09462 Operating Instructions R1.docx
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09462 Operating Instructions R1.docx
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09462OperatingInstructionsR1
ChemicalDesignInc.
PROCESSES•PLANTS•EQUIPMENT
OPERATINGINSTRUCTIONS
POLYPLANTVENTGASRECOVERY
CDI0946-2
GOUDIANINNERMONGOLIAJINGYANGENERGYCO.,LTD.
INNERMONGOLIA,CHINA
CONFIDENTIAL
Preparedby
CHEMICALDESIGN,INC.
285MarketStreet
P.O.Box513
Lockport,NewYork14095-0513
Phone(716)433-6744Fax(716)439-4019
Rev.0:
8July2010
Rev.1:
9August2010
1.0PROCESSDESCRIPTION
1.1VENTGASCONDENSING
1.2COMPRESSION
1.3ABSORPTIONANDDISTILLATION
1.4ADSORPTIONSYSTEM
1.5DESIGNBASIS
1.6UTILITIES
2.0PRESTARTUP
2.1INSTALLTOWERPACKING
2.2PUMPS
2.3FILLANDDRYHEATINGMEDIUMSYSTEM
2.4LOADCARBONINTOADSORBERST-204A/B/C
2.5BLANKETSYSTEMWITHNITROGEN
2.6COMPRESSORS
2.7CALIBRATEINSTRUMENTS
2.8CHECKPROGRAMLOGIC
2.8.1VALVEAUTO/MANUAL
2.8.2SEQUENCEAUTO/MANUAL
2.8.3STEPADVANCE
2.8.4STEPINCOMPLETEALARM
2.8.5VALVEPOSITIONALARM
2.8.6UNITSHUTDOWN
2.8.7DEPRESSURINGSTEPRAMP
2.9CHECKSEQUENCECONTROL
2.10CHECKEMERGENCYSHUTDOWNSYSTEMS
2.11COMMISSIONUTILITIES
2.12PUMPDOWNANDCHARGEREFRIGERANTSYSTEMS
2.13INSULATION
3.0STARTUP
3.1PURGEWITHNITROGEN
3.2DRYADSORBERS
3.3CYCLEADSORBERS
3.4DRYFEEDCOMPRESSORS
3.5DISPLACENITROGENWITHHYDROGEN
3.6ESTABLISHLIQUIDLEVELSINTOWERS,T-202ANDT-203
3.7STARTCOMPRESSORS
3.8CIRCULATECHLOROSILANELIQUIDS
3.9COMMISSIONREFRIGERATIONSYSTEM
3.10ESTABLISHTEMPERATUREPROFILEINHCLTOWER,T-203
3.10.1COMMISSIONPRESSURECONTROL
3.10.2ADMITSTEAMTOREBOILER
3.10.3ESTABLISHREFLUXFLOW
3.11INCREASEFEEDVENTGASFLOW
4.0SHUTDOWNS
4.1PROCESSUPSETS
4.2LONGTERMUPSETS
4.3NORMALSHUTDOWN
5.0OPERATINGPROCEDURES
5.1TYPICALCOMPRESSORSTARTUPPROCEDURES(TOBECONFIRMEDBYCOMPRESSORVENDOR)
5.2CARBONLOADINGPROCEDURE
5.3CARBONDRYINGPROCEDURE
6.0SAFETY
6.1HYDROGENSAFETY
6.2HCLSAFETY
6.3CHLOROSILANESAFETY
APPENDIX
A.SAFETYHCL
B.SAFEHANDLINGOFCHLOROSILANES
C.FIREFIGHTINGINSTRUCTIONS
1.0
PROCESSDESCRIPTION
TheCVDReactorVentGasRecoveryUnittakestheventgasfromthereactorsthatdepositsilicononhightemperaturerods,andseparatesthestreamintoliquidchlorosilanes,hydrogenchloridegas,andhydrogengas.Thehydrogengasisreturnedtothehydrogensystematveryhighpurity(<1vppmtotalcontaminants)andisrecycledtotheCVDReactors.Nitrogen,methane,andothercontaminantsnotspecifiedinthefeedgasarenotremovedbytheVentGasRecoveryUnit.TheHClvaporandliquidchlorosilanesarerecoveredandrecycledtootherpartsoftheplant.
TheprocessisdesignedbyCDI;componentsarepurchasedandinstalledbyGoudianInnerMongoliaJingyangEnergyCo.,Ltd.accordingtotheP&ID’s.TheheatandmaterialbalanceisshownonCDIdrawing0946-2-PF-100.
1.1VentGasCondensing
IncomingventgasentersaseriesofverticalBEMexchangersthatareusedtocondensethebulkofthechlorosilanesfromthegas.Agas/gasinterchanger,E-202,isfirstusedtochillthegasdownto~25°Cwhilewarmingupthereturninggasbeforeenteringthefeedcompressors.A-15°CR-507Achiller,E-204,furthercondensestheliquidanddrainstothechlorosilaneseparator,D-202.Thecondensedliquidsaredrainedintochlorosilanesurgetank,D-201;hydrogen,HCl,anduncondensedchlorosilanesaresenttoventgaschiller,E-205,wherechlorosilanesarefurthercondensed.Theliquidgasmixtureisthenalsosenttochlorosilanesurgetank,D-201,wherethegasisseparatedfromtheliquid.
1.2Compression
Ventgasfromthereactorsenterstheunitat4.0kg/cm2-G.Thepurificationstepshavebeendesignedtooperateat11kg/cm2-G,whichisthehighestpressureexpectedfromasinglestage-reciprocatingcompressorbeforehittingatemperaturelimitationonthedischarge.Mechanicaldesignis18.3kg/cm2-G.
1.3AbsorptionandDistillationSystem
Theabsorber/distillationsystemreducestheloadofcontaminantstothecarbonadsorbersbyabsorbingHClinarefrigeratedsiliconchlorideliquid.
Theincominggascontactsaliquidstreamcontainingprimarilytrichlorosilaneandsilicontetrachlorideat-40°CintheHClAbsorber,T-202,where99%ofincomingHClisabsorbed.TheHClrichliquidfromthebottomoftheHClabsorberisstrippedoftheHClintheHClTower,T-203,andseparatedintherefluxdrum,D-207,at-40°C.ThevaporenterstheHClheater,E-217,toheatuptheHClto20°Cbeforebeingsenttostorage.
Thecompositionofthefeedgaswilldeterminethecirculatingchlorosilaneliquidcomposition.Theflowofchlorosilanesreturningtotheabsorbertower,T-202,iscontrolledbylevelinthebottomoftheHClTower,T-203.Variationsingasflowtotheabsorberarenotcritical.Thissystemwilloperatesatisfactorywithdesignliquidrateevenwhenthegasflowrateiswellbelowdesign.
TheperformanceoftheHClTower,T-203,issensitivetothechlorosilanefeedflowrateandtemperaturebecausetheserepresentthemajorheatload.VariationinHClcontent,fromzerotodesignvalue,haslittleimpactonperformance.Therefore,theflowandtemperatureofthechlorosilanefeedtotheHClTowerarecontrolled.Thereboilerdutyusesafeedforwardtypecontrolmethodthatcalculatedtheoreticalsteamflowratebasedonfeedtemperatureandfeedflow(seeSection3.10.2)
1.4AdsorptionSystem
ActivatedcarbonatambienttemperatureremovesHClandchlorosilanesfromthehydrogenleavingtheHClAbsorber,T-204.ThegasentersthebottomofthecolumnandflowsupwardthroughtheChlorsorbRL-13carbon;effluenthydrogenis99.9999%pure.Carbondioxide,carbonmonoxide,nitrogen,methanearenotremovedasnoneofthesecontaminantswerespecifiedintheincomingventgas.
Theadsorbertowersoperateona7-houradsorptioncycle,withonetoweralwaysinservicewhileasecondandthirdtowerregenerate.Regenerationconsistsofdepressuring,heating,hotpurge,cooling,andrepressuring.
Duringregeneration,make-upH2at9.5kg/cm2-Gisusedforpurgingandpressurizingtheadsorbervessels.AdsorbersuseSylthermXLTpumpedthroughthecoilslocatedinsideandoutsidethevesselsforheatingandcooling.
1.5DesignBasis
VentGas
RecoveredChlorosilanes
RecoveredHydrogen
RecoveredHCl
Pressure,kg/cm2-A
5.0
>7.0
>10.5
>7.0
Temperature,°C
45
40
50
20
Composition,kg/hr
H2
1,973
nil
1,934
0.1
HCl
1,131
<200wppm
nil
1,127
SiH2Cl2
74.6
71.2
nil
nil
SiHCl3
25,593
25,183
nil
nil
SiCl4
6,744
6,709
nil
nil
N2
<500vppm
nil
<500vppm
nil
Notes:
1.NitrogeninfeedgasisnotremovedbyCDIunit.
2.Flowslistedabovearesharedbetweentwoventgasrecoveryunits.
1.5.1DetailofPerformanceTest
Duringtheinitialstartup,theadsorberheatingandcoolingsystem,theliquidchlorosilanecirculationbetweentheHClAbsorber,T-202,andtheHClDistillation,T-203,canbeprovenatdesignrate.Compressorswillalsobeprovenatdesigncapacitysincefeedcompressorcapacitycontrolrecyclesgasfromthedischargedrum,D-204,toE-202.Dependingonavailablereactorventgas,itmaybepossibletoprovecapacityofthecondensationequipment,refrigerationsystems,andcarbonadsorbers.
Flowmetersandlaboratoryanalysisofperiodicsampleswillbeusedtoconstructamaterialbalancebasedontheactualfeedfora24-hourperiod.Recoveryofvariouscompoundswillbeasfollows:
H2:
99.2%recovery
HCl:
99.3%recovery
DCS:
99.2%recovery
TCS:
99.4%recovery
STC:
99.5%recovery
CompositionofrecoveredstreamswillmeettherequirementsoftheContractandallAmendments.
TherecycledH2gasshallproducepolysiliconcrystalproductequivalenttothatproducedusingvaporizedliquidH2inanevaluationreactor.
1.6Utilities
Seeutilitiessummary(publishedseparately)forestimatedvalues.Pleaseaddanallowanceforheatloss,etc.
2.0
PRE-STARTUP
2.1InstallTowerPacking
RemoveliquiddistributorsandcheckbedsupportgridsforT-202,andT-203.Installthefollowingpackingmaterialineachtower:
T-202Top:
1,067mmI.D.x4,572mm1”(25mm)diameterPallRings
T-202Bottom:
1,067mmI.D.x4,572mm1”(25mm)diameterPallRings
T-203Top:
914mmO.D.x2,000mmKoch-GlitschFlexipak1.4YHCstructuredpacking
T-203Middle:
914mmO.D.x1,000mmKoch-GlitschFlexipak1.4YHCstructuredpacking
T-203Bottom:
1,829mmI.D.x6,096mm2”(50mm)diameterPallRings
Aswithallpackedtowers,goodliquiddistributioniscriticaltosatisfactoryoperation.
Confirmthatliquiddistributortraysarelevel,bolteddown,andinletdistributordischargesliquidwheredesired.
2.2Pumps
Checkpumpbreakersettings,andbumppumpstoconfirmcorrectrotation.
2.3FillandDryHeatingMediumSystem
Purgeentiresystemwithdrycompressedairornitrogentoremoveasmuchwater,debris,andcontaminantsaspossible.
CheckandcleanstrainerspriortoP-205A/B/C.
UseNozzleAonexpansionTank,D-205,tofillwithSylthermXLTasnecessary.CDIrecommendsfillingallthree(3)vesselswithSylthermXLTatthesametime.Usingthepumps,flowthroughthecoldheatingmediumsupplyvalvesandoutthehotheatingmediumreturnvalves.AdjustmanualvalvesaroundP-205BtoflowthroughtheexpansiontankandtouseP-205AorB.Afterfillingthelines,closethecoldheatingmediumsupplyvalvesandhotheatingmediumreturnvalves,thenopenthehotheatingmediumsupplyvalvesandthecoldheatingmediumreturnvalves.AdjustmanualvalvesaroundP-205BtoflowthroughtheexpansiontankandallowuseofP-205BorC.Thiswillhelpremovealltheairoutofthepiping.OpenHPV’sandLPD’s,includingthecoreventontheadsorber(NozzleK)
Continuefillinguntillevelinexpansiontankis
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