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United States Patent Office Patented Nov 3,007,770 United States Patent Office Patented Nov. 7, 1961 2 3,007,770 umene from the other components of the ore such as EXTRACTION OF LITHUM quartz and feldspar gangue. The alpha-spodumene, thus Henry C. Kawecki, Fleetwood, and Albert J. Cole, Potts in a form at least as fine as that which results from sim town, Pa., assignors to Kawecki Chemical Company, ple crushing of the ore, is then heated in an indifferent Boyertown, Pa., a corporation of Pennsylvania or ambient atmosphere to a temperature of about 1000 No Drawing. Filed July 8, 1954, Ser. No. 442,218 1300 C. Temperatures below about 1000 C. are rel 3 Claims. (C. 23-33) atively ineffective in bringing about the conversion of alpha-spodumene to beta-spodumene, and temperatures This invention relates to the extraction of lithium above about 1300 C. tend to promote agglomeration by from spodumene ore and includes not only a new meth 10 fusion of the spodumene or gangue constituents. The od for transforming this spodumene to a novel chemical length of this heat treatment is determined solely by the product.ly reactive form but also a method of purifying this novel condition of the resulting product, the decrepitation of r the beta-spodumene (but not of the gangue constitu Lithium ores are notoriously refractory. Spodumene, ents) being visible evidence of effective conversion of the a lithium aluminum silicate which is generally represented 15 alpha-spodumene to beta-spodumene. by the formula Li2O'Al2O3'4SiO2, is a relatively com The resulting decrepitated beta-spodumene, after its mon lithium ore and is particularly refractory. In fact, separation from the relatively coarse non-decrepitated the naturally occurring alpha-spodumene is so unreactive gangue constituents if the latter are present during this that the art considers this raw material to be rendered conversion step, is then converted to the new reactive considerably more reactive when, by heating it to a tem 20 lithium mineral pursuant to our invention. This conver perature within the range of about 1000° C. to 1300° C., sion is effected by heating the beta-spodumene while sus the lithium component of the resulting beta-spodumene pending it in an aqueous solution of a strongly alkaline can be made to go into aqueous solution by roasting the compound of sodium or potassium. The beta-spodu beta-spodumene in admixture with concentrated sulfuric mene may thus either be slurried with water and the alka acid. line compound then added to the slurry, or the beta-spod We have now discovered that beta-spodumene can be umene may be slurried with the alkaline compound solu converted by a very simple procedure into solid form tion itself. In either event, the amount of water re which can best be described as a new lithium mineral and quired during this conversion step is merely that which that the lithium component of this mineral is, chemically is necessary to form a fluid slurry of the beta-spodumene. speaking, very reactive. This conversion of beta-spodu 30 The alkaline compound of sodium or potassium used mene to the new mineral form is effected by heating the to convert the beta-spodumene to a chemically reactive beta-spodumene in an aqueous solution of strongly alka lithium-containing mineral pursuant to our invention is line compounds of sodium and potassium. Thus, our preferably either the hydroxide or carbonate of sodium or new method for converting naturally occurring alpha potassium. The amount of this alkaline compound which spodumene to the form of a chemically reactive mineral 35 is useful in effecting such conversion may vary widely. comprises heating the alpha-spodumene in the crushed For example, we have found that as little as 10 parts by state to a temperature of at least about 1000 C. but be weight of sodium or potassium hydroxide per 100 parts by low its fusion temperature with the resulting conversion weight of beta-spodumene are effective in converting the and decrepitation of the alpha-spodumene to beta spod beta-spodumene to the new chemically reactive form and umene, suspending the resulting decrepitated beta-spod 40 that solutions containing as much as 100 parts by weight umene in an aqueous solution of a strongly alkaline of the hydroxide per 100 parts by weight of beta-spodu compound of sodium or potassium containing at least 10 mene are also effective. Similar amounts of the car parts by weight of the alkaline compound per 100 parts bonates of sodium and potassium are also effective. Actu by weight of beta-spodumene, heating the resulting slurry ally, when used in amounts of at least 10% by weight of to a temperature at least to its boiling point, and there the beta-spodumene, the amount of alkaline compound after separating the resulting solid material comprising a which is used affects only the time required to effect the lithium-containing mineral the lithium component of conversion of the beta-spodumene to the new mineral which is chemically reactive. form. For example, in order to effect conversion of 90% This novel lithium-containing mineral can be purified of the beta-spodumene to the chemically active mineral pursuant to our invention by admixing the mineral with 50 form in boiling sodium hydroxide solutions, and expressed dilute sulfuric acid to effect the solubilization of the lith in terms of parts by weight per 100 parts of beta-spodiu ium component of the mineral in the form of a lithium mene, 15 parts of the hydroxide requires a 16-hour con sulfate solution, adding hydrogen peroxide to the lithium version period, whereas 20 parts of the hydroxide reduces sulfate solution in amount sufficient to precipitate any the conversion period to 8 hours and 25 parts of the hy dissolved iron and manganese contained in the solution, droxide effects the conversion in about 4/2 hours. In and separating any resulting precipitated iron hydroxide order to convert 85% of the beta-spodumene to the and manganese dioxide from the lithium sulfate solution chemically active form, and again expressed as parts by while the latter is at a pH at least as high as 4.2 so as to weight of sodium hydroxide per 100 parts of beta-spodu obtain a substantially pure lithium sulfate slution. mene in boiling water, 10 parts of the hydroxide requires In practicing the method of our invention, the step of 60 a 24-hour conversion period, 15 parts of the hydroxide converting alpha-spodumene to beta-spodumene is not lowers the conversion period to 4/2 hours, 25 parts of novel and is carried out according to conventional pro the hydroxide still further lowers the conversion period cedure. The alpha-spodumene may be treated while ad to 334 hours, and 50 parts of the hydroxide effects the mixed with other gangue constituents in the form of conversion in only 2 hours. In order to increase the crushed but unbeneficiated spodumene ore or an alpha 65 conversion above about 95%, 20 parts of sodium hy spodumene concentrate may be used as the starting mate droxide, expressed as hereinbefore, requires a conversion rial. Any conventional wet or dry beneficiation practice period of 15 hours, 25 parts of the hydroxide lowers the may be used for the physical separation of the alpha-spod conversion period to 5 hours, and 50 parts of the hy 8,007,770 3. 4. droxide effects the conversion in only 1 hour. It will be merely that which will effect permanent acidification of readily appreciated, therefore, that the concentration of the resulting aqueous medium. The solubilization of the the sodium hydroxide solution (which is representative lithium can be accelerated by heating the aqueous reac of the other useful solutions mentioned heretofore) and tion medium, although the reaction will proceed some the length of the conversion period are inversely related 5 what more slowly at normal ambient temperature. Com to one another and that the actual concentration of the pletion of the reaction is thus indicated by the develop alkaline compound of sodium or potassium which is used ment of a permanent acidic pH value in the aqueous re for this conversion is not critical provided it is used in action medium. s amount of at least about 10% by weight of the beta In effecting dissolution of the lithium component of the spodumene. 0 new lithium mineral by its reaction with sulfuric acid, The temperature required to effect this conversion also we have found that the aluminum present in the mineral influences the time required to effect the conversion. In will not enter into the solution to any significant extent general, the higher the temperature the shorter the con if the ultimate pH of the reaction medium is not lowered version period, and for this reason we presently prefer below about 4.2. If a lower pH is inadvertently or in to use reaction temperatures which are close to, and are 5 tentionally attained, the aluminum which thereupon goes advantageously at, the boiling point of the alkaline com into solution may be readily thrown out of solution by pound solution. Thus, in order to carry out this con neutralizing the aqueous medium with ammonia until version, the only special requirement for the conversion the pH rises to at least about 4.2. The resulting acidic apparatus is that it be capable of withstanding the cor solution of lithium sulfate which is obtained when the rosive effect of boiling strongly alkaline solutions. 20 pH of the solution is maintained below 7 but not below The chemical change which takes place as the beta about 4.2 contains, in addition to the lithium sulfate, a spodumene is converted to the new chemically reactive significant amount of iron and manganese which were ini lithium mineral form appears to comprise primarily the tially present in the spodumene ore.
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