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United States Patent (11) 3,615,174

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United States Patent (11) 3,615,174 United States Patent (11) 3,615,174 72 Inventor William J. Lewis 3,342,548 9/1967 Macey....... A. 2319 X South Ogden, Utah 3,432,031 3/1969 Ferris........................... 209/166 X 21 Appl. No. 740,886 FOREIGN PATENTS 22, Filed June 28, 1968 45 Patented Oct. 26, 1971 1,075,166 4f1954 France ......................... 209/66 (73) Assignee NL Industries, Inc. OTHER REFERENCES New York, N.Y. Chem. Abst., Vol. 53, 1959, 9587e I & EC, Vol. 56, 7, Jy '64, 61 & 62. Primary Examiner-Frank W. Lutter 54 PROCESSFOR THE SELECTIVE RECOVERY OF Assistant Examiner-Robert Halper POTASSUMAND MAGNESUMWALUES FROM Attorney-Ward, McElhannon, Brooks & Fitzpatrick AQUEOUSSALT SOLUTIONS CONTAINING THE SAME 11 Claims, 4 Drawing Figs. ABSTRACT: Kainite immersed in brine in equilibrium con 52) U.S. Cl........................................................ 23138, verted to carnalite by cooling to about 10 C. or under. Car 209/11, 209/166,23191, 22/121 nallite so obtained purified by cold flotation. Purified carnal (5) Int. Cl......................................................... B03b 1100, lite water leached to yield magnesium chloride brine and B03d 1102, C01f 5126 potassium chloride salt. Latter optionally converted to potas 50 Field of Search............................................ 209/166,3, sium sulfate by reaction with kainite, or by reacting the carnal 10, 11; 23.19, 38, 121 lite with kainite. Naturally occurring brine concentrated to precipitate principally sodium chloride, mother liquor warm 56 References Cited concentrated to precipitate kainite, cooled under mother UNITED STATES PATENTS liquor for conversion to carnallite. A crude kainite fraction 2,479,001 8/1949 Burke........................... 23.191 purified by warm flotation and a crude carnallite fraction pu 2,689,649 9, 1954 Atwood..... 209/166 rified by cold flotation reacted together to yield magnesium 3,099,528 7 11963 Hadzeriga .................... 23/91 X chloride brine and potassium sulfate salt. Age SOLe Swaporation ConCEna RNE 23 2" 28 trator sel 57 arise N7 a -55 KAnte 25c+ 64. cARNALLute loc Ca. So es 59 64 60 N1igo 6ta-63 65 7 626 3. -KCl/NacilSalt 66 drey 68 spreader 6. HMsCl salt 43 cleaner 70 O 49 Conc. Mscleri NE M3so RefNed each cc sate-reactor K2SOs 441 carnaults ter o SA 47 48 PATENTEDOCT 26 1971 SHEET 1. Of 4. 3, 6l 5, 74 % MgCl 200 50 00 50 O (Na, Ms.K)(elso.) 25c v3 PATENTEDOCT 26 197 3, Sl. 5, 74 SHEET 2 OF 4 2OO BSCHOFTE NO MgCl2, 6H2O T s E 12 O CARN A TE s 2 O MgCl, KCl 6-O 150 Y O s C o C | s OY L t L EPSON1 TE 100 - O c S. aS O s PCROMETE Mg'so KSO-6HO 50 MRAL TE O - 50 O + 50 (Na, M3, k)(C1,SO) o'c inventore Will AM J. Lewis Fine 2 t4r14, ( /te '', 4. 1 f is /32 c -la. Y /// A -/ ATO Re NES PATENTEDOCT 26 (97. SHEET 3 OF A al??nnanzibo-0,01 EY M 3,615,174 1 2 PROCESS FOR THE SELECTIVE RECOVERY OF Based on the above discoveries, the present invention em POTASSUMAND MAGNESUMWALUES FROM ploys basically the principles of fractional solar evaporation of AQUEOUSSALT SOLUTIONS CONTAINING THE SAME naturally occurring brines for eliminating the bulk of sodium chloride and thence precipitating crude kainite salt upon This invention pertains to improvements in the selective 5 further concentration, but differs basically at this stage from recovery of potassium and magnesium values from aqueous prior techniques, in that the kainite salt is not harvested as salt solutions containing chloride and sulfate salts of sodium, such, but is retained under the mother liquor from which it is potassium and magnesium. precipitated and the mother liquor cooled thence to a suff The invention pertains more particularly to the recovery of ciently low temperature to convert the kainite salt into carnal such values from naturally occurring brines, such as salt lakes, 10 lite, which is harvested and purified by flotation in a cold bitterns, inland seas, etc. which are high in such metallic salt system, i.e., at about 0 C. employing the flotation agents concentrations. Where such brines are so located that solar above discussed. evaporation is available throughout a substantial portion of the year, it becomes economically feasible to process the same In the practical application of this basic process in tem for recovery in particular of potassium salts for use as a fertil 5 perate climates, such as that prevailing in the area of the Great izer or soil enricher among others, and magnesium salts for Salt Lake, the lake brine is subjected to successive stages of use in the production of metallic magnesium by electrolysis. solar evaporation during the warm summer months ultimately Fractional crystallization by solar evaporation of brines to precipitate kainite salt which is retained under the mother similar in composition to those of the Great Salt Lake in Utah, liquor until cold weather at sufficiently low temperature yields first common salt, NaCl, and then a mixture of common prevails to convert the kainite into carnallite. The mother salt with various complex double salts. Under most conditions liquor is thereupon withdrawn and the crude carnallite salt of solar evaporation in warm or summertime environment, the harvested and processed as above. crude complex harvest salts thus obtained will consist almost In accordance with a modification of the basic process some entirely of kainite salt, MgSOKSO, MgCl6HO or Mg of the kainite salt is harvested and purified by flotation at SOKC13H,0, admixed with common salt NaC1, from which 25 warm temperature and stored. When the weather turns suffi latter the kainite slat may be separated and purified by flota ciently cold to convert the remaining kainite into carnallite, tion. Long chain fatty amine acetates or chlorides preferably the latter is harvested and purified in a cold flotation system. of at least eight carbon atoms, may be employed as floating The purified kainite and carnallite values are then admixed agents and aliphatic alcohols of at least five carbon atoms, and reacted in accordance with equation (2) above to such as pentasol, as frothing agents. produce KSO, salt and MgCl, brine. The purified kainite salt thus obtained as well as the mother The invention thus provides an extremely simple and liquor from which the crude salt is precipitated, may be economical process for selectively recovering potassium and processed by various techniques for selective recovery of the magnesium values from naturally occurring brines wherein potassium and magnesium values. In all such processes of solar evaporation is relied on for concentrating the brine and which I am aware, however, the starting point for recovery of 35 ultimately precipitating crude kainite salt, and wherein natu the potassium values is the purified kainite salt the processing rally occurring temperature changes are relied upon for con of which for separating the potassium and magnesium values verting the crude kainite salt into crude carnallite salt, which thereof is inherently complex and expensive. requires upon flotation purification, only treatment with water for separation and recovery of the potassium and magnesium The present invention eliminates this difficulty by employ 40 ment of several discoveries which have made and which are values, unique and basically novel insofar as I am aware. The first of The brine withdrawn from the carnallite or kainite these discoveries is that kainite will convert to carnalite, precipitation stages is high in magnesium chloride and sulfate MgCl, KC-6H,0, if cooled below about 10°C. (50 F.) under values, the magnesium sulfate content of which is converted the mother liquor from which the kainite salt is precipitated. 45 by desulfation as with CaCl, into magnesium chloride. This The second discovery is that crude carnallite salt may be combined with the MgCl, brine obtained from the reactions refined or purified by flotation in a cold flotation circuit main above discussed, is in accordance with the invention, concen tained below the above temperature. trated sufficiently for spray drying and then converted into a By thus converting crude kainite salt to crude carnallite salt dry MgCl, powder in this way for further processing as desired. and purifying the crude carnallite salt in a cold flotation 50 system, separation of the potassium and magnesium values is Having thus described the invention in general terms, readily effected by simply leaching the carnallite salt with reference will now be had to the accompanying drawings for a water to produce potassium chloride salt and magnesium more detailed description of the above and other features, chloride brine according to the reaction: wherein, 55 FIG. 1 is an equilibrium phase diagram of the (Na, Mg, K) (1) Carnallite Sait Salt (Cl, SO) salt solution system at 25' C. and FIG. 2 is a similar KCl diagram at 0°C. Both are in the familiar reciprocal pair form which are separated by filtration. plotting univalent mols per 1,000 mols of water. For many applications the KCl salt thus obtained is not so FIG. 3 is a flow sheet in diagrammatic form of the basic desirable as the sulfate salt, which leads to my third discovery, 60 process of the invention, while FIG. 4 is a similar flow sheet of namely, that kainite will react with carnallite to produce the above-mentioned modified embodiment thereof. KSO, salt and MgCl, brine according to the reaction: Referring to FIG. 1, a brine in equilibrium with kainite and halite (NaCl) is shown plotted at 10, and will precipitate these (2) Kaillite -- Carnallite two salts upon evaporation and drive the composition of the MgSO-KCl3HOMgCl2. KCl-6H.O.--Ho 65 brine in the direction of the arrow 11. If, instead of being evaporated, the brine is cooled, the same two salts are Salt -- Brine precipitated due to reduced solubility and the brine equilibri KSO.
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