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United States Patent Office Patented May 1, 1962 2 Event, a Test Run Suffices to Indicate a Time Sufficient to 3,032,389 Solubilize the Lithium Content

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United States Patent Office Patented May 1, 1962 2 Event, a Test Run Suffices to Indicate a Time Sufficient to 3,032,389 Solubilize the Lithium Content 3,032,389 United States Patent Office Patented May 1, 1962 2 event, a test run suffices to indicate a time sufficient to 3,032,389 solubilize the lithium content. SEPARATION OF LITHIUM FROM LITHUM The process of this invention is operable with lithium BEARNG MECAS AND AMBLYGONTE bearing micas and amblygonite only. Spodumene, for Ludo IK. Frevel, Midland, and Leonard J. Kressley, Sagi example, is not operable in this process, even with prior naw, Mich., assignors to The Dow Chemical Company, preheating at 1100 C. to transform it to beta-spodumene. Midland, Mich., a corporation of Delaware When it is attempted to react spodumene or beta-spodu No Drawing. Filed Feb. 19, 1959, Ser. No. 794,241 mene with SO at 600 C. to 900 C., only a negligible 2 Claims. (CI. 23-31) amount of lithium is thereby rendered soluble. This invention concerns the separation and recovery 10 The following examples represent specific embodiments of lithium values from lithium-bearing micas, such as of this invention. Parts and percentages therein are by lepidolite, and from amblygonite. More specifically, it weight. In each example, a quartz reactor provided with concerns a process in which a lithium-bearing mica or a condenser followed by a filter to remove entrained amblygonite is subjected to high temperature attack with mist was charged with coarse particles of lithium-bearing a stream of sulfur trioxide for a relatively short time 5 mica or amblygonite, 4 inch being the largest dimension. and to the subsequent aqueous extraction of enriched Each charge was treated at about 600 to 900 C. with lithium values from such treated lithium-bearing ore. a stream of SO carried by He, or a mixture of SO2 and This application is a continuation-in-part of application O2 forming SO under conditions of reaction, or with a Serial No. 575,972 filed April 4, 1956, now abondoned. stream of SO.8 per se, the SO3 being in excess of that Until the present time, lithium values have been sep 20 required to transform the lithium values to Li2SO4. arated and recovered from lithium-bearing ores by pro Any gas which is inert under conditions of reaction, such longed fusion processes and complete dissolution of the as helium, neon, argon, nitrogen, etc., can be used as (ore. Thus, tedious, time-consuming reactions and sep an SO carrier. The so-treated charge was transferred aration processes had to be resorted to in the past in to a Soxhlet thimble and leached in water. The aqueous order to recover a purified lithium salt. See, for example, 25 solution so obtained was evaporated to obtain the weight Schieffelin, Manufacture of Lithium from Lepidolite, Jl. of the salt, and dried at 120° C. Anhydrous lithium Soc. Chem. Ind. 27: 549-550 (1908), and Weidmann chloride was obtained by (1) titrating the salt solution U.S. Patent No. 1,544,114, patented June 30, 1925. with the requisite quantity of aqueous barium chloride Furthermore, the ores first had to be finely ground be solution to precipitate the sulfate; (2) filtering the re fore being processed according to the prior art. 30 sulting chloride solution; (3) evaporating the water It has now been discovered, in accordance with this from the filtrate so-obtained; (4) extracting the lithium invention, that a lithium-bearing mica or amblygonite in chloride from the resulting residue with n-amyl alcohol; coarsely particulate or sub-divided form can be reacted (5) evaporating the alcohol, from the solution, so ob at an elevated temperature ranging from about 600 to tained, as by blowing a gentle stream of dry nitrogen into about 900 C. with a stream of SOs for a relatively short 35 the alcoholic lithium chloride solution. time so as to render lithium values water-soluble without EXAMPLE 1. at the same time dissolving the ore matrix. Aluminum and iron values are not attacked thereby, rendering sub Time Charge Operation sequent separation and recovery of lithium much less Temp., C. difficult and considerably more satisfactory with respect 40 to high purity and high recovery of lithium salt. The o - - - - - - - - - - - - - - - - - - - - - - - - 550 Started18 g. liquidpassing SO3 Ee at through rate of lithium values, as sulfate concentrate, are thereafter dis 170ml.fmin. solved out in water and can be recovered in a highly 55mins-------------------- 890 Heatvaporized). off; SO3 off (15 g. SOs purified form, such as lithium chloride, by titrating the 2hrs. 5 mins-------------- 850 aqueous concentrate with the requisite amount of aqueous 45 barium chloride to precipitate the sulfate, filtering the Weight of lepidolite charge=14.9493 g. chloride solution, evaporating water from the filtrate, and extracting the lithium chloride therefrom with n-amyl Weight gain of SO-treated charge=1.5775 g. alcohol and evaporating the alcohol. Weight of condensate from reactor effluent=0.2540 g. The amount of SOs used must be sufficient to react Weight of dried, H2O-leached residue=13.0444 g. with the bound lithium, but otherwise is not critical, since 50 Weight of extracted salts (LiSOHO, KLiSO, unreacted SOs can be recovered for re-use. The SO etc.) =3.4638 g. can be formed catalytically in known manner, during or Lithium balance: immediately before its reaction with the lithium-bearing LiO content of initial charge=0.623. g. = 4.17 wt. mica or amblygonite from a mixture of SOa and O, ad percent - vantageously by passing a mixture of SO2 and O. over 55 LiO content of dried, HO-leached solid resi a conventional platinum-on-silica gel catalyst or equiva due=0.070 g.=0.54 wt. percent lent at 450 C. or above in the usual way. Also, while Percent Li removals 88.8% oxygen will react with SO2 in the presence of iron impurity present in lepidolite and amblygonite at reaction tempera EXAMPLE 2. tures of 600 to 900 C. to form SO3, SO and air will 60 not react appreciably under similar conditions to form Time Temp., C. Operation SO3, even when excess air over theory is present. 0-------------------------- 500 Started SO2 flow at 0.41 gif The temperature of reaction ranges from about 600 min. Started O2 flow at 137 ml/min. 25C, 1 atm. to 900 C. Below 600° C., dissolution of the ore takes 65 SO3 formed in situ. place and iron and aluminum, in particular, are attacked lhr. 20 mins-------------- 800 and rendered water-soluble. Above 600 and up to 900 2hrs. 10 mins------------- 850 Heating current off, SO2 off, C., however, the ore matrix is not attacked and the iron N2 on. and aluminum values are not rendered soluble. The reaction time varies with the batch size and tem Weight of lepidolite charge=8.6139 g. perature used. Generally one to two hours is sufficient 70 Weight gain of SO-treated charge=1.2993.g. within the temperature range of 600 to 900 C. In any Weight of condensate=1.0196.g. 3,082,389 3 4. Weight of dried, HO-leached residue=7.8970 g. Among the advantages of the process of this invention Weight of extracted salts (LiSOHO, KLiSO, etc) = over the prior art are (1) the lithium-containing mica 2.7998 g. or amblygonite need not be finely ground before re Lithium balance: action with SOs; (2) the ore matrix is not attacked and LiO content of initial charge 0.359 g. = 4.17 wt. per dissolved, thus it is much less difficult to separate lithium cent from associated impurities; (3) the reaction is not time LiO content of dried, HO-leached residue-0.0466 consuming; (4) aluminum and iron are not dissolved, g. =0.59 wt. percent therefore less reagent SO is needed; (5) unreacted SO3 Percent Li removal-87.0% is readily recirculated. Weight of isolated LiCl, from extracted salts=0.8704 IO EXAMPLE 5 g=0.326 g. LiO Crushed lepidolite containing quartz was heated at Percent Li recovery=90.8% 600 C. for one hour in a quartz reactor while exposed EXAMPLE 3 to a stream of a mixture of SO2 and air (run ) and at 5 300° C. for one hour in the presence of a mixture of SO2 and air (run 2). In contrast thereto, runs 3 and 4 utilized Time Temp., C. Operation SO at 600 C. and at 630 C., each for one hour, the SOs 0-------------------------- 500 Started SO2 flow at rate of having been prepared catalytically by passing a mixture 0.4 g/min. of SO2 and O. over a conventional platinum-on-silica-gel 35 mini-------------------- 900 Started O2 flow at rate of 137 20 ml.fmin. SO3 formed in situ. catalyst at 450° C. The amount of SO2 oxidized to 2hrs. 10 mins------------- 860 Heating current off, SO2 off, SO was equivalent to the SO2 present in the mixtures N2 on. of runs 1 and 2. The sulfated lithium values were ex tracted with water and recovered. In runs 1 and 2, more Weight of amblygonite=18.1887 g. than sufficient air was present to oxidize the SO2 to SOs 25 if a catalytic reaction were used. Runs 1 and 2 concern Weight gain of SO3-treated charge=2.1763 g. experiments outside the scope of the invention and are Weight of dried, HO-leached residues = 15.9296 g. included for purposes of comparison. Weight of extracted salts=5.1189 g. Results are summarized in the following table. Table Run 3 SO3 (from Run 1 (Blank) Run 2 (Blank) SO 70 ml.1 Run 4 SO3 (from SO 70 ml.1 SO 70 mi./ min. and O SO 70 mlf main. air 80 min. air 180 90 ml finin.
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