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TABLE 4 resultsoffourstagesolidliquidcros-flowextractionbytributylphosphatefrom anoldbrinewithamagnesium tolithiummassratioof20.0inasaltlakelocatedinQinghaiprovince E(Lit)/%L E (Mg2+)/% Stageof Single Accumulative Single m(Mg2+)/m(Lit) Single Accumulative extraction stage stages stage stage stages Accumulative stage m(Mg2+)/m,(Li+) ?? 40.07 40.07 16.01 16.01 7.97 7.97 27.97 ?M?? ? 43.14 65.92 16.02 29.47 10.39 8.92 41.31 44.35 81.03 15.75 40.57 14.67 9.99 62.54 44.99 89.57 15.83 49.98 22.00 11.14 95.69 US 10,246,341B2 Theextractedphasesfrom fourstagesweremergedand 15phasewasfinalyobtainedafterphaseseparation,with a organicextractionphaseandwaterwererespectivelyaded decreasedmagnesiumtolithiumratio.Sampleswereana inaseparatingfunelwithaphaseratiooforganicphaseto lyzedandresultsshowedthatreverseextractionrateofLit waterV/Vwequivalentto1:1andreverseextractionwas isupto96.5%;reverseextractionrateofMg2+is87.2%and cariedout.Themixtureswerevibratedfor30minsrepeat- amassratiomagnesiumtolithiumdeclinedto3.9inthe edlyinatemperature-constantcolingwaterbathSHA-2A 20reserveextractedwaterphase.Intheconcentratedreverse at20°C.andataspedof200r/min.Thesolutionswere extractedsolutionwithalowmagnesiumtolithiumratio, thenplacedstilfor30minsandareverseextractedwater sodiumcarbonatesolutionwasadedtoremovemajorityof phasewasfinalyobtainedafterphaseseparation,witha Mg2+,thensodiumhydroxidewasagainaddedintothe decreasedmagnesiumtolithiumratio.Sampleswereana- solutionafterseparation,tocompletelyprecipitatemagne lyzedandresultsshowedthatreverseextractionrateofLi*25sium.Solutionofsodium carbonatewasaddedintothe wasupto94.7%;reverseextractionrateofMg2+was filteredsolutiontoformprecipitation,andseparationand 92.6%;andamassratiomagnesiumtolithiumdeclinedto desicationwerecariedouttoobtainalithiumcarbonate 10.9inthereserveextractedwaterphase.Intheconcen- product. trated reverse extracted solution with a low magnesium to lithium ratio, sodium carbonate solution was added to 30 Embodiment6 removemajorityofMg2+,thensodium hydroxidewasagain adedintothesolutionafterseparation,tocompletelypre 20mLoftheoldbrineinembodiment1wastakenintoa cipitatemagnesium.Solutionofsodiumcarbonatewas 10mLbeakerandthemassratioofmagnesiumtolithium adedintothefilteredsolutiontoformprecipitation,and inthemixturewasequalto52.58.Thebrinewasheatedfor separation and desicationwerecaried outtoobtain a35condensationaboveatemperatureadjustablefurnace.Water lithium carbonateproduct. Embodiment5 was evaporated,which accounted for25% oftotalmass of thebrine,andthesolutionwerechangedintohydratedhalide saltsaftercooling.Thesaltsweretransferredintoamechani calmixingvesel,and20mL oftributylphosphateaswell 20mLoftheoldbrineinembodiment1wastakenintoa40as20mLofdl-2-octanolwereadedtoachieveamassto 10mLbeakerandthemassratioofmagnesiumtolithium volumeratioequivalentto1:2(g/mL). wasequalto52.58.Thebrinewasheatedforcondensation Solid-liquidextractionwascariedoutfor30minsunder aboveatemperatureadjustablefurnace.Waterwasevapo- roomtemperature.Thensolidliquidmixturesweretrans rated,whichaccountsfor25%oftotalmassofthebrine,and feredinasandcorefunnelandvacuumfiltrationwas thesolutionwerechangedintohydratedhalidesaltsafter45cariedout,and theextractedorganic-phase filtrateand coling.Thesaltswastransferedintoamechanicalmixing remaininghalidesaltswereobtained.Theremaininghalide vessel,and20mLoftributylphosphateaswellas20mLof saltsweredisolvedinwaterandfixitsvolumeto1000ml 2-ethylhexanolwereaddedtoachieveamasstovolume inavolumetricflask.Samplesweretakentoanalyzethe ratioequivalentto1:2(g/mL).Solid-liquidextractionwas concentrationofLitandMg2+thereof.Theresultsshowed cariedoutfor30minsunderroom temperature.Thensolid 50 thataextractionrateofLi*was32.4%;aextractionrateof liquidmixturesweretransferedinasandcorefuneland Mg2+was4.6%andamassratioofmagnesiumtolithium vacuumfiltrationwascariedout,obtainingtheextracted was7.4intheorganicextractedphase. organic-phase filtrate and remaining halide salts. The Theextractedphasesfrom fourstagesweremergedand remaininghalidesaltsweredisolvedinwaterandfixits organicextractionphaseandwaterwererespectivelyadded volumeto1000mL inavolumetricflask.Sampleswere55 inaseparatingfunnelwithaphaseratiooforganicphaseto takentoanalyzetheconcentrationofLitandMg2+thereof. waterVN,equivalentto2:1andreverseextractionwas TheresultsshowedthataextractionrateofLitis50.2%;a cariedout.Themixtureswerevibratedfor30minsrepeat extractionrateofMg2+is4.1%andamassratioofmag- edlyinatemperature-constantcoolingwaterbathSHA-2A nesium tolithium is4.3intheorganicextractedphase. at20°C.andataspeedof200r/min.Thesolutionswthen The extracted phases from four stages aremerged and 60 placed stilfor30minsand areverseextracted water phase organicextractionphaseandwaterwererespectivelyadded wasfinalyobtainedafterphaseseparation,withadecreased inaseparatingfunnelwithaphaseratiooforganicphaseto magnesiumtolithiumratio.Sampleswereanalyzedand waterV V,equivalentto2:1andreverseextractionwas resultsshowedthatreverseextractionrateofLi*wasupto cariedout.Themixtureswerevibratedfor30minsrepeat- 91.6%;reverseextractionrateofMg2+was87.6%;anda edlyinatemperature-constantcoolingwaterbathSHA-2A 65massratiomagnesium tolithium declinedto7.1inthe at20°C.andataspeedof200r/min.Thesolutionswere reserveextractedwaterphase.Intheconcentratedreverse thenplacedstilfor30minsandareverseextractedwater extractedsolutionwithalowmagnesiumtolithiumratio, 10PDF Image | PRODUCING LITHIUM CARBONATE FROM LOW LITHIUM BRINE
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