US2724635A - Production of an alkali metal double fluoride of titanium - Google Patents
Production of an alkali metal double fluoride of titanium Download PDFInfo
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- US2724635A US2724635A US269695A US26969552A US2724635A US 2724635 A US2724635 A US 2724635A US 269695 A US269695 A US 269695A US 26969552 A US26969552 A US 26969552A US 2724635 A US2724635 A US 2724635A
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- titanium
- alkali metal
- fluoride
- solution
- potassium
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- 239000010936 titanium Substances 0.000 title claims description 30
- 229910052719 titanium Inorganic materials 0.000 title claims description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 24
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims description 20
- 229910052783 alkali metal Inorganic materials 0.000 title claims description 15
- 150000001340 alkali metals Chemical class 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 238000000354 decomposition reaction Methods 0.000 claims description 13
- -1 TITANIUM IONS Chemical class 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 229910001508 alkali metal halide Inorganic materials 0.000 claims description 5
- 150000008045 alkali metal halides Chemical class 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 3
- 229910001413 alkali metal ion Inorganic materials 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 16
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 14
- 229910052700 potassium Inorganic materials 0.000 description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000011591 potassium Substances 0.000 description 10
- 238000005868 electrolysis reaction Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 6
- SQTLECAKIMBJGK-UHFFFAOYSA-I potassium;titanium(4+);pentafluoride Chemical compound [F-].[F-].[F-].[F-].[F-].[K+].[Ti+4] SQTLECAKIMBJGK-UHFFFAOYSA-I 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- 239000011698 potassium fluoride Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 235000013024 sodium fluoride Nutrition 0.000 description 4
- 239000011775 sodium fluoride Substances 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 3
- 235000003270 potassium fluoride Nutrition 0.000 description 3
- 229910001414 potassium ion Inorganic materials 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 150000002222 fluorine compounds Chemical class 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 239000002198 insoluble material Substances 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- BTYJRQCMLKRMLD-UHFFFAOYSA-H iron(2+) titanium(4+) trisulfate Chemical compound S(=O)(=O)([O-])[O-].[Fe+2].[Ti+4].S(=O)(=O)([O-])[O-].S(=O)(=O)([O-])[O-] BTYJRQCMLKRMLD-UHFFFAOYSA-H 0.000 description 2
- 150000003609 titanium compounds Chemical class 0.000 description 2
- SMNDYUVBFMFKNZ-UHFFFAOYSA-N 2-furoic acid Chemical compound OC(=O)C1=CC=CO1 SMNDYUVBFMFKNZ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- GEHLLHAUIUKKFH-UHFFFAOYSA-L [F-].[F-].[Na+].[K+] Chemical class [F-].[F-].[Na+].[K+] GEHLLHAUIUKKFH-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical class [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/002—Compounds containing titanium, with or without oxygen or hydrogen, and containing two or more other elements
Definitions
- the invention involves cycling thealkali metal component for compound fluorides of titanium through zones reacting alkali metal fluoride with a titanium. compound to formation of double fluoride, and
- titanium compounds as raw material for preparation of titanium double fluoride are such raw materials as ilmenite and other ores of titanium, more or less purified oxide of titanium, meta-titanic acids, slags containing high percentages of titanium dioxide, titanium sulfates, and the like.
- alkali metal fluoride component it will be understood that this comprises metals of the alkali group, potassium and sodium being preferred, and the term alkali fluoride concisely designates all these hereinafter.
- the double fluoride of titanium and alkali metal is subjected to decomposition in a decomposing zone to form titanium metal, and the alkali fluoride is a byproduct. While the decomposition of the double fluoride may be carried out by heat reaction, electrolysis is here more generally involved and in presence of chlorine, and as the details are not a part of the present invention, it is here suflicient to state that the compound fluoride of titanium and alkali metal as afore-mentioned, is decomposed to metallic titanium and fluorides such as of potassium and sodium. It is such latter material that is then recycled to the formation of double fluoride of titanium and alkali metal.
- a desirable procedure is to reduce the iron content to the ferrous state, either by heating in the presence of carbon (finely divided, or a reducing gas or reducing furnace atmosphere) or by addition of scrap iron and sulfuric acid. If the amount of the sulfuric acid is sufficient to react with all of the constituents of the ilmenite, there results titanium sulfate and iron sulfate solution. After such reaction is "ice completed, the solution is diluted and the insolubles such as silicates, etc., are removed by settling, decantation, filtration, and the like.
- the alkali metal fluoride as from the afore-mentioned decomposition of double fluoride of titanium and alkali metal.
- the alkali fluoride remaining from the electrolysis is recycled to the zone reacting'titanium compound with alkali metal fluoride in the first instance.
- an electrolytic bath based on double fluoride of titanium, together with a molten bath constituent of halide, a chloride of alkali or alkaline earth metal i.
- the decomposition may be generally represented by the following equation:
- reaction of sulfuric acid on the ilmenite as above-mentioned may be represented by the following equation:
- the reaction of the sulfuric acid on the ilmenite in the first instance involves raised temperature, and to the clear hot liquor, after filtration, the remaining fluoride requirement is added. Reaction occurs, and then the solution is evaporated down until crystals appear, and potassium titanium fluoride thus separates out. This potassium titanium fluoride is then re-dissolved and recrystallized, and made up for electrolysis with further sodium chloride, and is again subjected to decomposition. Chlorine is evolved, but fluorine is not. Thus, the prooess is completely cyclical, and the only losses are the minor losses normally encountered in properly controlled chemical operation. Costly fluorine is conserved and cycled through the respective reaction zones.
- a continuous type of operation may be applied, removing molten bath material from the reaction zone as the process proceeds, this being possible by reason of the fact that the titanium metal formed is segregated at the cathode.
- Ilmenite finely ground, is reacted upon .with sulfuric acid solution in amount to substantially completely dissolve it. Any insolubles are eliminated.
- reaction involves raised temperature, and to the clear hot solution, there is then added alkali metal fluorides, KF and NaF from the electrolysis of potassium titanium fluoride, in proportions of one mole of titanium sulfate and 2 until crystals begin to appear, and then on cooling, the
- potassium titanium fluoride separates out, and is removed by filtration. It is then re-dissolved and re-crystallized, I and mixed with sodium chloride in about the proportions And later with voltage increased to 5-8, and current density 200-500 amp., titanium metal sponge is deposited in a tightly adhering mass at the cathode, and the potassium fluoride isby-product for recycling to the production of potassium titanium fluoride.
- the solution is then evaporated furic acid to produce a solution containing titanium ions, separating any insoluble phase from the solution produced, reacting the solution with a source of fluoride ions and potassium ions consisting substantially of the spent salt bath resulting from the electrolytic decomposition of potassium fluotitanate in a fused alkali metal halide bath and recovering potassium fiuotitanate from the resulting solution by crystallization.
- the method of producing potassium fluotitanate from ilmenite which comprises reducing the iron content of the ilmenite to ferrous iron, digesting the resulting material in sulfuric acid to produce an aqueous solution containing titanium ions, separating insoluble materials therefrom, reacting the remaining aqueous solution with a source of fluorine ions and potassium ions consisting essentially of the spent salt bath resulting from the electrolytic decomposition of potassium fluotitanate in a fused alkali metal halide bath and recovering potassium fluotitanate from the resulting solution by crystallization therefrom.
- the method of producing potassium fluotitanate from ilmenite which comprises reducing the iron content of the ilmenite to ferrous iron, digesting the resulting material in sulfuric acid to produce an aqueous solution containing titanium ions, separatiing any insoluble materials therefrom, reacting the remaining aqueous solution with a source of fluorine ions and potassium ions in the proportion of one mole of KF to two mols of NaF consisting essentially of the spent salt bath resulting from the electrolytic decomposition of potassium fluotitanate in a fused sodium chloride bath and recovering potassium fluotitanate from the resulting solution by crystallization therefrom- References Cited in the file of this patent UNITED STATES PATENTS Great Britain of 1904
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
United States Patent P PRODUCTION OF AN ALKALI METAL DOUBLE FLUORIDEOF TITANIUM Eugene Wainer, Cleveland Heights, Ohio, assignor, by mesne assignments, to Horizons Titanium Corporation, Princeton, N. J., a corporation of New Jersey No Drawing. Application February 4, 1952, i Serial No. 269,695 r Claims. CI. 23-88 In the production and use of compounds of titanium,
and particularly the fluoride compounds, a serious disadcompactly workable process may be had, with elimination of losses heretofore serious. Other objects and advantages will appear from the following description.
To the accomplishment of the foregoing and related ends, said invention then comprises the features hereinafter fully described and particularly pointed out in the claims, the following description setting forth in detail certain illustrative embodiments of the invention, these being indicative, however, of but a few of the various ways in which the principle of the invention may be employed.
In general, the invention involves cycling thealkali metal component for compound fluorides of titanium through zones reacting alkali metal fluoride with a titanium. compound to formation of double fluoride, and
, a zone decomposing such double fluoride to titanium metal and alkali fluoride, and then to such first reaction zone to form double fluoride. Thus, by-product alkali fluoride otherwise left by decomposing a double fluoride of titanium is recycled to the reaction zone forming double The titanium compounds as raw material for preparation of titanium double fluoride are such raw materials as ilmenite and other ores of titanium, more or less purified oxide of titanium, meta-titanic acids, slags containing high percentages of titanium dioxide, titanium sulfates, and the like. For the alkali metal fluoride component, it will be understood that this comprises metals of the alkali group, potassium and sodium being preferred, and the term alkali fluoride concisely designates all these hereinafter.
The double fluoride of titanium and alkali metal is subjected to decomposition in a decomposing zone to form titanium metal, and the alkali fluoride is a byproduct. While the decomposition of the double fluoride may be carried out by heat reaction, electrolysis is here more generally involved and in presence of chlorine, and as the details are not a part of the present invention, it is here suflicient to state that the compound fluoride of titanium and alkali metal as afore-mentioned, is decomposed to metallic titanium and fluorides such as of potassium and sodium. It is such latter material that is then recycled to the formation of double fluoride of titanium and alkali metal.
With a raw material such as ilmenite, a desirable procedure is to reduce the iron content to the ferrous state, either by heating in the presence of carbon (finely divided, or a reducing gas or reducing furnace atmosphere) or by addition of scrap iron and sulfuric acid. If the amount of the sulfuric acid is sufficient to react with all of the constituents of the ilmenite, there results titanium sulfate and iron sulfate solution. After such reaction is "ice completed, the solution is diluted and the insolubles such as silicates, etc., are removed by settling, decantation, filtration, and the like. To the combined titanium iron sulfate solution there is then admixed the alkali metal fluoride as from the afore-mentioned decomposition of double fluoride of titanium and alkali metal. Thus, where the decomposition has been in an electrolytic zone, the alkali fluoride remaining from the electrolysis is recycled to the zone reacting'titanium compound with alkali metal fluoride in the first instance. Usually, an electrolytic bath based on double fluoride of titanium, together with a molten bath constituent of halide, a chloride of alkali or alkaline earth metal (i. e., K, Na, Li, Sr, Ba, or mixtures, and preferably sodium chloride), after the electrolysis consists of potassium fluoride and sodium fluoride. Thus, with a bath in the first instance of potassium titanium fluoride and a sodium chloride bath component subjected to electrolysis, the decomposition may be generally represented by the following equation:
electrolysis lllustratively also, the reaction of sulfuric acid on the ilmenite as above-mentioned may be represented by the following equation:
2. FeO.TiO2+3H2SO4- Ti (S04 2+FeSO4+ 3H2O The combined titanium iron sulfate solution is treated with the constituents remaining from the decomposition or electrolysis, viz., the alkalimetal fluorides. Usually these will include sodium chloride which has not been In the presence of varying amounts of sodium chloride, somewhat better results are obtained if roughly two-thirds of the total fluorine requirement to make double fluoride, in the form of the mixed potassium sodium fluoride salts isfirst added to the titanium sulfate solution in dissolved 1 form, and then if any precipitate occurs it is removed by filtration. The reaction of the sulfuric acid on the ilmenite in the first instance, involves raised temperature, and to the clear hot liquor, after filtration, the remaining fluoride requirement is added. Reaction occurs, and then the solution is evaporated down until crystals appear, and potassium titanium fluoride thus separates out. This potassium titanium fluoride is then re-dissolved and recrystallized, and made up for electrolysis with further sodium chloride, and is again subjected to decomposition. Chlorine is evolved, but fluorine is not. Thus, the prooess is completely cyclical, and the only losses are the minor losses normally encountered in properly controlled chemical operation. Costly fluorine is conserved and cycled through the respective reaction zones.
Instead of operating batch-wise in decomposition for electrolysis of the double fluoride of titanium and alkali metal, in some cases a continuous type of operation may be applied, removing molten bath material from the reaction zone as the process proceeds, this being possible by reason of the fact that the titanium metal formed is segregated at the cathode.
Illustratively, then, with ilmenite as the starting material, the only raw materials which are consumed in the operation are ilmenite, sulfuric acid, and the sodium chloride or alkali metal halide bath component, and the entire operation may be summarized illustratively by the following equation:
4. FeO.TiO2l-3H2SO4+4NaCl- I In similar manner, other raw materials than ilmenite,
,and other alkali metal bath halide components apply in the same general way.
As an example: Ilmenite, finely ground, is reacted upon .with sulfuric acid solution in amount to substantially completely dissolve it. Any insolubles are eliminated. The
, reaction involves raised temperature, and to the clear hot solution, there is then added alkali metal fluorides, KF and NaF from the electrolysis of potassium titanium fluoride, in proportions of one mole of titanium sulfate and 2 until crystals begin to appear, and then on cooling, the
. potassium titanium fluoride separates out, and is removed by filtration. It is then re-dissolved and re-crystallized, I and mixed with sodium chloride in about the proportions And later with voltage increased to 5-8, and current density 200-500 amp., titanium metal sponge is deposited in a tightly adhering mass at the cathode, and the potassium fluoride isby-product for recycling to the production of potassium titanium fluoride.
Other modes of applying the principle of the invention may be employed, change being made as regards the details described provided the features stated in any of the following claims, or the equivalent of such, be employed.
I therefore particularly point out and distinctly claim as my invention:
. 1. The method of producing an alkali metal fluotitanate .which comprises digesting an oxidicore of titanium in sulfuric acid to produce a solution containing titanium ions, effecting separation of any insoluble phase from the solution, reacting the said solution with a source of fiuo- Y ride ions and of alkali metal ions consisting essentially of the spent salt bath resulting from the electrolytic decomposition of an alkali metal fluotitanate in a fused alkali metal halide bath and crystallizing from said solution the resulting alkali metal fluotitanate.
2. The method of producing an alkali metal fluotitanate which comprises digesting ilmenite in sulfuric acid, efiecting separation of any insoluble phase from the resulting aqueous solution reacting the aqueous solution so obtained which comprises digesting an oxidic ore of titanium in sulmoles of potassium fluoride and 4 moles of sodium fluoride, with slight excess. The solution is then evaporated furic acid to produce a solution containing titanium ions, separating any insoluble phase from the solution produced, reacting the solution with a source of fluoride ions and potassium ions consisting esentially of the spent salt bath resulting from the electrolytic decomposition of potassium fluotitanate in a fused alkali metal halide bath and recovering potassium fiuotitanate from the resulting solution by crystallization.
4. The method of producing potassium fluotitanate from ilmenite which comprises reducing the iron content of the ilmenite to ferrous iron, digesting the resulting material in sulfuric acid to produce an aqueous solution containing titanium ions, separating insoluble materials therefrom, reacting the remaining aqueous solution with a source of fluorine ions and potassium ions consisting essentially of the spent salt bath resulting from the electrolytic decomposition of potassium fluotitanate in a fused alkali metal halide bath and recovering potassium fluotitanate from the resulting solution by crystallization therefrom.
5. The method of producing potassium fluotitanate from ilmenite which comprises reducing the iron content of the ilmenite to ferrous iron, digesting the resulting material in sulfuric acid to produce an aqueous solution containing titanium ions, separatiing any insoluble materials therefrom, reacting the remaining aqueous solution with a source of fluorine ions and potassium ions in the proportion of one mole of KF to two mols of NaF consisting essentially of the spent salt bath resulting from the electrolytic decomposition of potassium fluotitanate in a fused sodium chloride bath and recovering potassium fluotitanate from the resulting solution by crystallization therefrom- References Cited in the file of this patent UNITED STATES PATENTS Great Britain of 1904
Claims (1)
1. THE METHOD OF PRODUCING AN ALKALI METAL FLUOTITANATE WHICH COMPRISES DIGESTING AN OXIDE ORE OF TITANIUM IN SULFURIC ACID TO PRODUCE A SOLUTION CONTAINING TITANIUM IONS, EFFECTING SEPARATION OF ANY INSOLUBLE PHASE FROM THE SOLUTION, REACTING THE SAID SOLUTION WITH A SOURCE OF FLUORIDE IONS AND OF ALKALI METAL IONS CONSISTING ESSENTIALLY OF THE SPENT SALT BATH RESULTING FROM THE ELECTROYLTIC DECOMPOSITION OF AN ALKALI METAL FLUOTITANATE IN A FUSED ALKALI METAL HALIDE BATH AND CRYSTALLIZING FROM SAID SOLUTION THE RESULTING ALKALI METAL FLUOTITANATE.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US269695A US2724635A (en) | 1952-02-04 | 1952-02-04 | Production of an alkali metal double fluoride of titanium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US269695A US2724635A (en) | 1952-02-04 | 1952-02-04 | Production of an alkali metal double fluoride of titanium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2724635A true US2724635A (en) | 1955-11-22 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US269695A Expired - Lifetime US2724635A (en) | 1952-02-04 | 1952-02-04 | Production of an alkali metal double fluoride of titanium |
Country Status (1)
| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2832731A (en) * | 1955-12-15 | 1958-04-29 | Horizons Titanium Corp | Preparation of alkali metal-titanium fluorides |
| US2900234A (en) * | 1957-02-11 | 1959-08-18 | Allied Chem | Manufacture of titanium tetrafluoride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB190413759A (en) * | 1903-06-18 | Borchers Wilhelm | Process for the Production of Titanium from its Oxygen Compounds Electrolytically. | |
| US1815054A (en) * | 1928-05-04 | 1931-07-21 | Westinghouse Lamp Co | Method of producing tantalum and other rare refractory metals by electrolysis of fused compounds |
| US2031554A (en) * | 1933-04-05 | 1936-02-18 | Alais & Froges & Camarque Cie | Recovery of the gases and dust evolved in the electrolytic manufacture of aluminium |
| US2465287A (en) * | 1947-07-15 | 1949-03-22 | Redler Conveyor Co | Conveyer |
-
1952
- 1952-02-04 US US269695A patent/US2724635A/en not_active Expired - Lifetime
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB190413759A (en) * | 1903-06-18 | Borchers Wilhelm | Process for the Production of Titanium from its Oxygen Compounds Electrolytically. | |
| US1815054A (en) * | 1928-05-04 | 1931-07-21 | Westinghouse Lamp Co | Method of producing tantalum and other rare refractory metals by electrolysis of fused compounds |
| US2031554A (en) * | 1933-04-05 | 1936-02-18 | Alais & Froges & Camarque Cie | Recovery of the gases and dust evolved in the electrolytic manufacture of aluminium |
| US2465287A (en) * | 1947-07-15 | 1949-03-22 | Redler Conveyor Co | Conveyer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2832731A (en) * | 1955-12-15 | 1958-04-29 | Horizons Titanium Corp | Preparation of alkali metal-titanium fluorides |
| US2900234A (en) * | 1957-02-11 | 1959-08-18 | Allied Chem | Manufacture of titanium tetrafluoride |
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