09462 Operating Instructions R1.docx

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