammoniaanalyzersamplestheeffluentairstream
andindicatestheammonialevel,typically50to1000ppm,inthisstream.Thesignalfromthisanalyzeris
acquiredbyaA/DboardmountedinamicrocomputerandprocessedbyaLabVIEWprogram.
ThepackingconsistsofceramicRaschigrings,length3/8inch,width3/8inch,wallthickness1/16inch,
weight51lbs/cubicfoot,equivalentsphericaldiameter0.35inch,0.68voidfraction,surfacearea134sq
feet/cubicfoot.
Asyringeisusedtoinjectpotassiumorsodiumchloridesolutionatthetoporbottomofthecolumn.
Typically10mlof0.2MKCltracerisinjected.Thetracerconcentrationismeasuredbyaconductivitycell
locatedinthewatereffluentline,thecellbeingconnectedtoaYSIconductivitymeter.Thesignalfromthe
meterisacquiredbyaLabVIEWprogramviaaNationalInstrumentsA/Dboard.Fromtheresponseto
impulsetracerinjectionthevolumeofwaterbetweentheinjectionpointandmeasurementpointmaybe
calculated.
Regulatorsaremountedinwaterandairsupplylinesinordertoreducetheeffectofsupplypressure
variationsontheflowrates.Ifthesupplypressuresarerelativelyconstanttheseregulatorsmayberemoved.
E.PROCEDURE
Inspection
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Theapparatusshouldbeexaminedcarefully.Checkthattheeffluentwaterlinefromthecolumnisoverthe
drainandthat,ifammoniaistobeused,theeffluentairentersthelaboratorychemicalhoodsystem.Theball
valvesonthetracerinjectionlinesshouldbeclosed.Theairpressureregulatorshouldread20to40psig.
Notethattheairrotameteroperatesatessentiallyatmosphericpressure,regardlessoftheregulatorsetting.
CalibrationoftheWaterFlowRotameter
Withtheairflowoff,setthewaterflowratetoalowvalueusingthewaterrotameter(readthecenterofthe
ball),andrecordthetimeneededtocollect250mlofeffluentwater.Adjustthewaterexitlinelevelif
necessarytoproduce5to10cmofwaterinthebottomofthecolumn.Thenincreasethewaterflowratein
about6incrementsovertherangeavailable,measuringit(inml/min)ateachsetting.Thewaterrotameteris
nowcalibrated.
DryColumnPressureDrop
Withnowaterflowbutwithawatersealinthewatereffluentline,settheairflowrateateightortenevenly
spacedpointsontheairrotameter,withamaximumratetypically6to10scfm.Ateachsteadystatethe
pressuredropacrossthedrypackingshouldbemeasuredusingthewatermanometer.Afterthefinalhigh
pressuredrophasbeenrecorded,theprocessshouldbereversedanddatashouldbetakenatdecreasingair
flowratesoverthesamerange.Fromthesedataadrycolumnpressuredropvs.airflowrateplotcanbe
constructed.
PressureDropasaFunctionofAirandWaterRates
Forarangeofwaterflowratesandairflowrates,allowthecolumntocometosteadystateandmeasurethe
pressuredropusingthewatermanometer.Atthehigherwaterandairflowratesyoumayseeflooding,i.e.a
continuingaccumulationoflargeamountsofwateronthepacking,coupledwithaveryhighpressuredrop
(whichmayblowtheliquidsealatthebottomofthecolumn).Infullfloodingasteadystatewillnotbe
possible.Takedatathatdefinetheairrate/waterrateregionthatproducesfloodingaswellaspossible.Atair
flowratesbelowfloodingthetimeconstantofthecolumnisquiteshort,ontheorderof10to30seconds,so
thatmanyrunscanbemadeinarelativelyshorttime.
Pleasereportyourresultsinthefollowingunits:length=ft,volume=ft3,time=seconds,mass=pounds
mass(lbm)andmassflux=lbm/(ft2s).
LiquidHoldupMeasurement
Atagivensteadystate,theliquidholdupcanbemeasuredbyanindicatordilutiontechnique.Usinga
syringe,10mlof0.2NKClisinjectedrapidlyintoeitherthetoporbottominjectionport(Notethattracer
concentrationmaybevariedtogivethebestresponse,andthatNaClorNH4Clmayalsobeusedastracers).
Theconductivityofthewaterexitingfromthecolumnismeasuredusingtheconductivitymeterandrecorded
asafunctionoftimeusingacomputerbaseddataacquisitionsystem.
ThecomputerusedwiththeexperimentisaPentiummachine.WeassumethatdirectoryZZQB45containsa
recentversionofMicrosoftQuickBASIC,andthatprogramTRACER04.BASisinZZQB45.Afterbooting
thecomputer,attheDOSprompttypeCD\ZZQB45toconnecttoZZQB45,andthentypeQBTRACER04.
Thisloadstheprogram.NowhitALTRtoruntheprogram,andfollowtheinstructionsissuedbythe
program.Theprogramwillcollectbaselinedata,andthencallfortheinjectionoftracer.Usually10mlof0.2
MKCltracerisinjected.
AlternatelyaNationalInstrumentsLabVIEWprogramwillbeusedtoacquire,plot,andprocessthetracer
responsedata.
Fromthedataontracerconcentrationasafunctionoftimethemeanresidencetimecanbedetermined,as
discussedinsectionHbelow.Sincethewaterflowrateisknown,thewatervolumebetweentheinjectionand
measurementpointscanbefound.Thentheholduponthepackingisfoundbydifference.Notethatthese
calculationsaredonebytheprogram,andcanalsobedonebyloadingthedatawrittentoafilebythe
programintoaspreadsheet,e.g.EXCEL.
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Severaltracerinjectionrunsshouldbemade,someathigherairandwaterflowratesthatproducesignificant
holdup.Typically,atahighwaterflowrate,severaldifferentairflowrateswouldbeused,thelast
correspondingtoincipientflooding,i.e.toalargeholdupofwateronthepacking.Duringtheserunsthe
waterexitlineshouldbeadjustedtogiveminimalwaterlevelinthecolumnbottom,say2to4cm.Butbe
surethatnoairleavesthewatereffluentline,i.e.thatthewatersealatthebottomofthecolumnisnotlost.A
lostsealcanberecoveredbyturningdowntheairflowrateforashorttimeandallowingthewaterdischarge
linetofill.
Youcanverify,atleastroughly,theholdupdeterminedasabovebyshuttingoffthewaterflowuntilasteady
stateisreached,measuringtheincreaseinwaterlevelinthecolumnbottom,andcollectingthewaterthat
drainsfromthecolumnfollowingwatershutoff.
AmmoniaAbsorption
oTurnontheMSAanalyzerandallowtowarmupfor30minutes.Theanalyzershoulddrawaroomair
sample.Zerotheanalyzermeterusingthecontrolprovided.
oOpentheammoniacylindervalveabout1/2turn,settheregulatorpressureto20psig,openanyvalves
betweentheregulatorandtherotameterwide,adjusttherotametervalvetoproduceareadingof150atthe
centeroftheball.Optionally,opentherotametervalvefurthertoproducealargerflowofammonia,andthus
alargereffluentammonialevel.(IfnecessaryCAREFULLYcheckforammonialeaksusingamodified
squeezebottleofmoderatelyconcentratedHCluseeyeprotection!tosprayastreamofHClontubing
jointsandvalvepacking.)
oSetabaseairflowrateandammoniaflowrate,asindicatedbytherotameters.Withnowaterflow,allow
thecolumntocometosteadystateandnotetheanalyzerreading.
oConverttheairflowratefromSCFMtogmol/minandcalculatetheammoniaflowrateingmol/minfrom
theammoniarotametercalibrationdata(fullscaleis329standardcc/minat20psigpressureinthe
rotameter).Fromthesevaluescalculatetheammonialevelintheairfeedstream.(Notethatasamplingpoint
couldbeaddedtotheair+ammoniafeedline,butthattheammonialevelatthispointmay,atlowairflow
rates,exceedthe1000ppmmaximuminputtotheanalyzer.Ifthecolumnisrundry,afterafewminutesthe
ammonialevelintheeffluentairwillequalthefeedlevel,andtheanalyzerwilldisplaythislevelifitisless
than2000ppm.)
oSet(andthenmonitor)thedesiredNH3,airflow,andwaterflowrates.Connecttheanalyzertotheeffluent
gasstream,recordtheanalyzerreading(assumedtobemolefraction).Taketheammoniarotameterreading
whenasteadystatehasbeenachieved,whichshouldtakeabout5minutes.
oRecordthepressuredropacrossthepackedcolumn.
oBasedontheattachednotes,calculatethenumberoftransferunits(NTU)andtheheightofatransferunit
(HTU).
oRepeattheabovestepsforcombinationsofwaterflowratesandairflowrates.Combinationsleadingto
floodingshouldbediscarded.Theammoniafeedrateshouldbesuchthatmeasurableammoniaispresentin
theeffluentair.
Anammoniamassbalance,usedtofindxB,is
Lx0+VyF=LxB+Vy1
Withx0=0,wehave
xB=(V/L)(yFy1)
whereVisthevaporrate(g/min)andListheliquidrate(g/min).
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F.AMMONIAROTAMETERCALIBRATION
UsethevalveprovidedtopassNH3fromtherotameterthroughafrittedglassabsorptiondeviceintoanHCl
solution(ofsuitableconcentration)containingphenolphthalein.Findthetimeneededtoneutralizeallthe
HCl.Fromthedataobtained,findtheflowrateofNH3atseveralrotametersettings.
G.REPORT
Showthecalibrationcurveforthewaterrotameter.Plotthepressuredrop(inchesH20)asafunctionofair
flowrate(SCFM)onaloglogplot,withwaterflowrateasaparameter.Includethedrypackingdata.Note
that,ifpressuredropvariesasthesquareofairflowrate,astraightlinewithaslopeof2shouldbeobtained.
Departure(inthedirectionofhigherpressuredrop)fromthecurvedefinedbythelowairflowpointsmay
indicateflooding.Leva(seereferencebelow,page28,Figure10)providesdataforasimilarcolumn.
CompareyourresultsalsowiththecorrelationinPerry'sHandbook.
Presentanddiscusstheresultsoftheindicatordilutionmeasurements.Provideacompletesamplecalculation
foratleastonerun,includingplotsoftracerconcentrationvs.timefortopandbottominjections.Usearun
inwhichtheliquidholdupwasrelativelylarge.Doesthewaterholduponthepackingincreasesignificantly
asthefloodingpointisapproached?
Fortheammoniaabsorptionruns,calculateforeachruntheheightofatheoreticalplate,anddiscusshowthis
varies(ifatall)withtheairandwaterflowrates.
Clickhereforguidelinesforthewrittenandoralreports.
H.NOTESONGASABSORPTION
Asthecarriergasmovesupthecolumnthesolutegastransfersfromthecarriergastothedescendingliquid.
Letrbetherateoftransferingmol/mincm,andletzbethedistancefromthebottomofthecolumnincm.
Thenwehave(seedrawingbelow)
Vdy/dz=r
and
Ldx/dz=r
whereVandLare(assumedconstant)vaporandliquidrates(gmol/min),andyandxarethegasphaseand
liquidphasemolefractions.Wecandefinethemasstransferrateas
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r=k[yy*(x)]
wherey*(x)isthegasphasemolefractioninequilibriumwiththeliquidphasemolefractionx,andkisa
masstransfercoefficient.Forthegasphasewehave
dy/dz=(k/V)(yy*)ordy/(yy*)=(k/V)dz
or,integratingfromz=0toz=zF,
Theintegralontherightisameasureofthedifficultyoftransferringsolutegasthesmallerthedrivingforce
yy*,thelargertheintegral,whichwecallthenumberoftransferunits(NTU).Inordertoevaluatethe
integralwemustfindx(y)andthusy*(x(y)).x(y)followsfromasolutebalancearound,say,thetopofthe
column.Inparticular,wehavetheoperatinglineequation
LxB+Vy=Lx+VyB
or
x=(V/L)(yyB)
when,asisusual,xB=0.Theintegrand
[yy*((V/L)(yyB))]1
canbeevaluatedintermsofywhenthevaporliquidequilibriumfunctiony*(x)isknown.Wheny*=KHx,
theintegralcanbefoundanalytically.(KHistheHenry'sLawconstant.)FromzFandNTUtheheightofa
transferunit(HTU)isfound.
SampleCalculation
Airflowrate=7.0cfmat70Fand1atm
Waterflowrate=500ml/min
xB=0
NH3inairfeed=20,000ppm(calculatedfromairandNH3flowrates)
NH3ineffluentair=250ppm(fromAnalyzer)
V=7(ft3/min)(28.32L/ft3)(gmol/22.4L)(492/530)=8.125gmol/min
L=500(ml/min)(1g/ml)(1gmol/18g)=27.8gmol/min
yA=(20,000/17)/(1,000,000/29)=0.03400
yB=(250/17)/(1,000,000/29)=0.00043
AssumingT=50F,fromPerrywehavethatthepNH3over0.05molefractionaqueousammonia=0.47psia,
whichgivesy=0.47/14.7=0.0319molefractionammonia.Thus
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KH=y/x=0.0319/0.050=0.638
Fortheoperatingline
x=(V/L)yyB=0.296y0.00043
and
yy*=yKHx=y0.638(0.296y0.00043)
or
yy*=0.811y+0.000274
WenowhaveforNTU,usingMATHEMATICAorproceedinganalytically,
whichseemsreasonable.TheMATHEMATICAexpressionwhichcarriesouttheintegrationanalyticallyis
Integrate[(0.811y+0.000274)1,{y,0.00042,0.03400}]
I.RESIDENCETIMEDISTRIBUTIONTHEORY
Withoutderivingthetheory,weconsideranimpulseinjectionofaninerttracerintoaflowsystem(wellor
poorlymixed)withvolumetricflowrateQandvolumeV.Wecansay,first,thatallthetracerinjectedmust
leaveeventually.Second,allthefluidinthesystemattimezeromusteventuallybewashedoutandreplaced
bynewfluid.Thesestatementscanbeshowntocorrespondtotheequations
and
whereC(t)istheconcentrationoftracerintheeffluentfollowingtheinjectionofamountDoftraceratthe
systeminletattimet=0.Also,V/Qisthemeanresidencetimeoffluidinthesystem.NotethatCmaybe
replacedinthesecondequationbyamultipleofC,saykC,withoutaffectingthemeanresidencetimeV/Q.
FromV/Q,ifQisknown,wecanfindV.Forevenlyspacedeffluentconcentrationdatawecanusenumerical
integration,saySimpson'sRule,tofindV/Q,asshowninthefollowingexample,whereWdenotesthe
Simpson'sRuleweights(1424....241).
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Then,usingSimpson'sRule[(Dt/3)(142424....241)],withDt=2,
and
IfQ=200ml/min,thesystemvolumeVis200*3.368=673.6ml.Suchcalculationscanbedoneeasily
usingaspreadsheetiftandC(t)aregivenatevenlyspacedtimes.
AnalternatetoSimpson'sRuleistrapezoidalrulenumericalintegration,[(Dt/2)(1222...21)],whichcan
beusedwithasmalllossinaccuracy.
J.SAMPLECALCULATIONOFPRESSUREDROP
InPerry'sHandbook(FifthEdition,Figure1839)wehaveaplotinwhichtheabscissaXis
X=(L/G)(rg/rL)0.5
andtheordinateYis
Y=G2Fpfm0.2/(rgrLg)
HereListheliquidmassflux(lbm/ft2s)basedontheareaoftheemptycolumn,Gisthegasmassflux
(lbm/ft2s),fistheratioofthedensityofwatertotheliquiddensity,FpisapackingfactorfoundinPerry
Table185(ft1),rgisthegasdensity(lbm/ft3),rListheliquidmassdensity(lbm/ft3),mistheliquid
viscosity(centipoises),andgistheaccelerationofgravity(32.2ft/s2).NotethatYisnotdimensionless.
Asanexample,consideranairflowrateof6.0ft3/minatSTP,awaterflowrateof1200g/s,andacolumn
IDof4inches(correspondingtoacolumnareaof0.0872ft2),
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G=((6*29)/(359*60))(1/0.0872)=0.0926lbm/ft2s
L=1200/(453.6*60*0.0872)=0.506lbm/ft2s
m=1.0centipoise
Fp=1000(1/ft)
f=1
rL=62.3lbm/ft3
rg=(29/359)(273.2/298.2)=0.0740lbm/ft3
and
X=(0.506/0.0926)(0.0740/62.3)0.5=0.188
Y=(0.09262*1000*10.2)/(0.074*62.3*32.2)=0.0578
BasedonFigure1839inPerry,thegasphasepressuredropperfootofpackingisabout1.40inchesofwater.
Ifthepackingheightis30inchesthepredictedpressuredropis3.5inchesofwater.
K.REFERENCES
1.Leva,Max.TowerPackingsandPackedTowerDesign,2ndEdition,U.S.StonewareCompany,Akron
Ohio(1953).
2.Perry,J.H.,Editor.ChemicalEngineersHandbook,5thEdition,McGrawHillBookCompany,pp.2119
(1973).
3.McCabeandSmith.UnitOperationsofChemicalEngineering,3rdEdition,pp.709715(1976).
L.COMMENTS
1.Useastripchartrecorder(ifavailable)torecordtheanalyzeroutputsignal.Therecordertracecanbeused
toseewhetherasteadystatehasbeenachieved.
2.Besuretoturnofftheammoniacylindermainvalvewhentherunsarecomplete.Alsoclosetheregulator
outletvalve,butnottootightly.
3.Positionanelephanttrunkconnectedtothelaboratoryventilationsystemnearthewatereffluentcollection
point,andmakesurethelaboratoryventilationblowerison.
4.Ammonia/watervaporliquidequilibriumdataatvarioustemperaturesareavailableinPerry'sHandbook.
FromthesedataaHenry'sLawconstantcanbederived(seesamplecalculationabove),andthisisusedinthe
NTUcalculation.Useathermometertomeasuretheeffluentwatertemperature.
5.Checktheammoniacylinderpressuregaugebeforeandaftertherun.Itshouldshow80to120psig.A
lowerpressuremeanstheammoniacylindercontainsnomoreliquid,andtheTAorafacultymembermust
beinformed.
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BacktoE3810homepage
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