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United States Patent (19) (11) Patent Number: 4,980,136 Brown Et Al

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United States Patent (19) (11) Patent Number: 4,980,136 Brown Et Al United States Patent (19) (11) Patent Number: 4,980,136 Brown et al. 45) Date of Patent: Dec. 25, 1990 54 PRODUCTION OF LITHIUM METAL GRADE LITHUM CHILORIDE FROM OTHER PUBLICATIONS LITHIUMCONTAINING BRINE D. S. Arnold-"Process Control in Boric Acid Extrac tion', 12-5-66. D. S. Arnold 'A New Process for the Production of 75 Inventors: Patrick M. Brown, Exton; Susan J. Boric Acid', 10-23-64. Beckerman, Phoenixville, both of Pa. C. R. Havighorst "AP & CC New Process Separates Borates From Ore by Extraction', 1 1-11-63. 73 Assignee: Cyprus Foote Mineral Company, R. R. Grinstead "Removal of Boron and Calcium from Malvern, Pa. Magnesium Chloride Brines by Solvent Extraction', 11-4-72; Indus. Eng. Chem. Dev., vol. 11, No. 4, 1972 21 Appi. No.: 380,089 pgs. 454-460. N. C. Nelson and J. E. Hudgens “Liquid-Liquid Ex traction of Boric Acid Using Aliphatic Alcohols'- (22 Filed: Jul. 14, 1989 -Quarterly Progress Report for Period ending Mar. 31, 1953, New Brunswick Lab., pp. 24-32-34. 51 Int. Cl....................... B01D 11/04: CO1D 15/04 W. F. Linke "Solubilities Inorganic & Metal-Organic 52 U.S. C. .................................. 423/1795; 423/181 Compounds', American Chemical Society, Washing 58 Field of Search ............ 423/179.5, 181, DIG. 14; ton, DC-1965, pp. 394–395. 210/634 Kozerchuk et al. "Extracting Boron. From Magnesium Chloride Brines', 1981. 56 References Cited Kristanova et al. "Extraction of Boronfrom Bulgarian Natural Brines with Two-Ethylhexanol'-1984. U.S. PATENT DOCUMENTS Petrov et al. “Removal of Boron from Magnesium 2,969,275 l/1961 Garrett ................................ 423/283 Chloride Solutions by Liquid Extraction'-1977. 3,111,383 11/1963 Garrett ................................ 423/283 Smirnov et al. "Development of Technology for Ex 3,268,289 1/1981 Macey ....... ... 42.3/79.5 tracting Boron from Hydro Minerals'-1982. 3,278,260 10/1966 Hermann .. ... 423/179.5 Sologubenko et al. “Study of the Extraction Purifica 3,297,737 1/1967 Weck ... ... 423/179.5 tion of Magnesium Chloride Solutions by Removing 3,336,115 8/1967 Reburn .................................. 23/296 Boron'-1980. 3,370,093 2/1968 Longoria III ....................... 558/290 3,410,653 1 1/1968 Theodore ............................ 423/8. Primary Examiner-Jeffrey E. Russel 3,479,294 11/1969 Weck .................................. 252/180 Assistant Examiner-Brian M. Bolam 3,789,059 1/1974 Cuevas ...... ... 423/179.5 3,855,392 12/1974 Folkestad ............................ 423/497 Attorney, Agent, or Firm-Howson and Howson 4,243,392 l/1981 Brown et al. ...................... 23/295 S 57 ABSTRACT 4,261,960 4/1981 Boryta...... ... 423/179.5 4,261,961 4/1981 Davis .................................. 423/18 The present invention relates to a novel process for 4,271,131 6/1981 Brown. ... 423/179.5 producing, from a lithium-containing brine, a substan 4,274,834 6/1981 Brown ...... 23/302. R. tially pure lithium chloride product. This product is 4,324,771 4/1982 Barlow et al. .... 423/283 particularly useful for the production of lithium metal by electrolysis. FOREIGN PATENT DOCUMENTS 115415 12/1963 Fed. Rep. of Germany . 21 Claims, No Drawings 4,980, 136 1. 2 lithium ratio, generally about 1:1 to 6:1, which allow PRODUCTION OF LITHIUM METAL GRADE for concentrating, purifying and recovering lithium LITHIUM CHILORIDE FROM chloride brine While these brines are viable reserves for LTHUM-CONTAINING BRINE lithium recovery, they also contain varying amounts of 5 alkali and alkaline earth metal impurities, such as, mag The present invention relates to a novel process for nesium, calcium, sodium, sulfate, boron, and other com producing, from lithium-containing brine, substantially ponents. Some typical components of naturally occur pure lithium chloride, which may be used in the produc ring brines are identified in the Table below entitled tion of lithium metal. "Saline Brine Analyses'. TABLE SALINE BRINE ANALYSES Weight Percent Great Geothermal Silver Atacama Dead Sea Salt Lake Bonneville Salton Sea Peak Brine Ocean Israel Utah Utah California Nevada Chile Na .05 3.0 7.0 9.4 5.7 6.2 7.17 K 0.038 0.6 0.4 0.6 .42 0.8 1.85 Mg 0.123 4.0 0.8 0.4 0.028 0.02 0.96 Li OOOO 0.002 0.006 0.007 0.022 0.02 0.5 Ca 0.040 O.3 O.03 0.12 2.62 0.02 0.03 SO4 0.25 O.OS 1.5 0.5 O,OO 0.71 .46 C 1900 16.0 14.0 16.0 15.06 10.06 16.04 Br 0.0065 0.4 O.O 0.0 0.0 0.002 0.005 B 0.0004 0.003 0.007 0.007 0.039 0.005 0.04 Li/Mg 1/12720 A2000 1/35 1/60 1A1.3 1/1 1/6 Li/K 1/3800 A300 1/70 1/90 1/71 1A20 1/12 Li/Ca MA-00 A50 1/5 1/17 1/119 Al 1/0.2 Li/B A. 1/1.5 1/1.2 A1 1A1.8 AO.25 1/0.27 BACKGROUND OF THE INVENTION These metal ion contaminants in lithium containing natural brines, should be substantially eliminated or Lithium metal has a variety of industrial uses, includ- 30 minimized to produce a lithium chloride product suit ing applications for aluminum-lithium alloys. Addi able for production by electrolysis of an uncontam tional uses of this metal include lightweight, compact inated lithium metal. During electrolysis of lithium primary and secondary lithium batteries, compact lithi chloride to produce lithium metal, contaminating metal um/sulfur batteries for electric cars and power plant ions report to the lithium metal due to the high elec load leveling products Lithium metal is also employed 35 trode potential required for reduction of lithium. Also as a degasifier in the production of high-conductivity any contaminating anion in the lithium chloride which copper and bronze and in the synthesis of organometal is not oxidized at the anode to form a volatile species lic compounds for applications in the fields of rubber, will build up in the electrolyte and eventually cause plastics and medicines. substantial losses in current efficiency. For example, Lithium metal is generally produced by electrolysis estimates have been made that concentrations in excess of an eutectic mixture of highly pure molten lithium of about 100 ppm of borate ion or about 25 ppm of chloride and potassium chloride. The lithium chloride boron present in the lithium chloride produced via brine for metal applications has been conventionally pro production technology are not satisfactory for long duced according to several methods. In one method term electrolytic cell operation. lithium chloride is produced by directly reacting hydro 45 Simple technical means for the removal of all of these chloric acid with lithium carbonate produced from contaminants from the ultimately produced lithium spodumene as its genesis. However, lithium chloride metal or from the lithium chloride brines are currently produced in this manner contains substantial contami not cost effective. As presently practiced in the indus nants which are not suitable for many of the present try, boron is removed from, or substantially reduced in, applications of lithium metal. 50 lithium chloride brine on a commercial basis by first To obtain highly purified lithium chloride suitable for converting the lithium chloride brine containing sub all lithium metal applications, another method involves stantial impurities into lithium carbonate via a process converting lithium carbonate to lithium hydroxide. This of precipitation of lithium carbonate with soda ash. The process requires considerable effort to generate a highly lithium carbonate is subsequently converted to lithium pure form of lithium hydroxide. Lithium hydroxide 55 produced in this way is subsequently reacted with puri hydroxide by lime treatment of lithium carbonate to fied hydrochloric acid and evaporated to dryness to produce lithium hydroxide and waste calcium carbon produce highly pure lithium chloride. While this ate. Crystallization of the lithium hydroxide substan method is technically viable, it is far more costly than tially removes the boron and alkali metal impurities by yet another method involving the production of lithium way of a bleed stream. The lithium hydroxide is then chloride directly from naturally occurring lithium chlo treated with hydrochloric acid to produce lithium chlo ride brines. ride or treated with CO2 to produce high purity lithium Direct production of high purity lithium chloride carbonate. These conversions are accomplished accord from brine, however, is not a simple process. Naturally ing to the following series of reactions: occurring brines found, e.g., in the United States and 65 2LiCl-Na2Co3-2NaCl--Li2CO3 (1) Chile, contain reasonable concentrations of lithium, in the form of lithium chloride Some of these brines have high concentrations of lithium and a low magnesium to 3 4,980,136 4. LiOH.H2O-HCL-LiCl-2H2O (3) the extraction of boron from magnesium chloride solu tions using a solution of iso-octanol in petroleum ether. 2LiOH.H2O--CO2-Li2CO3-3H2O (4) These processes are nevertheless costly for production This process, while both complex and costly, is conven or purification of lithium chloride with boron concen tionally utilized to obtain lithium chloride of sufficient trations less than 25 ppm B. U.S. Pat. No. 4,271,131 and purity for use in the electrolytic production of lithium related U.S. Patent Nos. 4,243,392; 4,274,834; 4,261,960 metal from lithium chloride. teach the concentration of lithium chloride to about Lithium carbonate crystals precipitated from lithium 40% by weight, followed by heating at high tempera chloride brines containing boron typically retain a con tures in excess of 200 C. to insolubilize the boron in an taminating quantity of lithium borate.
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