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UNITED STATES PATENT Office Process and Agents for the Recovery of MAGNESUMONS from BR NE Melvin J

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UNITED STATES PATENT Office Process and Agents for the Recovery of MAGNESUMONS from BR NE Melvin J Patented Oct. 22, 1946 2,409,861 UNITED STATES PATENT office PROCEss AND AGENTs FoR THE REcovERY OF MAGNESUMONS FROM BR NE Melvin J. Hunter and William C. Bauman, Mid land, Mich., assignors to The Dow Chenniea Company,Michigan Midland, Mich., a corporation of No Drawing. Application February 2, 1942, Serial No. 429,303 5 Claims. (C. 23-50) 2 This invention concerns an improved process agents vary considerably as regards the con for the recovery of magnesium ions in relatively venience and economy with which they may be concentrated form from brines containing the employed. Sulphonated organic resins are pre Same. It also concerns certain base exchange ferred, since they have the properties of rapidly agents (also known as cation exchange agents) absorbing magnesium ions from sea water, of rap suitable for use in the process. idly and nearly completely liberating the ab It is well known that the chemical reaction Sorbed magnesium ions upon subsequent treat involved in the use of a base exchange agent is ment with an alkali metal salt solution and of reversible and that the direction in which it pro Swelling or shrinking only moderately during ceeds is dependent to a large extent upon the O use in the process. relative proportions of the reactive positive ions, We have now found that organic resins which e.g. alkali metal ions and alkaline earth metal contain carboxyl groups (which resins are here ions, on the exchange agent and in the liquor inafter referred to generically as “carboxylated in contact with the exchange agent. For in resins') possess cation exchange properties and stance, in usual Water Softening processes the s that when employed in the form of their am water is passed through a bed of a granular monium or other alkali metal salts they are far base exchange agent Such as Sodium aluminum more Selective as regards their ability to absorb silicate, whereby the alkaline earth metal ions in magnesium ions from brines which also contain the water are absorbed by the exchange agent alkali metal salts than are the sulphonated resins, with displacement of alkali metal ions from the 20 i. e. the atomic ratio of magnesium ions to alkali latter so that the water is depleted of alkaline metal ions which may be absorbed from Such earth metal ions and enriched in alkali metal brine by a carboxylated resin is far higher than ions. After becoming saturated with alkaline may be absorbed from a like brine by a sul earth metal ions by Such use in Softening Water, phonated resin. In this connection it may be the exchange agent is reconditioned usually by 25 mentioned that during use for the absorption passage of a dilute, e.g. of about 5 per cent Con of magnesium ions from a brine containing the centration, sodium chloride solution over the same and an equal or larger proportion of alkali same. The absorbed alkaline earth metal ions metal ions no exchange agent is converted en are displaced from the exchange agent by the tirely into its magnesium salt. Instead, the re Sodium ions of the Salt Solution, thus recon 30 action proceeds to a point at which there is verting the exchange agent into its Sodium Salt equilibrium between the magnesium and alkali which may, of course, be used to soften further metal ions on the exchange agent and those quantities of Water. in the brine contacted therewith. The alkali In a co-pending application of John J. Grebe salts of the carboxylated resins usually also pos and William C. Bauman, Serial No. 429,185, filled 35 sess an exceptionally high absorptive capacity for concurrently herewith, and issued October 30, magnesium ions. s 1945, as U. S. Patent 2,387,898, it is disclosed that However, the carboxylated resins have certain base exchange agents may be used to absorb properties which render them inferior to the magnesium ions from sea water, or similar brines sulphonated resins when employed for the ab containing a higher concentration of alkali metal 40 sorption of magnesium ions from brines using than of magnesium ions, and that by thereafter the hereinbefore described preferred procedure of treating the exchange agent with a fairly con the co-pending Grebe and Bauman application, centrated solution of sodium chloride or other Serial No. 429,185. For instance, most carboxyl alkali metal salt, the absorbed magnesium ions ated resins swell or shrink markedly with change may be displaced from the exchange agent with 45 in the salinity of the aqueous liquors contacted formation of a magnesium salt solution which therewith and, although these resins are excep contains the magnesium ions in higher concen tionally selective as regards the absorption of tration than in the initial brine. It is also shown magnesium ions from brines which also contain that although any of a wide variety of base alkali metal salts, they do not satisfactorily re exchange agents may be used in the process, such 50 lease the absorbed magnesium ions upon subse 2,409,861 3. e 4 quent treatment with an aquecus solition of sodius boxylated resins are described in U. S. Patents um chloride or other aikali metal salt, i. e. tile i,945,307, 2,047,398 and 2,230,240, which patents, magnesium sait Solutions tii is regenerated aire however, do not recognize the fact that the resins of undesirably iow concentration. possess properties rendering then useful as base It is an object of this invention to provide a exchange agents. method whereby carboxylated resins may satis in addition to the previously known carboxy factorily be used for the recovery of magnesilim ated resins just mentioned, we have prepared cer. ions in relatively concentrated form from brines tain new carboxylated resins which are especially which also contain alkali metal Saits and where well suited for use in the process. These new by the magnesium sait solution formed by dis carboxylated resins are co-polymers of an alpha placement of the absorbed magnesium ions from beta-unsaturated dicarboxylic acid, a readily the resin may be obtained in unusually high polymerizable vinyl or vinylidene compound concentration and in a form containing not more which contains only a single olefine group in the than a minor amount of other salts. Another molecule, and a polymerizazle organic compound object is to provide certain new carboxylated 5 containing at least two olefine groups in the resins which possess a combination of physical molecule. Examples of alpha-beta-unsaturated and chemical properties rendering them espe acids which may be used in making these resins cially well suited to use in the process. Other are maleic acid, fumaric acid, citraconic acid, ita objects will be apparent from the following de conic acid, etc. In place of these free acids, the . scription of the invention. 20 corresponding acid anhydrides may be used. Ex The present process comprises as its essential amples of vinyl and vinylidene compounds con steps (1) passage of brine containing a magnesium taining a single olefinic group which may be salt and an equimolecular or higher proportion used in making the products are styrene, alpha of an alkali metal salt through a bed of an am methyl-styrene, Ortho-methyl-styrene, meta-me monium or other alkali salt of a carboxylated 25 thyl-styrene, para-methyl-styrene, meta-ethyl resin, whereby the latter absorbs the magnesium styrene, para-isopropyl-styrene, ortho-cloro-sty ions (and other polyvalent metal ions if present) rene, para-chloro-styrene, vinyl chloride, vinyl from the brine; (2) thereafter passing an aque acetate, etc. Among the various polymerizable ous solution of an acid through the bed to dis compounds containing two or more olefinic groups place the absorbed magnesium ions from the car 30 in the naoiecule which may be used in making the boxylated resin to form a relatively concentrated resins are divinyl benzene, butadiene, isoprene, solution of a magnesium Salt and at the same tung oil, oiticica oil, divinyl ether, etc. The pol time convert the resin into its acid form; and (3) yolefinic reactant serves as an agent for de treating the resin with an aqueous solution of an creasing the tendency of the resin product to alkali and a soluble alkali metal salt to form Swell or shrink during use as a base exchange the alkali metal salt of the carboxylated resin so agent. It is believed to function principally as that the latter may be reemployed for the absorp an agent for bonding together, or vulcanizing, the tion of magnesium ions from the brine. In the linear co-polymers of the other reactants and only first of these steps it is important that the resin a very Small proportion thereof, e. g. an amount be used in the salt form specified, since the car 4. corresponding to 0.01 mole or less per mole of the boxylated resins when in their acid form do not unsaturated dicarboxylic acid is required. It Satisfactorily absorb magnesium ions fron brines. nay, of course, be used in much larger propor The use of an acid capable of forming a soluble tions. The alpha-beta-unsaturated dicarboxylic magnesium salt for displacement of the absorbed acid, or its anhydride, is preferably used in magnesium ions from the resin in the Second step 45. armount equai to or exceeding the sum of the is required in order to recover the major portion molecular equivalents of the other polymerizable of the magnesium absorbed by the resin. As reactants So as to obtain a large number of car hereinbefore mentioned, solutions of alkali metal boxyl groups in the resin molecule.
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