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17 byco-currentupflow.Samplealiquotswerecolectedafter 100cyclesandthepresenceofmetalswasanalyzedwithICP. Diferentialpressureacrossthebedremainedlowthroughout thecycles,althoughpressureinthetubingincreasedseveral 18 wasusedtotitrateforuptoabout4hourstoprovideastable pHofbetweenabout6.5and7,ensuringthatthepHisgreater than6.Thewaterandsupernatantareremovedandtheresult ingsolidmaterialisdriedinanoven.Theyieldwasabout80 kg(90%)providingLAIparticleshavingabimodaldistribu tionofabout100-125umandabout10um,asdetermined withaMicrotracLaserDifrationTypeAnalyzer.Thefre flowbulkdensitywasabout0.6g/mLandthetappedbulk densitywasabout0.8g/mL. Example15 AnalternateroutetopreparingtheLAImaterialsforuse herein according to a dry process that includes mixing approximately16kg.Al(OH)andabout17.1kgLiOH.HO inareactoruntilthedrymaterialsarethoroughlymixedand addingtothemixtureapproximately16.3Lofwater,andthe mixturewasheatedtoatemperatureofbetweenabout85and 90°C.andcontinuouslystifedforatleast4hours.Reaction progresswasmonitoredbytitratingsamplesfromthereac tionandafterthereactionwasdeterminedtobeatleast92% complete,thereactionwasslowlyneutralizedwithasolution containing31%byweightHCloveraperiodofabout2hours toprovideapHofbetweenabout5.5and7.5.Ametering pumpwasusedtotitrateforuptoabout4hourstoprovidea stablepHofbetweenofgreaterthan5.5.Thewaterand Supernatantareremovedbyheatingthereactortoatempera tureofabout110°C.untilatleast90% ofthemoisturehas beenremoved,andtheresultingSolidmaterialisdriedinan oven.Theyieldwasabout23kg(90%)providingLAIpar ticleshavingdiameteroflesthanofabout1um,asdeter minedwithaMicrotracLaserDifractionTypeAnalyzer.The freflowbulkdensitywasabout0.83g/mLandthetapped bulkdensitywasabout1g/mL. Asisunderstoodintheart,notalequipmentorappara tusesareshowninthefigures.Forexample,oneofskilinthe artwouldrecognizethatvariousholdingtanksand/orpumps maybeemployedinthepresentmethod. Thesingularforms“a”,“an and“the includepluralref erents,unlesthecontextclearlydictatesotherwise. Optional or optionaly means that the Subsequently describedeventorcircumstancesmayormaynotocur.The descriptionincludesinstanceswheretheeventorcircum stanceoccursandinstanceswhereitdoesnotoccur. Rangesmaybeexpressedhereinasfromaboutonepar ticularvalue,and/ortoaboutanotherparticularvalue.When Sucharangeisexpressed,itistobeunderstoodthatanother embodimentisfromtheoneparticularvalueand/ortothe otherparticularvalue,alongwithalcombinationswithin saidrange. Throughoutthisaplication,wherepatentsorpublications arereferenced,thedisclosuresofthesereferencesintheir entiretiesareintendedtobeincorporatedbyreferenceinto thisaplication,inordertomorefulydescribethestateofthe arttowhichtheinventionpertains,exceptwhentheserefer encecontradicttheStatementsmadeherein. timesduetoSorbentparticlesbypassingtheglaswooland5 colectingintheinfluentandefluenttubing.Fineswerenot observed,butbedvolumedecreasedduringthetestingdueto asorbentlosofapproximately19%overatotalof1300 cycles. The lithium capacity during loading ranged from about2.3mg Li/mLsorbentatthebeginningoftestingto about1.7mgLi/mLsorbentafterapproximately1300cycles ofloadingandunloadingofthecolumn.Correctionsforbed losweremadeindeterminingsorbentcapacitycalculations. Mechanical robustness of the sorbent material was tested asdescribedinExample1.Samplespreparedaccordingto15 Example12yieldedfinesreleasevaluesofabout0.17mg/J and0.10mg/J,forthe300-425and425-600umfractions, respectively. Example13 A 14LcapacityhighsheargranulatorfromLancaster (K-Lab)wasfitedwithapressuresprayertointroducethe binder/watersolutionuniformlyandrapidlytothepowder mixture.Approximately6000gofdriedLAIprepared25 accordingtoExample1(above)wasintroducedintotheLan castermixerandsheareduntilallargelumpswerebrokenup. Approximately100gofdistiledwaterwasintroducedand allowedtomixandthoroughlywetthepolymer/LAIpowder. Amixtureofabout1191gofKynarAquatec10,206fluo30 ropolymer/acrylicresin(Arkema,Inc.),approximately271g XL-702(apolycarbodiimidecroslinkeravailablefromPic asianPolymers),andabout1470gofdistiledwaterwere blendedandintroducedtothemixerstepwiseoveraperiodof 7minutesatmaximumpanspeedandmaximumbladespeed35 (about40RPM and3000RPM,respectively).Duringthis proces,about30%oftheagglomeratesproducedhadan averagediameterofgreaterthanabout850um.Thewet agglomeratedmixturewaspassedthroughtheVorti-Siv equippedwithan850 Limscreenusingceramicbals.The resultingmaterialwasthenpassedthrough600umScreenon theVorti-Sivwithceramicbalsandthendriedatatempera tureofabout60°C.,followedbycuringatatemperatureof about120°C.Thisresultedinafinaldistributionwhere80% ofmaterialfelinrangeofabout180to600um,suitablefor45 operationalcapacitytesting. Themechanicalrobustnessofparticlespreparedaccording toExample13havingdiametersrangingfromabout106-180 um, 180-300 um, and 300-425 um were tested, yielding samplefinesreleasevaluesofabout0.22mg/J,0.25mg/J,and50 0.27mg/J,respectively. Example14 AlargescalemethodforthepreparationofLAIparticulate55 materialforusehereinisprovided.Approximately20galof water was added to the reactor and heated to about 95° C. US 8,753,594B1 10 40 Approximately17.1kgofLiOH.HOwasaddedtothewater Asusedherein,recitationofthetermaboutandapproxi andagitateduntildisolved.Tothemixturewasaddedabout 57.7kgofAl(OH).Theresultingmixtureoflithiumand60 aluminumcompoundswasheatedtobetweenabout85-90°C. foratleastabout4hours.Waterwasadded,asnecesary,to maintainaconstantwatercontent.Reactionprogresswas monitoredbytitratingsamplesfromthereactionandafterthe reactionwasdeterminedtobeatleast92%complete,the65 reactionwasslowlyneutralizedwith6NHClover1hourto provideapHofbetweenabout6.5and7.Ameteringpump matelywithrespecttoarangeofvaluesshouldbeinterpreted toincludeboththeupperandlowerendoftherecitedrange. Although the present invention has been described in detail,itshouldbeunderstoodthatvariouschanges,Substi tutions,andalterationscanbemadehereuponwithoutdepart ingfromtheprincipleandscopeoftheinvention.Accord ingly,theScopeofthepresentinventionshouldbedetermined bythefollowingclaimsandtheirappropriatelegalequiva lents.PDF Image | Patent SORBENT FOR LITHIUM EXTRACTION
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