PDF Publication Title:
Text from PDF Page: 006
5,993,759 78 realizedpreferablyinathickener,anditsunderflow50is Thebrine,withaboronresidueof0.25%andapHof1.8, returnedtothefirstSolid/liquidSeparationSubstage46(or hydrocyclones). InthecasethattheSolid/liquidSeparationStages46and 48arenotaplied,theSolidspresentintheprecipitatedpulp 45ofthereactor43areseparateddirectlyinthesolid/liquid Separator51,whichcanbeabandfilterorcentrifuge,and also washed with demineralized or soft water 52 at 60-98 C. Thestrongfiltrate56oftheliquid/solidseparator,aswell astheeventualpool49ofthesecondoptionalSolid/liquid separation stage 48, contain between 0.1% and 0.3% by weightoflithiumandgenerates,inthisway,amotherliquor 23,whichisutilizedfordilutingthebrine21enteringthe purificationStageofthereactor22withlithium,andalsofor15 washingthemagnesiumcarbonatecake27(or25,inthe casewheretheoptionalthickeningstage26isnotused) which enters into the Separation Stage 28 as indicated previously. Thefiltrate57resultingfromthewashingofthelithium carbonatecakeformedintheSeparator51isusedfor preparingtheSodiumcarbonateSolution24,whichpartici patesinthefirstpurificationStageinthereactor22,aswell asforpreparingthecalciumhydroxideSolution34,which entersintothereactor33,andtheSodiumcarbonateSolution25 44,whichentersintothereactor43,increasinginthisway thegloballithiumrecoveryoftheproces. wastreatedbymeansofSolventextractionutilizinga mixtureof80%byvolumeof2-ethyl-1,3-hexanediol,5%by volumeofisoctylalcohol,and15%byvolumeoftributyl phosphate,disolvedinanaromaticSolvent(Escaid10)in aproportionof20%oftheextractantmixtureand80%of Escaid100. ThebrinewastreatedinfiveeXtractionStageswithan organic/brineratioequalto4/1,acontacttimeof8minutes, andaSetlingtimeof22minutes. Thebrinewithoutboronshowedunderanalysisaboron residueof0.005%byweight.Thechargedorganicextractant wastreatedwithasolutionof0.25molofsodiumhydroxide with an organic/aqueous ratio of 2/1, and in four re-extractionStageswitharetentiontimeof5minutesper Stage,andwasthenallowedtoSetlefor8minutesperStage forSeparatingthephases.Theboron-freeorganicextractant obtained was returned to the extraction Stage, while the alkaline Solution had a boron content of 1.8% in volume. The brineobtained,virtualydevoidofboron,witha contentof5.8%byweightoflithiumand0.07%byweight ofsodiumwasthenmixedwithmotherliquor(obtained duringthefiltrationinthelithiumcarbonateprecipitation Stage).Thebrine/motherliquorratiowas1/5forobtaininga lithiumconcentrationof1.20%byweight.Thedilutedbrine wastreatedwithasolutionof25%byweightofsodium carbonateformaintainingapHof9.5atatemperatureof82 C.duringareactiontimeof90minutes. Thetreatedpulpwasdecantedinathermallyinsulated thickenersoastomaintainthetemperatureabove75C.The densepulpwasfilteredinavacuumfilterandamagnesium carbonatecakewasobtainedwhichwaswashedwithtwo volumesofmotherliquorbeforediscarding.Thefiltrate obtained,togetherwiththeclearliquid,whichrepresentsthe brineinthisfirstpurificationstage,nowcontained0.025% magnesiumandwastreatedinaSecondpurificationStage withaSolutionSaturatedwithcalciumhydroxideformain tainingaconstantpHof10.2at80°C.andforatimespan of30minutes. Theresultingpulpwashotfilteredinapressfilterwith60 lbs.ofpresure.Thecakewaswashedwith2volumesof motherliquorandapurifiedbrinewith0.0008%magnesium and 0.001% calcium was obtained in this manner. Thepurifiedbrinewasfinalytreatedwithasolutionof 25%sodiumcarbonateformaintainingthepHof10.5ata temperatureof90°C.andforareactiontimeof45minutes. Theresultingpulpwashotthickenedat80-85 C.andthe densepulpobtainedwashotfilteredinavacuumfilterat80 C. and the lithium carbonate cake was washed in the filter with demineralized water at 90° C. Thelithiumcarbonatecakewasdriedat200 C.for30 minutesandalithiumcarbonatewasobtainedfinalywhich Thelithiumcarbonatecake60obtainedintheSolid/liquid separationstage51hastypicaly15%to35%humidityand isdriedinaSuitabledryerequipment61,Suchasarotary dryer,usingpreferablyhotairorgasattemperaturesof500 to1000C.,beforeitseventualgranulation,compaction,and packing62.Thelithiumcarbonate63obtainedinthis mannerisofhighpuritywithover99.2%LiCOandles than0.8%ofimpurities. Thepresentaplicationclaimsthebenefitofpriority under35U.S.C.S119fromChileanpatentaplication 484-96,filedMar.28,1996,theentirecontentsofwhichare herebyincorporatedbyreference. 35 Thefollowingisanexampleoftheprocessofthepresent40 invention. EXAMPLE A brine from the Atacama Salt mine, which has been 45 previouslyconcentratedbySolarevaporation,hadthefol lowingcompositionbyweight: Lithium Boron Chlorine Magnesium Sodium Potassium Calcium Sulfate Water(cryst.) 5.9% O.8% 35.8% 1.75% 0.07% O.O2% O.04% O.O2% 54.1% 50 Thisbrinewastreatedwithasolutionofhydrochloricacid of35weight%ofconcentrationformaintainingaconstant valueforthepHof1.8,measuredinabrine/waterdilution of1/10,mixingthesameinastiredtank.Theacidifiedbrine wascooledfor12hoursat10 C.,precipitatinginthisway 71.0% of the boron content as boric acid. The boric acid crystalswerewashedwithdistiledwaterat10 C.Theboric acidobtainedhadapurityof99.2%HBO,withaglobal65 recoveryof68.3%withrespecttotheinitialboroncontained inthebrine. LiCO, 99.2 B O.OOOS Na O.O6 K O.OOOS Mg O.OO6 C O.OO6 Ca O.04 Theinventionbeingthusdescribed,itwilbeobviousthat thesamemaybevariedinmanyways.Suchvariationsare nottoberegardedasadeparturefromtheSpiritandScope ofthe invention, and alSuch modifications as would be showedthefollowingchemicalanalysis(in96byweight): 55 60PDF Image | Patent PRODUCTION OF LITHIUM CARBONATE FROM BRINES
PDF Search Title:
Patent PRODUCTION OF LITHIUM CARBONATE FROM BRINESOriginal File Name Searched:
US5993759.pdfDIY PDF Search: Google It | Yahoo | Bing
Product and Development Focus for Infinity Turbine
ORC Waste Heat Turbine and ORC System Build Plans: All turbine plans are $10,000 each. This allows you to build a system and then consider licensing for production after you have completed and tested a unit.Redox Flow Battery Technology: With the advent of the new USA tax credits for producing and selling batteries ($35/kW) we are focussing on a simple flow battery using shipping containers as the modular electrolyte storage units with tax credits up to $140,000 per system. Our main focus is on the salt battery. This battery can be used for both thermal and electrical storage applications. We call it the Cogeneration Battery or Cogen Battery. One project is converting salt (brine) based water conditioners to simultaneously produce power. In addition, there are many opportunities to extract Lithium from brine (salt lakes, groundwater, and producer water).Salt water or brine are huge sources for lithium. Most of the worlds lithium is acquired from a brine source. It's even in seawater in a low concentration. Brine is also a byproduct of huge powerplants, which can now use that as an electrolyte and a huge flow battery (which allows storage at the source).We welcome any business and equipment inquiries, as well as licensing our turbines for manufacturing.CONTACT TEL: 608-238-6001 Email: greg@infinityturbine.com (Standard Web Page)