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US 2020/0399137A1 Dec.24,2020 mg/kg),Ca(2.8mg/kg),Mg(2.1mg/kg),Fe(0.3mg/kg),Ba (0.1mg/kg),Mn(0.08mg/kg),andSr(0.03mg/kg),fora purityofabout78.4%.Afterwashingwithaproximately 2-3volumeequivalentsofwater,thesodiumconcentration isreducedtoundetectablelevelsandthelithiumcarbonate hadthefolowingimpurities:Mg(5.9mg/kg),Ca(2.9 mg/kg),Ba(0.4mg/kg),Fe(0.4mg/kg),Mn(0.07mg/kg), andSr(0.07mg/kg),forapurityofgreaterthan9%. [0134] Thewashingconditionsmayafecttheamountof sodiumcarbonate/chlorideentrainedinthelithiumcarbon ateproduct. Example2 [0135] Theelectrolysisprocesconvertsapurified,con centrated lithium chloride solution into a concentrated [0137]Theanolyteflowsystemincludedafedtank, pump,degasingtank,chlorinescruber,andcolection tank.Alithiumchloridesolutionhavingaconcentrationof about21%byweightwasplacedintheanolytefedtankand heatedtoabout90°C.Theheatedsolutionwaspumpedinto theanodechamberofthecelinasinglepasmodeataflow rateofabout20cm3/min,corespondingtoafacevelocity ofabout0.13cm/s.Upon exitingthecel,thelithium chloridesolutionandentrainedchlorinegas(producedatthe anode)werepasedthroughintoadegasingtank,which was equipedwithachlorinescruber,toremovethe chlorine.Thelithiumchloridesolutionwasthenpumped intoacolectiontankforstorage. [0138] Thecatholyteflowsystemincludedafedtank, pump,andwaterfedsystem.Lithiumhydroxidewasplaced inthefeedtankandheatedtoabout95°C.andfedtothe cathodechamberoftheelectrochemicalcelinrecirculating modeataflowrateofabout50mL/min,corespondingto afacevelocityofabout0.3cm/s.Waterwasaddedcon tinuouslytothesystemusingaperistalticpumptomaintain aconstantlithiumhydroxideconcentration.Therateof aditionwasmonitoredbytheweightlosofthewatertank. Nitrogenwasbubledthroughthecatholyterecirculation tanktominimizethereactionoflithiumhydroxideand carbondioxidefromtheair. [0139] Table1summarizestheexperimentalconditions usedinteststodeterminetheefectoftheconcentrationof thecatholyte. TABLE 1 Experimentalparametersforelectrolysisexperiments. Value 3000 A/m 64 cm 60cm3 60cm3 21 wt % 0.5-0.7 90°C. 2-3 hours 0.13 cm/s 0.33 cm/s [0140] Duringoperationoftheelectrochemical cel, sampleswerecolectedatthecatholyteinletandoutletand anolyteoutletportsevery30minutes.Celvoltagewas monitoredatthecelterminalsusingahandheldmultimeter. Thediferencebetwentheinletandoutletcatholyte hydroxideconcentrationsandthecelvoltagewereusedto calculatetheeficiencyandenergyconsumptionofthecel. Results lithiumhydroxidesolutionforsubsequentconversionto lithiumbicarbonate.Thelimitingfactordeterminingthe eficiencyoftheelectrochemicalcelistheconcentrationof lithiumhydroxideinthecatholyte,duetoback-migrationof hydroxideacrosthemembrane.Therefore,theexperiment wasdesignedwhereintheelectrochemicalcelwasoperated atfourdiferenthydroxideconcentrationstomaptheefect ofthelithiumhydroxideconcentrationanddeterminethe maximumconcentrationthatcouldbeprepared.Theexperi mentwasdesignedtomeasurethecurenteficiencyand energyutilizationofthedialysisprocesasafunctionof hydroxideconcentration.Withintheelectrochemicalcel, underanapliedfield,lithiumcationsmigratefromthe anolytetocatholyte,whilewaterpresentiselectrolyzedto H,andOH atthecathode.Intheory,eachelectronpased intheexternalcircuitcorespondstoanincreaseofone lithiumhydroxidemoleculeinthecatholyte,leadingtoan increaseinconcentrationoflithiumhydroxidewithtime. Parameter Themainineficiencyintheproces,thebackmigrationof OH-ionsfromcatholytetoanolyte,isdependentontheOH concentrationofthecatholyte.Therefore,theexperiments reportedherewereperformedwiththeintentionofmain tainingtheOH concentrationofthecatholyteconstantby adingwaterataknownrate.Theeficiencyofthereaction wasmeasuredbycomparingtheactualrateofaditionof waterwiththetheoreticaladition. Example3.ElectrolyticProductionofLithium HydroxidefromLithiumChloride 14 [0136]ExperimentalSet-Up.Theelectrolysissystemcon sistedoftheelectrolysiscelhavinganolyteandcatholyte flowsystems.Electrolysisoflithiumchloridesolutionswas cariedoutusinganFM01electrolyzer(ascalemodelofthe FM21 electrolyzerusedcomercialyinthechlor-alkali industry)manufacturedbyICI.Theelectrolyzerincluded lantern blade-style electrodes (anode: ruthenium oxide coatedtitanium;andcathode:nickel),andaNafion®982 membrane.Theactivesurfaceareaofeachelectrodewas about64cm2(4x16cm),andthecelgap(distancemeasured anodetocathode)wasbetweenabout12-13mm.TheFM01 summarizedinTable2andareshowninFIGS.6to9.FIG. electrolyzerwasoperatedwiththeflowparaleltothe16cm direction(ascomparedwithaflowdirectionparaleltothe 4cmdimension,asitisintendedtobeoperated),asthis improvedthemanagementofchlorineandhydrogengases evolvedfromtheelectrodes.Inadition,althoughanolyte andcatholyteflowsarenormalyfedfromopositesidesof thecel,inthepresentexperiment,theanolyteandcatholyte werefedfromthesamesideoftheelectrochemicalcel. 6demonstratesthedificultyinmaintainingaconstant lithiumhydroxideconcentrationbasedsolelybyadjusting CurentDensity ElectrodeArea AnolyteVolume CatholyteVolume LiClInletConcentration LiClInletpH Temperature TimeofOperation Anolyte(LiCl)FlowVelocity Catholyte(LiOH)FlowVelocity [0141]Theresultsoftheconcentrationofthecatholyteare therateofwateradition,intheabsenceofreal-time measurementsofthehydroxideconcentration,because watercanbeconsumedoradedtothecatholytebyavariety ofmechanisms,includingelectrolysis,evaporation,and migrationacrosthemembranewithlithiumcations.In general,thedatasugestthatthehighertheinitialconcenPDF Image | Patent LITHIUM CHLORIDE CONTAINING BRINE
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