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(12) United States Patent (10) Patent No.: US 7.449,161 B2 Boryta Et Al

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(12) United States Patent (10) Patent No.: US 7.449,161 B2 Boryta Et Al USOO74491.61B2 (12) United States Patent (10) Patent No.: US 7.449,161 B2 Boryta et al. (45) Date of Patent: Nov. 11, 2008 (54) PRODUCTION OF LITHIUM COMPOUNDS 4,207,297 A * 6/1980 Brown et al. ............. 423,179.5 DIRECTLY FROM LITHIUM CONTAINING 4,243,641 A * 1/1981 Ishimori et al. .......... 423/179.5 BRINES 4.261,960 A * 4/1981 Boryta ............. ... 423,179.5 4,271,131. A * 6/1981 Brown et al. ...... ... 423,179.5 4,274,834. A 6/1981 Brown et al. .............. 23,302 R (75) Inventors: Daniel Alfred Boryta, Cherryville, NC 4,463,209 A * 7/1984 Kursewicz et al. .......... 585/467 (US); Teresita Frianeza Kullberg, 4,465,659 A * 8/1984 Cambridge et al. ......... 423,495 Gastonia, NC (US); Anthony Michael 4,588,565 A * 5/1986 Schultze et al. .......... 423,179.5 Thurston, Edmond, OK (US) 4,747.917 A * 5/1988 Reynolds et al. ............ 205,512 4,859,343 A * 8/1989 Frianeza-Kullberg (73) Assignee: Chemetall Foote Corporation, Kings et al. .......................... 210,679 Mountain, NC (US) 4,980,136 A * 12/1990 Brown et al. ... 423,179.5 5,049,233 A 9, 1991 Davis .......................... 216.93 (*) Notice: Subject to any disclaimer, the term of this 5,219,550 A * 6/1993 Brown et al. ............. 423 (419.1 patent is extended or adjusted under 35 5,599,516 A * 2/1997 Bauman et al. .......... 423/179.5 U.S.C. 154(b) by 0 days. 5,939,038 A * 8/1999 Wilkomirsky ............... 423,276 5.993,759 A * 1 1/1999 Wilkomirsky ............ 423,179.5 6,048,507 A * 4/2000 AmouZegar et al. ...... 423,179.5 (21) Appl. No.: 11/706,027 6,143.260 A * 1 1/2000 Boryta .................... 423,179.5 6,207,126 B1* 3/2001 Boryta et al. ..... ... 423,499.3 (22) Filed: Feb. 14, 2007 6,497.850 B1* 12/2002 Boryta et al. ..... ... 423,179.5 6,592,832 B1* 7/2003 Friedrich et al. ......... 423/179.5 (65) Prior Publication Data 6,921,522 B2 * 7/2005 Boryta et al. ..... ... 423,499.3 US 2007/O 148077 A1 Jun. 28, 2007 6,936.229 B1* 8/2005 Boryta et al. ............... 422,187 7,157,065 B2 * 1/2007 Boryta et al. ............... 423 (421 7,214,355 B2 * 5/2007 Boryta et al. ..... ... 423,179.5 Related U.S. Application Data 2001/0028871 A1* 10, 2001 Harrison et al. ............. 423 (421 (60) Division of application No. 1 1/332,134, filed on Jan. 13, 2006, now Pat. No. 7,214,355, which is a division FOREIGN PATENT DOCUMENTS of application No. 10/395.984, filed on Mar. 25, 2003, CL 550-95 * 7/1998 now Pat. No. 7,157,065, which is a continuation-in DE 257 245 * 6, 1988 part of application No. 09/707.427, filed on Nov. 7, DE 1954.1 558 A1 * 5, 1997 2000, now Pat. No. 6,936,229, which is a division of WO WO94, 1928O A1 * 9, 1994 application No. 09/353,185, filed on Jul. 14, 1999, now WO WO99,29624 A1 * 6, 1999 Pat. No. 6,207,126. OTHER PUBLICATIONS (60) Provisional application No. 60/100,340, filed on Sep. The English abstract of the article titled “Production of high-purity 14, 1998, provisional application No. 60/093,024, silicon for semiconductors. I. Production of boron free silicon rods filed on Jul. 16, 1998. from silicon tetrachloride and lithium aluminum hydride.” by P. Roman et al., Revistade Chimie (Bucharest, Romania), 11, pp. 464 (51) Int. Cl. 468, (1960), ISSN: 0034-7752.* COLD I5/04 (2006.01) (52) U.S. Cl. ..................... 423/1795; 423/197; 423/202 * cited by examiner (58) Field of Classification Search .............. 423/179.5, Primary Examiner Timothy CVanoy 423/197,202 (74) Attorney, Agent, or Firm Fulbright & Jaworski L.L.P. See application file for complete search history. (57) ABSTRACT (56) References Cited U.S. PATENT DOCUMENTS Methods and apparatus for the production of low sodium lithium carbonate and lithium chloride from a brine concen 2,516,109 A * 7/1950 Ellestad et al. .............. 423, 193 trated to about 6.0 wt % lithium are disclosed. Methods and 2,793.934. A * 5/1957 Cunningham ... ... 423,179.5 apparatus for direct recovery of technical grade lithium chlo 3,112,171 A * 1 1/1963 Archambault...... ... 423,179.5 ride from the concentrated brine are also disclosed. 3,857,920 A * 12/1974 Grantham et al. ........ 423/179.5 4,036,718 A * 7/1977 Brown et al. ................ 522,156 4,124,684. A * 1 1/1978 Olivier et al. ............ 423,179.5 1 Claim, 7 Drawing Sheets U.S. Patent Nov. 11, 2008 Sheet 1 of 7 US 7.449,161 B2 LITHIUM CARBONATE PROCESS FLOW DIAGRAM (A) 2 CD SOLID SODAASH 4 3 Mg MUD SAS 6% RAFFINATE 6 FROM C5 5 1ST STAGE MOTHER REACTOR QUOR MOTHER LOUOR WASH (10) BRENE + WASHFLTRATE 0.5 - 1.2% Li 2ND STAGE 12 REACTOR Mg(OH)2 & CaCO3 MUD (7) MOTHER LOUOR (19) WASH WATER FLTRATE PROCESS BLEED WET LITHIUM CARBONATE9 21 DRYER WET Li2CO3 22 TO B1 TECH GRADE Li2CO3 FIG. 1 U.S. Patent Nov. 11, 2008 Sheet 2 of 7 US 7.449,161 B2 LOWSODIUMLITHIUM CARBONATE PROCESS FLOW DIAGRAM (B) WET Li2CO3 3 FROM A20 1 LITHIUM 2 BICARBONATE Li2CO3 SPARGER T SLURRY TANK 12 REACTOR & SETTLER O CO2 MAKE-UP is is is . 10 Li2CO3 MOTHER CO2 RECYCLE (1) PRECIPITATION QBLEED TO TANK A15 7 MOTHER RECYCLE MAXISACK PACKAGING FIG. 2 U.S. Patent Nov. 11, 2008 Sheet 3 of 7 US 7.449,161 B2 DIRECT LITHIUM CHLORIDE PROCESS FLOW DIAGRAM (C) 1 3 RAFFINATE LME FEED LMING TANK FEED 6 4 FLTRATE Ca/Mg MUDS TANK FILTER TANK TO A4 COOLNG FIRST STAGE REACTOR Li 2CO3 PLANT 9 11 FILTER NaCl SOLDS WATER 10 18 HCI BaCl2 FROM B8 LiOH H2O PURIFICATION LOWSODIUM Li2C2O4 12 i2CO3 + HC FILTER 13 pHADJUSTMENT 16 14 OPTIONAL LiC CRYSTALLIZERI WASH CENTRFUGE 15 17 TECH & LOW Na DRYER LiC PRODUCT FIG. 3 U.S. Patent Nov. 11, 2008 Sheet 4 of 7 US 7.449,161 B2 CO2 MAKE UP WET Li2CO3 CO2 CRYSTAL RECYCLE HEAT EXCHANGER 2b LiHCO SOLUTION MIXER PRE HEATED COO T LIHCO3 0-35°C ( SOLUTION HEAT 70-95C wit/ HOT DEONIZED HoO 95°C 2 MLBLEED FOR Na WET Li2CO3 WASHFILTRATE TODRYER TO #1 + #2 Li2CO3 PLANT BEL FILTER WASH HIGH PURITY Li2CO3 < 9ppm Na FIG. 4 U.S. Patent Nov. 11, 2008 Sheet 5 Of 7 US 7.449,161 B2 LOWSODIUM Li2CO3 Li2COFINES + WATER OR WET CAKE SLURRY 4.5% SODS l CO2 ABSORPTION COLUMN MOTHER LQUOR RECYCLE LiHCO3 SOLUTION DEONZED WASH WATER l Li2CO3 E-> FILTRATION -->WET CAKE MOTHER (>8PPM Na ON QUOR DRY BASIS) BLEED TOL2CO3 PLANT BEL FILTER WASHFLTRATE FIG. 5 U.S. Patent Nov. 11, 2008 Sheet 6 of 7 US 7.449,161 B2 Li2CO3/CO2REACTION PILOT PLANT WITH SIEVE TRAY COLUMN 75 CO2 TO - AC VENT LiCO-WATER SLURRY MESH DX T3 C T4 4' s T3 3"DIA. COLUMN WITH (24) CARTRIDGE SEVE TRAYS — 4' T1 om H T2 (2)|X o 1. TL a . X FIG 6 LiHCO3 SOLUTION CO2 U.S. Patent Nov. 11, 2008 Sheet 7 Of 7 US 7.449,161 B2 LicO/CO REACTION PILOT PLANT WITH SCHEIBELCOLUMN Y N. CO2 O O STAGES99 HE VENT LCO-WATER SLURRY T X T4 STAGEs X --- T3 3" D.A. SCHEBEL COLUMN X T1 /N om DKN1 GO X l?. T E M T2 SX Ctw. LiHCO3 SOLUTION CO2 FIG. 7 US 7,449,161 B2 1. 2 PRODUCTION OF LITHIUM COMPOUNDS Individual applications require that these ion impurities be DIRECTLY FROM LITHIUM CONTAINING reduced to specific maximum levels and a number of pro BRINES cesses have been described for removing these impurities. For example, U.S. Pat. No. 5.219,550 to Brown and Boryta This application is a divisional application of U.S. Ser. No. 5 describes a method for producing chemical grade lithium 1 1/332,134 filed Jan. 13, 2006, now U.S. Pat. No. 7,214,355, carbonate from natural lithium containing brine by first which is a divisional application of U.S. Ser. No. 10/395,984 removing most of the components from the brine by concen filed Mar. 25, 2003, now U.S. Pat. No. 7,157,065, which is a trating utilizing Solar evaporation techniques. Concentrating continuation-in-part of U.S. Ser. No. 09/707.427 filed Nov. 7, the brine with respect to lithium by solar evaporation causes 2000, now U.S. Pat. No. 6,936,229. which is a divisional 10 most of the unwanted components to precipitate from the application of U.S. Ser. No. 09/353,135 filed Jul. 14, 1999, brine, i.e., salt out. Boron, which concentrates with the now U.S. Pat. No. 6,207,126. lithium, is Subsequently removed using an extraction process. This application claims priority under 35 U.S.C. S 119(e) from U.S. Provisional Application Nos. 60/100,340 filed Sep. The remaining magnesium is removed by adding a base to 14, 1998 and 60/093,024 filed Jul 16, 1998. precipitate magnesium carbonate and/or magnesium hydrox 15 ide, and the lithium is finally precipitated from the purified BACKGROUND AND SUMMARY OF THE brine as lithium carbonate by the addition of soda ash. Other INVENTION processes related to the above process are disclosed in U.S. Pat. Nos. 4,036,718; 4,243,392; and 4,261,960.
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