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US 10,695,694B2 31 32 from about8pm toabout10ppm.When lithium ionsare TheLiMn3012 ionexchangematerialwas synthesized elutedfromthecoatedionexchangeparticlesusinganacid usingasolid-statemethodfromelectrolyticmanganese solution,somesmalamountofthecoatingmaterialare dioxideandlithiumnitrateprecursors.Theprecursorswere disolved.Thesedisolvedelementswilbereleasedwith bal-miledusing5mmZrO2grindingmediafor30minutes thelithium.Insomeembodiments,thelithiumispurified,5 inaplanetarybalmil.Theresultingmixturewasfiredina butsomeverysmalconcentrationofelementsfromthe furnacewithaheatingrateof5°C./minupto50°C.for36 coatingmaterialremainwithinthelithiumproductasan hoursandthencoledslowlytoromtemperature.The impurity.Insomeembodimentsthisimpurityconcentration resultingpowderwascomprisedofLiMn3012ion isontheorderofparts-per-bilion,andisdetectedusing exchangematerial.AZrO2coatingwasdepositedonthe Inductively Coupled Plasma-Atomic Emision Spectros-10 LiMn 012ionexchangematerial.Theionexchangemate copy(ICP-AES)orInductivelyCoupledPlasma-MassSpec rialwassuspendedinamixtureofbutanol,ethanol,and trometry(ICP-MS).Inoneembodiment,ICP-AESisusedto waterwithvigorousstiring,andamixtureofbutanoland measureimpurityconcentrationsofZrionsorTiionsfrom zirconiumbutoxidewasdripedintothesuspensionoverthe ZrO2orTiO2coatingsatwavelengthsof343.823nmor courseof30minutes.Thesuspensionwasstiredfor2hours 336.121nm. 15 toalowthezirconium butoxidetoreactwiththewaterand Insomeembodiments,theconcentratedlithiumionsolu formaZrO2precursorontheparticlesurfaces.Thecoated tionisfurtherprocesedintolithiumrawmaterialsusing powderwasthenfiredinafurnaceat40°C.for2hours. methodssuchassolventextraction,ionexchange,chemical Theresultingpowderwascoatedionexchangeparticles substitution,chemicalprecipitation,electrodialysis,elec comprisedofLi,Mn,012particleswithZro,coatings.The trowining,evaporation,heattreatment,orcombinations20particleswerecomprisedof98wt.%ionexchangematerial thereof.Insomeembodiments,theconcentratedlithiumion (Li_Mn3012)and2wt.%ofthecoating(ZrO2).The solutionisfurtherprocesedintolithiumchemicalssuchas particleshadameandiameterof1micron,andthecoating lithiumchloride,lithiumcarbonate,lithiumhydroxide, thickneswasaproximately2nm. lithium phosphate, lithium metal, lithium metal oxide, lithiummetalphosphate,lithiumsulfide,orcombinations25 Example3–SynthesisofCoatedIonExchange thereof. Insomeembodiments,thelithium chemicalsproducedis usedinanindustrialaplicationsuchaslithiumbateries, Thecoatedionexchangeparticleswerecomprisedofan metalaloys,glas,grease,orcombinationsthereof.Insome ionexchangematerialandacoatingmaterial.Theion embodiments,thelithiumchemicalsproducedareusedinan30exchangematerialwasLizTiO3andthecoatingmaterialwas aplicationsuchaslithiumbateries,lithium-ionbateries, SiO2.Theparticleswerecreatedbyfirstsynthesizing lithiumsulfurbateries,lithiumsolid-statebateries,and LiTiO3andthendepositingtheSiO2coatingonthesurface combinationsthereof. Particles(LiMnO,/ZrO2) resultingmixturewasfiredinafurnacewithaheatingrate of5°C./minupto70°C.for24hoursandthencoled Thecoatedionexchangeparticlesarecomprisedofanion40slowlytorom temperature.Theresultingpowderwas exchangematerialandacoatingmaterial.Theionexchange comprisedofLiTiOzionexchangematerial.ASiO2coating materialisLiMn3012andthecoatingmaterialisZrO2.The wasdepositedontheLiTiOzionexchangematerial.Theion particlesarecreatedbyfirstsynthesizingLi_Mn012and exchangematerialwassuspendedinamixtureofethanol thendepositingthecoatingonthesurfaceoftheLiMn012 andwaterwithvigorousstiring,andamixtureoftetraethyl The ion exchange material,LiMn2012 issynthesized 45 orthosilicate (TEOS),water,and hydrochloric acid was usinghydrothermalsynthesis,solidstatesynthesis,micro dripedintothesuspensionoverthecourseof120minutes. wavesynthesisorcombinationsthereof.Thecoatingmate Thesuspensionwasstiredfor2hourstoalowtheTEOSto rial(ZrO2)isdepositedonthesurfaceoftheLiMn012 depositontheparticlesurfaces,andthesolventwasevapo usingchemicalvapordeposition,hydrothermaldeposition, rated.Thecoatedpowderwasthenfiredinafurnaceat40° solvothermal deposition, sol-gel deposition, precipitation, 50 C. for 2 hours. The resulting powder was coated ion microwavedepositionorbysuspendingLi,Mn0.2ina exchangeparticlescomprisedofLi,TiO3particleswithSiO2 solventandthenadingreagentsincludingmetalchloride, coatings.Theparticleswerecomprisedof96wt.%ion metaloxychloride,metalalkoxide,water,acid,base,or exchangematerialand4wt%ofthecoating.Theparticles combinationsthereof.Theparticlescompriseof98wt.% hadameandiameterof4microns,andthecoatingthicknes ionexchangematerial(LiMn3012)and2wt.%ofthe5wasaproximately35nm. coating(ZrO2).Theparticleshaveamean diameterof1 microns,andthecoatingthicknesisaproximately2nm. Example4—UseofCoatedIonExchangeParticles EXAMPLES 35 method from titanium dioxide and lithium carbonate pre cursors.Theprecursorswerebal-miledusing5mm ZrO2 Example1-SynthesisofCoatedIonExchange grindingmediafor30minutesinaplanetarybalmil.The Example2 SynthesisofCoatedIonExchange (Li4Mn012/ZrO2) Particles(LiMn30,2/ZrO2) 60 Lithium is extracted from abrine using coated ion exchangeparticles(LiMn,012/ZrO2).Thebrineisanaque Thecoatedionexchangeparticleswerecomprisedofan oussolutioncontaining50,0pmNaand1,0pmLi. ionexchangematerialandacoatingmaterial.Theion ThecoatedionexchangeparticlesaretreatedwithHClacid exchangematerialwasLiMng012andthecoatingmaterial toyieldLiClinsolution.Duringacidtreatment,thecoated wasZrO2.Theparticleswerecreatedbyfirstsynthesizing65ionexchangeparticlesabsorbhydrogenionswhilereleasing LiMn,012andthendepositingthecoatingonthesurfaceof lithiumions.TheLi_Mn012activematerialisconvertedto theLiMn3012 Particles(Li,Ti0z/SiO2) oftheLiTiO3. TheLiTiO3powderwassynthesizedusingasolid-state aprotonatedstate.TheZrO2coatingalowsdifusionofPDF Image | Patent Lithium Extraction with coated ion exchange particles
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