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(12) Patent Application Publication (10) Pub. No.: US 2008/0233042 A1 Boryta Et Al

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(12) Patent Application Publication (10) Pub. No.: US 2008/0233042 A1 Boryta Et Al US 20080233042A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2008/0233042 A1 Boryta et al. (43) Pub. Date: Sep. 25, 2008 (54) PRODUCTION OF LITHIUM COMPOUNDS 11/332,134, filed on Jan. 13, 2006, now Pat. No. 7,214, DIRECTLY FROM LITHIUM CONTAINING 355, which is a division of application No. 10/395,984, BRINES filed on Mar. 25, 2003, now Pat. No. 7,157,065, which is a continuation-in-part of application No. 09/707, (76) Inventors: Daniel Alfred Boryta, Cherryville, 427, filed on Nov. 7, 2000, now Pat. No. 6,936,229, NC (US); Teresita Frianeza which is a division of application No. 09/353,185, filed Kullberg, Gastonia, NC (US); on Jul. 14, 1999, now Pat. No. 6,207,126. Anthony Michael Thurston, Edmond, OK (US) Publication Classification Correspondence Address: (51) Int. C. FULBRIGHT & JAWORSKI, LLP C22B 26/10 (2006.01) 666 FIFTHAVE NEW YORK, NY 10103-3198 (US) (52) U.S. Cl. ..................................................... 423/499.3 (21) Appl. No.: 12/114,054 (57) ABSTRACT (22) Filed: May 2, 2008 Methods and apparatus for the production of low sodium lithium carbonate and lithium chloride from a brine concen Related U.S. Application Data trated to about 6.0 wt % lithium are disclosed. Methods and (60) Continuation of application No. 1 1/706027, filed on apparatus for direct recovery of technical grade lithium chlo Feb. 14, 2007, which is a division of application No. ride from the concentrated brine are also disclosed. Patent Application Publication Sep. 25, 2008 Sheet 1 of 7 US 2008/0233042 A1 LITHIUM CARBONATE PROCESSFLOW DIAGRAM (A) 2 CD SOLID SODAASH 4 3 Mg MUD \ SAS 6 FROM C5 5 REACTOR LIQUOR MOTHER LIOUOR WASH FILTER (10) BRINE + WASHFILTRATE 0.5 - 1.2% Li 2ND STAGE 12 REACTOR FILTER Li2CO3 REACTOR 18 FILTER MOTHER LIQUOR (19) WASH WATER FLTRATE PROCESS BLEED WET LITHIUM CARBONATE9 21 DRYER WET Li2CO3 22 TO B1 TECH GRADE Li2CO3 FIG. 1 Patent Application Publication Sep. 25, 2008 Sheet 2 of 7 US 2008/0233042 A1 LOWSODIUM LITHIUM CARBONATE PROCESS FLOW DIAGRAM (B) WET Li2CO3 3 FROMA20 1 LITHIUM 2 BICARBONATE Li2CO3 SPARGER SLURRY TANK 12 REACTOR & SETTLER O CO2 MAKE-UP are - or - - - - 10 as s > sea eme me mo m sm me Li2CO3 1MOTHER CORECYCLE ()- PRECIPITATION LIQBLEED TO TANK A15 7 MOTHER RS FILTER QUOR O RECYCLE 9 8 MAX SACK Li2CO3 PACKAGENG TO C18 FIG. 2 Patent Application Publication Sep. 25, 2008 Sheet 3 of 7 US 2008/0233042 A1 DIRECT LITHIUM CHLORIDE PROCESS FLOW DIAGRAM (C) 3 LIME FEED LIMING ANK RAFFINATE FEED 6 FILTRATE TANK FILTER TO A4 - COOLNG FIRST STAGE REACTOR Li2CO3 PLANT 9 11 FILTER NaCl SOLIDS WATER 10 18 HCI BaCl2 FROMB8 LiOH H2O PURIFICATION LOWSODUM Li2C2O4. 12 FILTER 13 pH ADJUSTMENT 16 14 OPTIONAL LiCl CRYSTALLIZER/ WASH CENTRFUGE 15 17 TECH & LOW Na DRYER LiC PRODUCT FIG. 3 Patent Application Publication Sep. 25, 2008 Sheet 4 of 7 US 2008/0233042 A1 CO2 MAKE UP MIXER COOL ML WET Li2CO3 CO2 CRYSTAL RECYCLE HEAT EXCHANGER COOL 2b LiHCO SOLUTIONY, MIXER PRE HEATED SETTER 1E COOL T LIHCO3 24 eas O-35°C. ? SOLUTION HEAT 70-95C VEV HOT DEONIZED HoO 95C 2 MLBLEED FOR Na WETLi2CO3 WASHFILTRATE TO DRYER TO #1 + 2 Li2CO3 PLANT BELT FILTER WASH HIGH PURITY Li2CO3 < 9ppm Na FIG. 4 Patent Application Publication Sep. 25, 2008 Sheets of 7 US 2008/0233042 A1 LOWSODIUM Li2CO3 LCOFINES + WATER OR WET CAKE SLURRY 4.5% SOLIDS CO2 ABSORPTON COLUMN MOTHER LOUOR RECYCLE LiHCO3 SOLUTION DEONZED WASH WATER Li2CO3 > FILTRATION - WET CAKE MOTHER (>8PPM NaON LOUOR DRY BASIS) BLEED TOL2CO3 PLANT BELT FILTER WASHFLTRATE FIG. 5 Patent Application Publication Sep. 25, 2008 Sheet 6 of 7 US 2008/0233042 A1 Li2CO3/COREACTION PILOT PLANT WITH SEVE TRAY COLUMN 7 5 CO2 C TO Y VENT LiCO-WATER SLURRY MESH 2VV3 DXNY 2 e 4. 4' t E-Yo T3 3"DIA. COLUMN WITH (24) CARTRIDGE SEVE TRAYS - N - 4' T1 om H T2 ()K ... T Y t X FIG 6 LiHCO3 v W SOLUTION CO2 Patent Application Publication Sep. 25, 2008 Sheet 7 of 7 US 2008/0233042 A1 LicO/CO REACTION PILOT PLANT WITH SCHEIBELCOLUMN t LCO-WATER SLURRY STAGEs X --- T3 3" DA, SCHEBEL COLUMN X T1 /N om DKN1 (OX L?. r Ear V T2 X Cto. T LiHCO3 SOLUTION CO2 FIG. 7 US 2008/0233042 A1 Sep. 25, 2008 PRODUCTION OF LITHIUM COMPOUNDS 0006 Production of lithium carbonate and lithium chlo DIRECTLY FROM LITHIUM CONTAINING ride with acceptable qualities from Such brines requires BRINES employing techniques to remove specific cations and anions that accompany the lithium in Solution, and then concentrat ing the lithium for extraction. 0001. This application is a continuation-in-part of U.S. 0007 Individual applications require that these ion impu Ser. No. 09/707,427 filed Nov. 7, 2000, which is a divisional rities be reduced to specific maximum levels and a number of application of U.S. Ser. No. 09/353,185, now U.S. Pat. No. processes have been described for removing these impurities. 6,207,126. For example, U.S. Pat. No. 5.219,550 to Brown and Boryta 0002 This application claims priority under 35 U.S.C S describes a method for producing chemical grade lithium 19(e) from U.S. Provisional Application Nos. 60/100,340 carbonate from natural lithium containing brine by first filed Sep. 14, 1998 and 60/093,024 filed Jul. 16, 1998. removing most of the components from the brine by concen trating utilizing Solar evaporation techniques. Concentrating BACKGROUND AND SUMMARY OF THE the brine with respect to lithium by solar evaporation causes INVENTION most of the unwanted components to precipitate from the 0003. The present invention relates to an integral process brine, i.e., salt out. Boron, which concentrates with the that uses a minimum number of process steps for producing lithium, is Subsequently removed using an extraction process. chemical and high purity grades of lithium carbonate and The remaining magnesium is removed by adding a base to lithium chloride directly from the same natural brine source. precipitate magnesium carbonate and/or magnesium hydrox More generally, the method also relates to a method of pro ide, and the lithium is finally precipitated from the purified ducing purified metal carbonate salts that are generally brine as lithium carbonate by the addition of soda ash. Other insoluble in water but which have corresponding bicarbonate processes related to the above process are disclosed in U.S. salts that are more then 75% soluble in water by reaction with Pat. Nos. 4,036,718; 4,243,392; and 4,261,960. carbon dioxide. 0008. Other techniques for producing purified lithium 0004. It is desirable, from a commercial standpoint, to salts are known. For example, German Patent DE 19,541,558 provide a source of lithium low in Sodium content because to Wusson et al describes a process to reduce sodium from Sodium becomes reactive and potentially explosive in certain lithium chloride solutions by cooling. U.S. Pat. No. 4,859,343 chemical processes, particularly those in production of to Kullberg etal describes anion exchange method for remov lithium metal from lithium salts. A substantial portion of ing sodium from brines. U.S. Pat. No. 5.599,516 and Russian presently available lithium is recovered from brines, which Patent No. 9,419.280 describe absorption/ion exchange pro also contain high levels of sodium, making the production of cesses for recovering lithium from brine. low sodium lithium salts difficult and expensive. At the 0009 U.S. Pat. No. 4,980,136 discloses a procedure for present time, there does not exist a viable low cost integral preparing chemical grade and low Sodium lithium chloride processes for producing low sodium lithium carbonate and (battery grade, less than 20 ppm Sodium and less than 5 ppm chemical and high purity grades of lithium chloride directly magnesium) from concentrated natural brine by crystallizing from natural brines containing lithium. lithium chloride from a magnesium/lithium chloride brine to 0005 Natural brines that contain lithium also contain produce a chemical grade of lithium chloride crystal. This is many constituents as illustrated in the following Table: followed by alcoholic extraction of the soluble lithium chlo TABLE 1. NATURAL BRINE COMPOSITION Great Salton Silver Dead Salt Bonneville Sea Peak Salar de Atacama Sea Lake Brine Brine Brine Brines Ocean Israel Utah Utah Calif Nevada Chile Na 1.OS 3.0 7.0 9.4 5.71 6.2 7.17 5.70 K O.O38 O6 0.4 O.6 1.42 O.8 1.85 1.71 Mg O.123 4.0 O.8 0.4 O.O28 O.O2 O.96 1.37 Li O.OOO1 O.OO2 O.OO6 O.007 O.O22 O.O2 O.15 O.193 Ca O.04 O.OS 1.5 O.S O.O O.71 1.46 O.043 C 1.9 16.0 14.O 16.O 15.06 10.06 16.04 17.07 Br O.OO65 0.4 O.O O.O O.O O.OO2 O.OOS O.OOS B O.OOO4 O.OO3 O.007 O.007 O.O39 O.OOS O.04 O.04 Li/Mg O.OOO8 O.OOOS O.OO75 O.O175 O.786 1.O O.156 O.141 LiK O.OO26 O.OO33 0.015 O.0049 O.O155 O.O16 O.O81 O.113 LifCa O.OO2S O.OO64 O.2 O.OS83 O.OOO8 1.0 4.84 O.244 Li B O.25 O.6666 0.857 1.O O.OS1 4.0 3.75 4.83 (All values in weight percent) US 2008/0233042 A1 Sep.
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