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US 8,691,169B2 34 Lithium carbonate obtained employing conventional methodsasdescribedinU.S.Pat.Nos.5,993,759,5,219,550, 4.261,960,4,036,718and4.243,392normallycontain99.2% LiCOwith0.2to0.3%sodiumand0.05to0.1%magne sium,contaminationlevelsthatdonotallowforuseinthe productionofbaterygradelithium. Thereareseveralpatentedmethodsfortheproductionof lithiumchlorideandlithiumcarbonate.Forexample,U.S. Pat.No.4,980,136describesamethodforproducingbatery gradelithiumchloridefromlithiumrichbrinesusingsolvent extractionswithaliphaticalcohol,thatisSubsequentlyevapo ratedleavinghighpuritycrystalinelithiumchlorides.Other methods,asdescribedinU.S.Pat.No.4,859,343teachthe useofionexchangecolumnsthatremovesodiumionsfrom chloridebrines. Giventhatitisverydificulttoproducelithiumchlorides withlesthan0.16%sodiumdirectlyfromlithiumcarbonates, Such carbonates are generally transformed into lithium hydroxideandthenintolithiumchlorideorthelithiumcar bonateistreatedwithhydrochloricacidyieldinglithium chloridethatcanbefurtherpurifiedviasuccessivecrystali Zations.Thedescribedmethods,eventhoughrequiringmul tiplesteps,resultinalithiumchlorideproductwhichissuit ableforelectrolysis,havingasodiumlevelbelow0.06%. SUMMARY OF THE INVENTION 10 15 25 Said solution is then filtered and then heated in order to convert the bicarbonate of lithium into lithium carbonate whichprecipitatesleavingtheimpuritiesinSolutionandgen eratingCOwhichcanthenberecirculated.Thelithiumcar bonatepulpmaythenbefilteredandsaidpulpcanbewashed andheatedtherebyproducingpurifiedbatergradelithium carbonate.Allremainingsolutionsmaythenbereturnedto theSolarevaporationpols. BRIEF DESCRIPTION OF THE FIGURES FIG.1describesaflowchartofthemethodforproduction oflithiumcarbonateinaccordancewiththepresentinvention. FIG. 2 describes the details of the method as well as the equipmentrequirementsfortheproductionofbaterygrade lithiumcarbonateinaccordancewiththepresentinvention. DESCRIPTION OF THE PREFERRED EMBODIMENTS Inordertoprovideabeterunderstandingofthemethodsof thepresentinvention,anilustrativeembodimentisprovided thatisnotmeanttobelimiting.FIGS.1and2wilberefer enced. Brineswithtypicalcompositions,suchasthoseobtained fromtheSalardeCauchariinArgentina,seeTable2,are concentratedinevaporationpoolsinordertoincreaselithium content.Typicalcompositionsforthesebrinesarepresented inTable3. Removalofmagnesiumwithcalciumhydroxidebefore removalofboronisadvantageousbecauseonecanthusavoid losoflithiumduetoco-precipitationthatoccurswhenone usesSodaashtoprecipitatemagnesiumawayfromthecar bonate.Thisvariantmaybeemployedwhenthebrinehas been concentrated so that itcontains 0.9 to 1.2% lithium. Moreover,notonlyisvirtualyalmagnesiumprecipitatedin theformofmagnesiumhydroxide,butalsosignificantquan 35 titiesofcalciumintheformofgypsum(CaSO4.2H2O)and boronintheformofcalciumborate(CaBO.6H2O)thereby eliminatingbothboronandcalciumfromthesample. Given that precipitation of magnesium with calcium hydroxideleavesvirtualynoamountsofthismetalinthe40 brine,itisunnecessarytohaveaditionalstepstoremove magnesiumnorismotherliquorrequiredtobeaddedtodilute thebrine.Asaresult,itispossibletoprecipitatelithium carbonateabsentsignificantquantitiesofboronandmagne siumdirectlyfrombrine.Thelithiumcarbonatecanthenbe 45 furtherpurifiedinordertoreduceaditionalimpurities,such assodiumandcalciumtherebyconvertingsaidlithiumcar bonatetobicarbonateoflithium(LiHCO)byaddingcar bonicacid(HCO3)producedfromcarbondioxide(CO). One can then heat said bicarbonate of lithium solution in 50 ordertoproduceahighlypurifiedlithiumcarbonateprecipi tatewhiletheimpuritiesremaininsolution.Thus,thisinven tionrelatestoamethodforproductionofbaterygrade lithiumcarbonatebyemployingaconversiontobicarbonate oflithiumandthenbacktolithiumcarbonate.Saidmethod 55 beginswithprecipitationofmagnesiumfrombrineusinga gypsumsolution(Ca(OH))followedbyanevaporationstep wheremagnesium,calciumandboroncontainingcompounds areprecipitated.Themagnesiumdepletedbrineissubjectto Solventextractioninordertoremoveanyremainingboron. 60 Theresultantbrineisthenfurtherpurifiedbyreactionwithan aqueoussolutionofsodiumcarbonate,alsoknownasSoda ash(NaCO)at80to100°C.inordertoprecipitatethe lithiumcarbonate.Afterwashingandfilteringthelithium carbonatecake,saidcakeisre-dissolvedincoldwaterSatu 65 ratedwithCO containingcarbonicacidwhichreactswiththe lithiumcarbonatetoproducesolublebicarbonateoflithium. 30 % % TABLE 2 TypicalchemicalcompositionforbrinesfromSalardeCauchari. Element Li C Na K Ca Mg SO HBO HO O.OS 14.7O 9.80 4.81 O.OO O.14 O.197 0.60 72.33 TABLE 3 TypicalchemicalcompositionforbrinesconcentratedviaSolar evaporationfromtheSalardeCauchari. Element Li C Na K Ca Mg SO HBO H2O O.39 12.70 S.41 2.70 2.52 9.91 5.92 2.53 SS.42 InFIG.1,brine1,asdescribedinTable2,ismixedand allowedtoreactwithasaturatedslackedlime(Ca(OH)2)2 Solution,inaconventionalreactor3suchasareactioncham berwithstirer,inquantitiessuficienttoprovoketheprecipi tationofalmagnesiumchlorideandSulfatespresentinsaid brine,inaccordancewiththefollowingformulas: (3) TheNaOHproducedinreaction(3)alsoreactswiththe MgCl,toformMg(OH),inaccordancewiththefollowing reaction: Allthesereactionsarespontaneous,giventhatthestandard reactionfreenergies,inawidespectrumoftemperature,arePDF Image | Patent Production of Li from Industrial Brine
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