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United States Patent Office Patented Sept 3,000,702 United States Patent Office Patented Sept. 19, 196 2 since potassium fluoride is very soluble. In this case, a 3,000,702 MANUEFACTURE OF SODIUM FLUOR DE double or complex salt is formed in the melt between George L. Cunningham, Burtonsville, Md., assignor to potassium fluoride and the calcium salt and that is slowly W. R. Grace & Co., New York, N.Y., a corporation extracted with water in spite of the great solubility of of Connecticut potassium fluoride in water. The corrosion of the molten No Drawing. Filed May 23, 1958, Ser. No. 737,196 melt is also a considerable problem although suitable 4. Claims. (CI. 23-88) ceramic materials have been discovered for constructing the fusion vessel. This invention relates to a process for the manufac Processes have been devised for the production of so ture of sodium fluoride relatively low in silica content. 10 dium fluoride based on the thermal decomposition of More particularly, this invention relates to a cyclic proc sodium silicofluoride to sodium fluoride and silicon tetra ess whereby sodium fluoride, relatively low in silica con fluoride (U.S. 1,896,697, U.S. 2,588,786, 1,730,915, tent and ammonium chloride, may be manufactured from 2,602,726, and U.S. 1,664,348). These processes are cheap and readily available raw materials. faulty in that relatively high temperatures are required to As manufactured at the present time, technical sodium 15 decompose the sodium silicofluoride and thus it is very fluoride contains 94% to 97% NaF and 1.5% to 5.0% difficult to carry the reaction to completion. sodium silicofluoride (Na2SiFs). The latter impurity Numerous processes have been developed for react makes the sodium fluoride unsuitable for use in the man ing sodium silicofluoride or potassium silicofluoride with ufacture of cryolite. sodium carbonate or sodium hydroxide for the produc In accordance with the process described herein, the 20 tion of sodium fluoride and hydrated silica or sodium preparation of sodium fluoride is effected from relatively silicate (U.S. 1,382,165, U.S. 1,324,030, U.S. 1,464,990, inexpensive raw materials, without the use of acid-grade U.S. 1,701.225, U.S. 2,585,387, U.S. 1,581,819, U.S. fluorspar, without the use of sulfuric acid, without ex 1,634,122, British 647,395, and British 263,263). cessive evaporation, and with a minimum amount of A process has been developed whereby sodium chlo liquid in the several steps of the process, whereby an 25 ride is reacted with hydrofluoric acid. In this case, in economy of operation hitherto unobtainable is achieved. order to obtain economical yields of sodium fluoride, it Sodium fluoride has been prepared in a wide variety is necessary to neutralize, usually with ammonia, the hy of ways. For example, it has been produced by react drochloric acid generated so that the reaction may pro ing an alkaline earth fluoride such as fluorspar (CaF), ceed to substantial completion. Instead of sodium chlo with sulfuric acid to produce calcium sulfate and hy 30 ride, sodium nitrate and sodium sulfate have been used drofluoric acid. The relatively insoluble calcium sul (U.S. 1464,991 and U.S. 1464,990). It is clear that fate is filtered off or otherwise removed and the hydro the reaction is between ammonium fluoride and Sodium fluoric acid is reacted with sodium carbonate or sodium chloride, or sodium nitrate or sodium sulfate. Similar hydroxide to produce sodium fluoride. The sulfuric acid reactions are given by A.A. Chizhik, GoSundarst, Inst. used in the process is fairly expensive and corrosive. 35 Prikladnai Khim, Sparnik Statei, 1919–39, 56-73 (1939), The hydrofluoric acid produced is very corrosive and C. A. 36:2093. The yields of sodium fluoride in these quite poisonous. The sodium carbonate and sodium hy processes are quite good. However, the mother liquor droxide are relatively expensive and thus add to the cost contains sodium fluoride and ammonium chloride and of the sodium fluoride. - it is difficult to process this liquor to recover pure am Attempts have been made to simply substitute sodium 40 monium chloride and sodium fluoride. In most cases the chloride for the sodium carbonate or sodium hydroxide mother liquor was heated with milk of lime in order to of the above mentioned usual process of making sodium recover the ammonia. fluoride. However, the yield of sodium fluoride is not Sodium fluoride relatively low in silica has been made good, probably due to the effect of the hydrochloric acid from fluosilicic acid by first forming fluoboric acid and upon the reaction equilibrium. It has been attempted to then reacting this fluoboric acid with sodium carbonate, remove the HCl by heating but, in this case, a mixture 45 sodium bicarbonate or sodium hydroxide to form sodium of HCl and HF are removed. fluoride and recovering the boric acid as the sodium salt Numerous processes have been developed based on (U.S. 2,692,186). the fusion of fluorspar (CaF) with sodium carbonate A recent patent discloses the production of a mixture and an oxide such as SiO2, Al2O3, Fe2O3, etc., to pro of sodium fluoride and calcium oxide by fusing a mix duce a mixture of sodium fluoride and a calcium salt of 50 ture of fluorspar and sodium hydroxide (U.S. 2,690,430). the oxide in question. The sodium fluoride is then ex It is impossible to recover sodium fluoride from Such a tracted with water and the solution is evaporated to re mixture since, when it is added to water, it reverts to cal cover sodium fluoride. In these processes the yield of cium fluoride and sodium hydroxide. sodium fluoride is relatively high. However, such proc Many proposals have been made for making sodium esses suffer from one particularly noticeable disadvan 55 fluoride from fluosilicic acid. This interest is based on tage when employed for the production of sodium fluo the fact that this acid is an abundant waste product of ride, namely, the limited solubility of sodium fluoride in the manufacture of superphosphate, phosphoric acid and water. As a consequence the processes require very large of the purification of graphite. volumes of water and thus excessive evaporation. In My invention is based broadly on the discovery that addition to this, a double or complex salt composed of 60 the presence of ammonium hydroxide in aqueous solu sodium fluoride and the calcium salt forms when the tion depresses the solubility of sodium fluoride in water molten mass cools, and this compound is quite slow to and at the same time increases the solubility of ammoni dissolve. um chloride. This increases the proportional amount of A process has been developed whereby potassium car 65 sodium fluoride precipitated when sodium chloride, sodi bonate is substituted for sodium carbonate in the fusion um nitrate, or sodium sulfate is reacted with ammonium step. The fused mixture contains potassium fluoride fluoride, and also permits the removal of pure ammoni which is dissolved in water (U.S. 2,737,442). The re um chloride and sodium fluoride from the mother liquors. sulting potassium fluoride is reacted with sodium car The yields of sodium fluoride and ammonium chloride, bonate to precipitate sodium fluoride and regenerate po or ammonium nitrate or ammonium sulfate are quan tassium carbonate which is used in the next cycle. This titative. process avoids the use of excessiye yolumes of Water It is yisualized that the ammonium fluoride used in 8,000,702 3 4. my process would be produced from this waste fluosilicic The sodium fluoride residue is washed with water to acid although ammonium fluoride from any source is remove soluble salts. Obviously, a minimum amount of equally useful. For example the reaction of low grade water is used since the sodium fluoride is soluble to a fluorspar (containing relatively large amounts of silica) slight extent in water. The washings may be mixed with will react with sulfuric acid and other acidic materials the filtrate or may be discarded depending on the cost to produce fluosilicic acid and this acid is a suitable raw of evaporating the water. Since the washings are sub material for my new process. stantially saturated with sodium fluoride, it is contem In producing ammonium fluoride, fluosilicic acid at a plated that they will be mixed with the filtrate for fur emperature of about 50-90° C. and at a concentration ther processing to recover sodium fluoride. At this stage, of 25-30% is first admixed with anhydrous ammonia. 0 the filtrate from the ammonium chloride recovery step, This converts the fluosilicic acid to ammonium fluoride, described below, is added to the filtrate from the first which stays in solution, and silica, which precipitates as sodium fluoride filtration. The combined filtrates and a filterable solid. While the temperature of the reaction washings are then evaporated to crystallize a large por is stated to be about 50-90° C., a preferred range is tion of the sodium fluoride and a large portion of the 75-85° C. Above about 90° C., considerable difficulty 5 ammonium chloride. Then, anhydrous ammonia is added is experienced in retaining the ammonia in the system. to the mixture in an amount sufficient to dissolve all At the lower temperatures, i.e. below about 50 C., the of the ammonium chloride. It should be noted that am silica tends to be hydrated and is difficult to filter. It is monium chloride is relatively soluble in anhydrous am preferred to use fluosilicic acid at a concentration of monia or in aqueous solutions of ammonia. Addition of about 25-30%.
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