US2714564A - Production of metallic titanium - Google Patents
Production of metallic titanium Download PDFInfo
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- US2714564A US2714564A US20592A US2059248A US2714564A US 2714564 A US2714564 A US 2714564A US 20592 A US20592 A US 20592A US 2059248 A US2059248 A US 2059248A US 2714564 A US2714564 A US 2714564A
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- titanium
- tetraiodide
- metallic
- carbide
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 71
- 229910052719 titanium Inorganic materials 0.000 title claims description 71
- 239000010936 titanium Substances 0.000 title claims description 71
- 238000004519 manufacturing process Methods 0.000 title description 11
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical group I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 claims description 48
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 38
- 239000011630 iodine Substances 0.000 claims description 23
- 229910052740 iodine Inorganic materials 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 19
- 230000009471 action Effects 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 10
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 230000006872 improvement Effects 0.000 claims description 4
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 30
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 22
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 16
- 238000010494 dissociation reaction Methods 0.000 description 11
- 230000005593 dissociations Effects 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 11
- 230000009467 reduction Effects 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 239000003575 carbonaceous material Substances 0.000 description 8
- 239000004408 titanium dioxide Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 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 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1281—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using carbon containing agents, e.g. C, CO, carbides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/129—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds by dissociation, e.g. thermic dissociation of titanium tetraiodide, or by electrolysis or with the use of an electric arc
Definitions
- This invention relates to the production of metallic titanium and has for an object the provision of an improved method or process for producing high-purity metallic titanium. More particularly, the invention contemplates the provision of an improved method or process for producing high-purity metallic titanium by dissociation of titanium tetraiodide.
- titanium dioxide is subjected to a suitable treatment which will convert the titanium to a form in which it is capable of reacting with iodine to produce titanium tetraiodide.
- the titanium of the titanium dioxide may be converted into such a suitable form by reduction to the metallic state. Reduction of the titanium of the titanium dioxide is carried out by means of non-carbonaceous reducing agents such as sodium, calcium, magnesium, silicon and aluminum.
- the metallic titanium produced by reduction of titanium dioxide with a non-carbonaceous reducing agent can be used to produce titanium tetraiodide. I have found, however, that reduction with carbon produces a product which provides a better reaction material and which is less expensive than the product resulting from reduction by means of non-carbonaceous reducing agents.
- Titanium carbide can be produced by heating a mixture of titanium and carbon to a temperature of about 105 C. at atmospheric pressures, but the reaction is slow and can be made to go to completion only with drfiiculty. Incompletely reduced material does not react readily with iodine. Therefore, I prefer to carry out the reduction with carbon at a higher temperature. I have found that a highly reactive titanium carbide product maybe obtained by carrying out the reduction at temperatures in the range 1300 C. to 1800 C. At temperatures in the lower portion of the range, I prefer to effect the heating and reduction under a vacuum. Products formed at the lower temperatures under reduced pressures are more highly reactive than products formed at higher temperatures under atmospheric pressure. Thus, for example, titanium carbide formed at 1300 C.
- under vacuum may be as much as ten percent more reactive than titanium carbide formed at 1800 C. under atmospheric pressure.
- the advantage of greater reactivity may be offset to some extent by the cost and inconvenience of operating under a vacuum.
- An electric resistance furnace of the type employed in producing silicon carbide may be employed advantageously in carrying out the reduction of titanium with carbon and the production of titanium carbide.
- the titanium carbide produced is subjected to the action of iodine vapor at an elevated temperature. I have found that the rate of reaction reaches a maximum at 1100 C. and falls off at lower and higher temperatures.
- titanium dioxide is heated to a temperature in the neighborhood of 1800 C. at atmospheric pressure in the presence of sufiicient carbon to combine with all of the oxygen of the titanium dioxide to reduce the titanium and with all of the reduced titanium to form titanium carbide.
- the titanium carbide thus produced is subjected to the action of elemental iodine in vapor form at a temperature of about 1100 C. to produce a gaseous product containing titanium tetraiodide.
- the titanium tetraiodide of the gaseous product thus produced is contacted with a surface heated to and maintained at a temperature in the range 1100 C. to 1700 C.
- the gaseous product containing titanium tetraiodide resulting from treatment of titanium carbide with iodine may be treated for the separation of impurities and the production of pure titanium tetraiodide if necessary. Such treatment may include fractional condensation or complete cooling and condensation followed by tractional distillation to produce pure titanium tetraiodide. If the gaseous product is free of impurities, it may be passed directly into contact with the heated surface without any substantial reduction of temperature or loss of heat.
- the deposition surface may be formed of tungsten or titanium or other suitable material, and it may be heated in any suitable manner.
- the elemental iodine resulting from dissociation of the titanium tetraiodide is returned to the process and utilized in the treatment of additional titanium carbide.
- the titanium tetraiodide is contacted with the heated surface at a pressure not higher than about 30 mm.
- a method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material comprising treating the crude titanium-bearing material to produce a titanium carbide product subjecting titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated surface at a temperature in the range 1100 C. to 1700 C. to effect decomposition of the titanium tetraiodide and deposition of metallic titanium on the heated surface.
- a method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material comprising treating the crude titanium-bearing material to produce a titanium carbide product subjecting titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated surface at a temperature in the range 1100 C. to 1700 C. to effect decomposition of the titanium tetraiodide and deposition of metallic titanium on the heated surface.
- a method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material comprising treating the crude titanium-bearing material to produce a titanium carbide product subjecting titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to form a gaseous product comprising titanium tetraiodide, collecting and condensing the gaseous product, and contacting the titanium tetraiodide in vapor form with a heated surface at a temperature in the range 1100 C. to 1700 C. to effect decomposition of the titanium tetraiodide and deposition of metallic titanium on the heated surface.
- the method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature in the presence of sufficient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide with the production of highpurity metallic titanium and with deposition of the metallic titanium thus produced on the heated body.
- the method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature in the presence of sufiicient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body at a 6.
- the method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature not substantially lower than 1800 C.
- the method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature below 1800" C. at a pressure below atmospheric pressure in the presence of sufficient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to form a gaseous product comprising titanium tetraiodide, collecting and condensing the gaseous product, and contacting the titanium tetraiodide in vapor form with a heated body at a temperature in the range 1100 C. to 1700 C. to efiect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and With deposition of the metallic titanium thus produced on the heated body.
- the method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature near 1300 C. under a high vacuum in the presence of suflicient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body.
- the method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature in the presence of sufficient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body of metallic titanium at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body of metallic titanium.
- the method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature in the presence of sufficient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to form a gaseous product comprising titanium tetraiodide, collecting and condensing the gaseous product, and contacting the titanium tetraiodide in vapor form with a heated body of metallic titanium at a temperature in the range 1100 C. to 1700 C. to eifect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body of metallic titanium.
- the method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature near 1300 C. under a high vacuum in the presence of suflicient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body of metallic titanium at a temperature in the range 1100 C. to 1700 C. to etfect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body of metallic titanium.
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- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
Description
PRGDUCT ION OF METALLIC TITANIUM Alfred C. Loonam, New York, N. Y., assignor to Chilean Nitrate Sales Corporation, New York, N. Y., a corporation of New York No Drawing. Application April 12, 1948, Serial No. 20,592
11 Claims. (Cl. 117-107) This invention relates to the production of metallic titanium and has for an object the provision of an improved method or process for producing high-purity metallic titanium. More particularly, the invention contemplates the provision of an improved method or process for producing high-purity metallic titanium by dissociation of titanium tetraiodide. I
In the preparation of titanium metal of high purity, it has been proposed to reduce a compound of titanium and produce a gaseous product containing titanium tetraiodide which is dissociated through contact with a heated surface to effect dissociation of the titanium and iodine of the titanium tetraiodide with deposition of the separated metallic titanium taking place.
In accordance with heretofore customary procedures, titanium dioxide is subjected to a suitable treatment which will convert the titanium to a form in which it is capable of reacting with iodine to produce titanium tetraiodide. The titanium of the titanium dioxide may be converted into such a suitable form by reduction to the metallic state. Reduction of the titanium of the titanium dioxide is carried out by means of non-carbonaceous reducing agents such as sodium, calcium, magnesium, silicon and aluminum.
The metallic titanium produced by reduction of titanium dioxide with a non-carbonaceous reducing agent can be used to produce titanium tetraiodide. I have found, however, that reduction with carbon produces a product which provides a better reaction material and which is less expensive than the product resulting from reduction by means of non-carbonaceous reducing agents.
I prefer to reduce the titanium of the titanium dioxide with carbon and produce titanium carbide, as I have found iodine will react with titanium carbide rapidly and efficiently at a temperature near 1100 C. I
Titanium carbide can be produced by heating a mixture of titanium and carbon to a temperature of about 105 C. at atmospheric pressures, but the reaction is slow and can be made to go to completion only with drfiiculty. Incompletely reduced material does not react readily with iodine. Therefore, I prefer to carry out the reduction with carbon at a higher temperature. I have found that a highly reactive titanium carbide product maybe obtained by carrying out the reduction at temperatures in the range 1300 C. to 1800 C. At temperatures in the lower portion of the range, I prefer to effect the heating and reduction under a vacuum. Products formed at the lower temperatures under reduced pressures are more highly reactive than products formed at higher temperatures under atmospheric pressure. Thus, for example, titanium carbide formed at 1300 C. under vacuum may be as much as ten percent more reactive than titanium carbide formed at 1800 C. under atmospheric pressure. The advantage of greater reactivity may be offset to some extent by the cost and inconvenience of operating under a vacuum. Normally, I prefer to operate under atmospheric pressure at a high temperature in the neighborhood of 1800 C. in view of the large quantities of gas protates atent duced in the reaction. An electric resistance furnace of the type employed in producing silicon carbide may be employed advantageously in carrying out the reduction of titanium with carbon and the production of titanium carbide.
In order to limit contamination of the titanium carbide, I prefer to employ petroleum coke or charcoal as the reducing agent.
The titanium carbide produced is subjected to the action of iodine vapor at an elevated temperature. I have found that the rate of reaction reaches a maximum at 1100 C. and falls off at lower and higher temperatures.
In carrying out the reaction between iodine and titaniumcarbide at the higher temperatures, I prefer to employ a furnace lined with graphite, as the results of my investi gations indicate that graphite is not attacked at any temperature by iodine vapor. I prefer, also, to employ electrical resistance heating because of ease of control, efiiciency and the absence of any gaseous products of combustion which, if present, might contaminate the titanium tetraiodide produced.
According to a complete process of the invention, titanium dioxide is heated to a temperature in the neighborhood of 1800 C. at atmospheric pressure in the presence of sufiicient carbon to combine with all of the oxygen of the titanium dioxide to reduce the titanium and with all of the reduced titanium to form titanium carbide. The titanium carbide thus produced is subjected to the action of elemental iodine in vapor form at a temperature of about 1100 C. to produce a gaseous product containing titanium tetraiodide. The titanium tetraiodide of the gaseous product thus produced is contacted with a surface heated to and maintained at a temperature in the range 1100 C. to 1700 C. Contact of the titanium tetraiodide with the heated surface results in dissociation of the titanium tetraiodide into elemental or metallic titanium and elemental iodine and deposition on the heated surface of the metallic titanium in a high state of purity.
The gaseous product containing titanium tetraiodide resulting from treatment of titanium carbide with iodine may be treated for the separation of impurities and the production of pure titanium tetraiodide if necessary. Such treatment may include fractional condensation or complete cooling and condensation followed by tractional distillation to produce pure titanium tetraiodide. If the gaseous product is free of impurities, it may be passed directly into contact with the heated surface without any substantial reduction of temperature or loss of heat.
The deposition surface may be formed of tungsten or titanium or other suitable material, and it may be heated in any suitable manner.
The elemental iodine resulting from dissociation of the titanium tetraiodide is returned to the process and utilized in the treatment of additional titanium carbide.
Preferably, the titanium tetraiodide is contacted with the heated surface at a pressure not higher than about 30 mm.
I claim:
1. In a method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material, the improvement which comprises treating the crude titanium-bearing material to produce a titanium carbide product subjecting titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated surface at a temperature in the range 1100 C. to 1700 C. to effect decomposition of the titanium tetraiodide and deposition of metallic titanium on the heated surface.
2. In a method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material, the improvement which comprises treating the crude titanium-bearing material to produce a titanium carbide product subjecting titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated surface at a temperature in the range 1100 C. to 1700 C. to effect decomposition of the titanium tetraiodide and deposition of metallic titanium on the heated surface.
3. In a method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material, the improvement which comprises treating the crude titanium-bearing material to produce a titanium carbide product subjecting titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to form a gaseous product comprising titanium tetraiodide, collecting and condensing the gaseous product, and contacting the titanium tetraiodide in vapor form with a heated surface at a temperature in the range 1100 C. to 1700 C. to effect decomposition of the titanium tetraiodide and deposition of metallic titanium on the heated surface.
4. The method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature in the presence of sufficient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide with the production of highpurity metallic titanium and with deposition of the metallic titanium thus produced on the heated body.
5. The method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature in the presence of sufiicient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body at a 6. The method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature not substantially lower than 1800 C. at atmospheric pressure in the presence of suflicient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to form a gaseous product comprising titanium tetraiodide, collecting and condensing the gaseous product, and contacting the titanium tetraiodide in vapor form with a heated body at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body.
7. The method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature below 1800" C. at a pressure below atmospheric pressure in the presence of sufficient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to form a gaseous product comprising titanium tetraiodide, collecting and condensing the gaseous product, and contacting the titanium tetraiodide in vapor form with a heated body at a temperature in the range 1100 C. to 1700 C. to efiect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and With deposition of the metallic titanium thus produced on the heated body.
8. The method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature near 1300 C. under a high vacuum in the presence of suflicient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body.
9. The method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature in the presence of sufficient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body of metallic titanium at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body of metallic titanium.
10. The method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature in the presence of sufficient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature near 1100 C. to form a gaseous product comprising titanium tetraiodide, collecting and condensing the gaseous product, and contacting the titanium tetraiodide in vapor form with a heated body of metallic titanium at a temperature in the range 1100 C. to 1700 C. to eifect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body of metallic titanium.
11. The method of recovering titanium in the form of a high-purity metallic product from titanium oxide which comprises heating the titanium oxide to an elevated temperature near 1300 C. under a high vacuum in the presence of suflicient carbonaceous material to reduce titanium of the oxide and form titanium carbide, subjecting the titanium carbide to the action of gaseous iodine at an elevated temperature to produce titanium tetraiodide, and contacting the titanium tetraiodide in vapor form with a heated body of metallic titanium at a temperature in the range 1100 C. to 1700 C. to etfect dissociation of the titanium tetraiodide with the production of high-purity metallic titanium and with deposition of the metallic titanium thus produced on the heated body of metallic titanium.
References Cited in the file of this patent UNITED STATES PATENTS 1,497,417 Weber June 10, 1924 1,671,213 Van Arkel et al May 29, 1928 1,891,124 Van Arkel et al. Dec. 13, 1932 2,237,503 Ridgeway Apr. 8, 1941 2,393,264 Rentschler et al Jan. 22, 1946
Claims (1)
1. IN A METHOD OF RECOVERING TITANIUM IN THE FORM OF A HIGH-PURITY METALLIC PRODUCT FROM CRUDE TITANIUM-BEAR-. ING MATERIAL, THE IMPROVEMENT WHICH COMPRISES TREATING THE CRUDE TITANIUM-BEARING MATERIAL TO PRODUCE A TITANIUM CARBIDE PRODUCT SUBJECTING TITANIUM CARBIDE TO THE ACTION OF GASEOUS IODINE AT AN ELEVATED TEMPERATURE TO PRODUCE TAINING SAID COMMINUTED MATERIAL INTO AN ELONGATED BARREL IODIDE IN VAPOR FORM WITH A HEATED SURFACE AT A TEMPERATURE IN THE RANGE 1100* C. TO 1700* C. TO EFFECT DECOMPOSITION OF THE TITANIUM TETRAIODIDE AND DEPOSITION OF METALLIC TITANIUM ON THE HEATED SURFACE.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US20592A US2714564A (en) | 1948-04-12 | 1948-04-12 | Production of metallic titanium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US20592A US2714564A (en) | 1948-04-12 | 1948-04-12 | Production of metallic titanium |
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| Publication Number | Publication Date |
|---|---|
| US2714564A true US2714564A (en) | 1955-08-02 |
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| US20592A Expired - Lifetime US2714564A (en) | 1948-04-12 | 1948-04-12 | Production of metallic titanium |
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| US (1) | US2714564A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2885281A (en) * | 1954-11-22 | 1959-05-05 | Mallory Sharon Metals Corp | Method of producing hafnium-free "crystal-bar" zirconium from a crude source of zirconium |
| US3107179A (en) * | 1959-09-21 | 1963-10-15 | Wilbur M Kohring | Process for making carbon-metal resistors |
| US3243174A (en) * | 1960-03-08 | 1966-03-29 | Chilean Nitrate Sales Corp | Dissociation-deposition apparatus for the production of metals |
| US9816192B2 (en) * | 2011-12-22 | 2017-11-14 | Universal Technical Resource Services, Inc. | System and method for extraction and refining of titanium |
| US10400305B2 (en) | 2016-09-14 | 2019-09-03 | Universal Achemetal Titanium, Llc | Method for producing titanium-aluminum-vanadium alloy |
| US11959185B2 (en) | 2017-01-13 | 2024-04-16 | Universal Achemetal Titanium, Llc | Titanium master alloy for titanium-aluminum based alloys |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1497417A (en) * | 1919-03-31 | 1924-06-10 | Henry C P Weber | Process of coating metals |
| US1671213A (en) * | 1925-03-14 | 1928-05-29 | Philips Nv | Process of precipitaing metals on an incandescent body |
| US1891124A (en) * | 1928-06-14 | 1932-12-13 | Philips Nv | Process of precipitating metals on an incandescent body |
| US2237503A (en) * | 1937-04-19 | 1941-04-08 | Norton Co | Titanium carbide and a method of making the same |
| US2393264A (en) * | 1942-09-23 | 1946-01-22 | Westinghouse Electric Corp | Photoelectric device and the manufacture thereof |
-
1948
- 1948-04-12 US US20592A patent/US2714564A/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1497417A (en) * | 1919-03-31 | 1924-06-10 | Henry C P Weber | Process of coating metals |
| US1671213A (en) * | 1925-03-14 | 1928-05-29 | Philips Nv | Process of precipitaing metals on an incandescent body |
| US1891124A (en) * | 1928-06-14 | 1932-12-13 | Philips Nv | Process of precipitating metals on an incandescent body |
| US2237503A (en) * | 1937-04-19 | 1941-04-08 | Norton Co | Titanium carbide and a method of making the same |
| US2393264A (en) * | 1942-09-23 | 1946-01-22 | Westinghouse Electric Corp | Photoelectric device and the manufacture thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2885281A (en) * | 1954-11-22 | 1959-05-05 | Mallory Sharon Metals Corp | Method of producing hafnium-free "crystal-bar" zirconium from a crude source of zirconium |
| US3107179A (en) * | 1959-09-21 | 1963-10-15 | Wilbur M Kohring | Process for making carbon-metal resistors |
| US3243174A (en) * | 1960-03-08 | 1966-03-29 | Chilean Nitrate Sales Corp | Dissociation-deposition apparatus for the production of metals |
| US9816192B2 (en) * | 2011-12-22 | 2017-11-14 | Universal Technical Resource Services, Inc. | System and method for extraction and refining of titanium |
| US10066308B2 (en) | 2011-12-22 | 2018-09-04 | Universal Technical Resource Services, Inc. | System and method for extraction and refining of titanium |
| US10731264B2 (en) | 2011-12-22 | 2020-08-04 | Universal Achemetal Titanium, Llc | System and method for extraction and refining of titanium |
| US11280013B2 (en) | 2011-12-22 | 2022-03-22 | Universal Achemetal Titanium, Llc | System and method for extraction and refining of titanium |
| US10400305B2 (en) | 2016-09-14 | 2019-09-03 | Universal Achemetal Titanium, Llc | Method for producing titanium-aluminum-vanadium alloy |
| US11959185B2 (en) | 2017-01-13 | 2024-04-16 | Universal Achemetal Titanium, Llc | Titanium master alloy for titanium-aluminum based alloys |
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