US2826493A - Method of producing titanium - Google Patents
Method of producing titanium Download PDFInfo
- Publication number
- US2826493A US2826493A US497322A US49732255A US2826493A US 2826493 A US2826493 A US 2826493A US 497322 A US497322 A US 497322A US 49732255 A US49732255 A US 49732255A US 2826493 A US2826493 A US 2826493A
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- Prior art keywords
- titanium
- molten
- metal
- sodium
- alkali metal
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 55
- 239000010936 titanium Substances 0.000 title claims description 54
- 229910052719 titanium Inorganic materials 0.000 title claims description 54
- 238000000034 method Methods 0.000 title description 17
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 27
- 229910052783 alkali metal Inorganic materials 0.000 claims description 18
- 150000001340 alkali metals Chemical class 0.000 claims description 18
- 230000009467 reduction Effects 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 description 31
- 239000002184 metal Substances 0.000 description 31
- 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 21
- 229910052708 sodium Inorganic materials 0.000 description 21
- 239000011734 sodium Substances 0.000 description 21
- 238000006722 reduction reaction Methods 0.000 description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 18
- 239000011780 sodium chloride Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 150000002739 metals Chemical class 0.000 description 7
- 239000000376 reactant Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 229910001514 alkali metal chloride Inorganic materials 0.000 description 5
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 150000004820 halides Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Chemical compound CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- -1 for example Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
Images
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
- C22B34/1268—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 alkali or alkaline-earth metals or amalgams
- C22B34/1272—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 alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
Definitions
- This invention relates to a method of producing reactive metals of groups IV, V and VI of the periodic table. More particularly the invention relates to a process for producing titanium metal.
- Vapor phase reactions lead to the deposition of products on nozzles and other parts of the equipment which makes control of the reaction and product removal more difiicult. Agitation of the reactants is complicated by the formation of solid products that interfere with the operation of mechanical agitators.
- the objects of the invention are accomplished by the reduction in -two stages of a halide of the metal to be produced.
- the halide is reduced to subhalides with a molten reducing metal.
- the subhalides are reduced to the metallic state by the further addition of molten reducing metal in an amount sutficient to provide the stoichiometric amount of reducing metal required to react with the halide.
- An inert or non-contaminating atmosphere is maintained throughout the reduction.
- the subject invention provides a method for the production of the designated metals that overcomes in great measure the difliculties and hazards encountered heretofore. Additionally, segregation and localized heating are virtually eliminated, and improved utilization of the reactants is realized.
- the reduction reaction is carried out in two stages These stages may be performed with or without intermediate delay and may be carried out in the same or diiferent reactors.
- molten alkali metal and titsnium tetrachloride are placed in a reactor.
- the amount of alkali metal used in this stage is insufficient to reduce the titanium tetrachloride to titanium.
- the titanium tetra- 70 chloride is reduced to subchlorides of titanium while an alkali metal chloride is simultaneously formed.
- the subchlorides are subsequently reduced, producing titanium metal and additional quantities of alkali metal chloride, by injecting molten alkali metal into the bath of titanium subchlon'des and alkali metal chlorides.
- An inert or non-contaminating atmosphere for example argon, is maintained throughout the reduction, and the alkali chloride and reactants are maintained in a molten state.
- a metallic reaction chamber 1 is provided in its upper portion with a feed line 2 terminating in a nozzle 3.
- a feed line for molten reducing metal 4 terminating in a nozzle 5.
- the feed line 4 may extend from the top of the chamber in which event provision may be made to lower it into the reactants if desired.
- a drain line 6 is provided for withdrawing the molten chlorides.
- the reduction of titanium tetrachloride with sodium will be de scribed.
- the reactor 1 is purged of air and filled with a non-contaminating gas, for example, argon.
- the reactor 1 is then charged with a quantity of molten sodium throng-h feed line 4 and nozzle 5.
- the temperature is maintained at a level above the melting point of the sodium.
- Approximately twice the stoichiometric quantity of titanium tetrachloride is injected at high velocity into the bath of molten sodium through feed line 2 and nozzle 3.
- the remaining sodium in a quantity sufficient to completely react with the chloride present in the reactor 1, is injected, for example, through a nozzle 5 immersed, for example, within the bath.
- the greater part of the resulting sodium chloride may then be drained from the reactor. Any remaining sodium chloride may be removed from the titanium metal formedin the reactor by conventional methods such as leaching or vacuum distillation.
- the injection velocity of the refractory metal halide may be between about 0.1 and 200 feet per second, and of the molten alkali metal in the second stage of the reduction at a velocity of between about 0.1 and feet per second. Relatively high velocities are preferred since the agitation of the reactants is promoted thereby.
- Example I About 97 pounds of sodium metal were charged in the liquid state to the reactor in an atmosphere of substantially pure argon. The metal bath was raisedto a temperature of approximately 400 C. About 416 pounds of titanium tetrachloride, approximately twice the quantity of titanium tetrachloride need to react stoichiometrically with the sodium metal to form titanium, were injected into the metal bath at a velocity of from 3 to 20 feet per second through a nozzle located in the lid of the reactor. During this injection period the temperature of the reacting bath slowly increases heating the reactor walls to approximately 850 C. After the feeding of the titanium tetrachloride was completed, 105 pounds of liquid sodium, the amount required to react stoichiometrically with the titanium compounds, were injected into the mixture.
- This injection was through a feed line located below the surface of the oath.
- the sodium traveled at a velocity of about 6 feet per second, and the temperature of the walls of the reactor was maintained between about 850 C. and 950 C.
- the contents of the reactor were then held at a temperature of between about 900 C. and 950 C. for two hours to permit the completion of the reactions.
- Much of the liquefied sodium chloride was drained leaving a mass of titanium sponge and some 'sodium chloride within the reactor. The remaining sodium chloride was removed by leaching.
- the titanium metal was found to have or ceptional purity, containing less than 0.15% oxygen, 0.03% nitrogen and 0.10% chlorine.
- Example II Sodium metal in the amount of 6.86 pounds and sodium chloride in the amount of 17.5 pounds were heated in an argon-filled reaction chamber to 850 C. Titanium tetrachloride in the amount of 28 pounds was injected into the molten bath at a velocity of about 60 feet per second through a nozzle located in the lid of the chamber. After the feeding of the titanium tetrachloride was completed, 7 pounds of molten sodium metal were injected into the mixture of molten chlorides through a second sodium feed line located above the surface of the bath at a velocity of 125 feet persecond. Upon the separation of the sodium chloride from the titanium metal, the metal was found to be of good quality and high purity.
- the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a'stream of titanium tetrachloride at high velocity into a bath of molten alkali metal at a rate and in amount in excess of that which the alkali metal can reduce to titanium so as to avoid the formation of titanium metal at this stage, and then injecting at high velocity into the thus formed molten titanium subchloride a further amount of molten alkali metal sufiicient to reduce the molten subchloride to the metallic state.
- the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a stream of titanium tetrachloride at high velocity into a bath of molten alkali metal at a rateiand in amount in excess of that which the alkali metal can reduce to titanium so as to avoid the formation of titanium metal at this stage, and then injecting at high velocity into the thus formed molten titanium subchloride a fur ther amount of molten alkali metal sufiicient to reduce the molten subchloride to the metallic state, said reductions being effected in a substantially non-contaminating atmosphere.
- the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a stream of titanium tetrachloride at high velocity into a bath of molten sodium at a rate and in amount in excess of that which the sodium can reduce to titanium so as to avoid the formation of titanium metal at this stage, and then injecting at high velocity into the thus formed molten titanium subchloride a further amount of molten sodium sufficient to reduce the molten subchloride to the metallic state.
- the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a stream of titanium tetrachloride at high velocity into a bath of molten sodium at a rate and in amount in excess of that which the sodium can reduce to titanium so as to avoid the formation of titanium metal at this stage, and then injecting at high velocity into the thus formed molten titanium subchloride a further amount of molten sodium sufficient to reduce the I molten subchloride to the metallic state, said reductions being effected in a substantially non-contaminatingatmosphere.
- the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a stream of titanium tetrachloride at high ve locity into a bath of molten sodium at a rate and in amount in excess of that which the sodium can reduce to titanium so as to avoid the formation of titanium metal at this'stage, and then injecting at high velocity into the thus formed molten titanium subchloride a further amount of molten sodium suflicient to reduce the molten subchloride to the metallic state, said reductions being effected in a substantially non-contaminating atmosphere and at a temperature not greater than 950 C.
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- Environmental & Geological Engineering (AREA)
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
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Description
' March 11, 1958 F w. GARRETT EI'AL 2,826,493
METHOD OF PRODUCING TITANIUM Filed March 28, 1955 Drain INVENTORS FREDERICK W. GARRETT ROBERT A.SKIM|N BY ORNEY 7" States 2,826,493 Patented Mar. 11, 1958 METHOD OF PRODUCING TITANIUM Frederick W. Garrett, Niagara Falls, Ontario, Canada, and Robert A. Skimin, Niagara Falls, N. Y., assignors to Union Carbide Corporation, a corporation of New York This invention relates to a method of producing reactive metals of groups IV, V and VI of the periodic table. More particularly the invention relates to a process for producing titanium metal.
Production of the metals'of groups IV, V and VI of the periodic table has long presented severe difiiculties. The most promising methods have been based on the reduction of a halide of the metal by one of the alkali metals. Although many procedures have been suggested for carrying out the basic reaction, and some have been employed on a semi-commercial scale, none of the pro cedures is without operational difficulties or hazards. The reduction reaction is exothermic in character and therefore the reactants must be brought together under carefully controlled conditions to achieve satisfactory results. Among the difliculties encountered with prior art techniques for the manufacture of metals like titanium is that of minimizing vaporization of the reactants. Vapor phase reactions lead to the deposition of products on nozzles and other parts of the equipment which makes control of the reaction and product removal more difiicult. Agitation of the reactants is complicated by the formation of solid products that interfere with the operation of mechanical agitators.
It is the object of this inventionto provide a method for producing reactive metals of groups IV, V and VI of the periodic table. it ,is a further object of this invention to I provide a successful method for producing such metals of high purity. Still another object is to provide a process for the productionof titanium of high purity.
Broadly the objects of the invention are accomplished by the reduction in -two stages of a halide of the metal to be produced. In the first stage the halide is reduced to subhalides with a molten reducing metal. In the second stage the subhalides are reduced to the metallic state by the further addition of molten reducing metal in an amount sutficient to provide the stoichiometric amount of reducing metal required to react with the halide. An inert or non-contaminating atmosphere is maintained throughout the reduction. i
The subject invention provides a method for the production of the designated metals that overcomes in great measure the difliculties and hazards encountered heretofore. Additionally, segregation and localized heating are virtually eliminated, and improved utilization of the reactants is realized.
According to the method of the invention, the reduction reaction is carried out in two stages These stages may be performed with or without intermediate delay and may be carried out in the same or diiferent reactors. For example, in the production of titanium metal following the teachings of the invention, molten alkali metal and titsnium tetrachloride are placed in a reactor. The amount of alkali metal used in this stage is insufficient to reduce the titanium tetrachloride to titanium. The titanium tetra- 70 chloride is reduced to subchlorides of titanium while an alkali metal chloride is simultaneously formed. The subchlorides are subsequently reduced, producing titanium metal and additional quantities of alkali metal chloride, by injecting molten alkali metal into the bath of titanium subchlon'des and alkali metal chlorides. An inert or non-contaminating atmosphere, for example argon, is maintained throughout the reduction, and the alkali chloride and reactants are maintained in a molten state. Certain efficiencies in the use of equipment may be realized by conducting the initial reduction in one relatively large chamber and the subsequent reduction of the subchlorides of titanium in a series of smaller vessels. Some advantage is obtained in providing a small amount of the alkali metal halide in the reactor initially to provide ample solvent for the refractory titanium subhalide.
The accompanying drawing is a schematic representation of an apparatus whereby the objects of the invention may be achieved.
In the drawing:
A metallic reaction chamber 1 is provided in its upper portion with a feed line 2 terminating in a nozzle 3. In the lower portion of the chamber is a feed line for molten reducing metal 4 terminating in a nozzle 5. Alternatively the feed line 4 may extend from the top of the chamber in which event provision may be made to lower it into the reactants if desired. A drain line 6 is provided for withdrawing the molten chlorides.
As an example of the practice of the invention the reduction of titanium tetrachloride with sodium will be de scribed. The reactor 1 is purged of air and filled with a non-contaminating gas, for example, argon. The reactor 1 is then charged with a quantity of molten sodium throng-h feed line 4 and nozzle 5. The temperature is maintained at a level above the melting point of the sodium. Approximately twice the stoichiometric quantity of titanium tetrachloride is injected at high velocity into the bath of molten sodium through feed line 2 and nozzle 3. This procedure will produce a mixture of titanium subchlorides and sodium chloride; It is thought that the titanium subchloride formed is either substantially TiCl or other titanium subchlorides dissolved in the alkali metal chloride, or complexes of these subchlorides and the alkali metal chloride. In any event the fluidity of the bath is not reduced and the melting point of the mixture is below that of pure sodium chloride. 7
After the injection of the titanium tetrachloride is completed the remaining sodium, in a quantity sufficient to completely react with the chloride present in the reactor 1, is injected, for example, through a nozzle 5 immersed, for example, within the bath. The greater part of the resulting sodium chloride may then be drained from the reactor. Any remaining sodium chloride may be removed from the titanium metal formedin the reactor by conventional methods such as leaching or vacuum distillation.
It has been determined that the injection velocity of the refractory metal halide may be between about 0.1 and 200 feet per second, and of the molten alkali metal in the second stage of the reduction at a velocity of between about 0.1 and feet per second. Relatively high velocities are preferred since the agitation of the reactants is promoted thereby.
Typical reductions illustrative of the method of the invention are as follows: a
Example I About 97 pounds of sodium metal were charged in the liquid state to the reactor in an atmosphere of substantially pure argon. The metal bath was raisedto a temperature of approximately 400 C. About 416 pounds of titanium tetrachloride, approximately twice the quantity of titanium tetrachloride need to react stoichiometrically with the sodium metal to form titanium, were injected into the metal bath at a velocity of from 3 to 20 feet per second through a nozzle located in the lid of the reactor. During this injection period the temperature of the reacting bath slowly increases heating the reactor walls to approximately 850 C. After the feeding of the titanium tetrachloride was completed, 105 pounds of liquid sodium, the amount required to react stoichiometrically with the titanium compounds, were injected into the mixture. This injection was through a feed line located below the surface of the oath. The sodium traveled at a velocity of about 6 feet per second, and the temperature of the walls of the reactor was maintained between about 850 C. and 950 C. The contents of the reactor were then held at a temperature of between about 900 C. and 950 C. for two hours to permit the completion of the reactions. Much of the liquefied sodium chloride was drained leaving a mass of titanium sponge and some 'sodium chloride within the reactor. The remaining sodium chloride was removed by leaching. The titanium metal was found to have or ceptional purity, containing less than 0.15% oxygen, 0.03% nitrogen and 0.10% chlorine.
Example II Sodium metal in the amount of 6.86 pounds and sodium chloride in the amount of 17.5 pounds were heated in an argon-filled reaction chamber to 850 C. Titanium tetrachloride in the amount of 28 pounds was injected into the molten bath at a velocity of about 60 feet per second through a nozzle located in the lid of the chamber. After the feeding of the titanium tetrachloride was completed, 7 pounds of molten sodium metal were injected into the mixture of molten chlorides through a second sodium feed line located above the surface of the bath at a velocity of 125 feet persecond. Upon the separation of the sodium chloride from the titanium metal, the metal was found to be of good quality and high purity.
What is claimed is:
1. In the production of titanium metal by the alkali metal reduction of titanium tetrachloride, the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a'stream of titanium tetrachloride at high velocity into a bath of molten alkali metal at a rate and in amount in excess of that which the alkali metal can reduce to titanium so as to avoid the formation of titanium metal at this stage, and then injecting at high velocity into the thus formed molten titanium subchloride a further amount of molten alkali metal sufiicient to reduce the molten subchloride to the metallic state.
2. A process in accordance with the process of claim 1 wherein the injection of molten alkali metal into the molten titanium subchloride is effected below the surface of said moltentitanium subchloride.
3. In the production of titanium metalby the alkali metal reduction of titanium tetrachloride, the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a stream of titanium tetrachloride at high velocity into a bath of molten alkali metal at a rateiand in amount in excess of that which the alkali metal can reduce to titanium so as to avoid the formation of titanium metal at this stage, and then injecting at high velocity into the thus formed molten titanium subchloride a fur ther amount of molten alkali metal sufiicient to reduce the molten subchloride to the metallic state, said reductions being effected in a substantially non-contaminating atmosphere.
4. In the production of titanium metal by the sodium reduction of titanium tetrachloride, the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a stream of titanium tetrachloride at high velocity into a bath of molten sodium at a rate and in amount in excess of that which the sodium can reduce to titanium so as to avoid the formation of titanium metal at this stage, and then injecting at high velocity into the thus formed molten titanium subchloride a further amount of molten sodium sufficient to reduce the molten subchloride to the metallic state. a
5. A process in accordance with the process of claim 4 wherein the injection of molten sodium into the molten titanium subchloride is effected below the surface of said molten titanium subchloride.
6. In the production of titanium metal by the sodium reduction of titanium tetrachloride, the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a stream of titanium tetrachloride at high velocity into a bath of molten sodium at a rate and in amount in excess of that which the sodium can reduce to titanium so as to avoid the formation of titanium metal at this stage, and then injecting at high velocity into the thus formed molten titanium subchloride a further amount of molten sodium sufficient to reduce the I molten subchloride to the metallic state, said reductions being effected in a substantially non-contaminatingatmosphere.
7. In the production of titanium metal by the sodium reduction of titanium tetrachloride, the improvement which comprises first reducing substantially all of the titanium tetrachloride to molten titanium subchloride by directing a stream of titanium tetrachloride at high ve locity into a bath of molten sodium at a rate and in amount in excess of that which the sodium can reduce to titanium so as to avoid the formation of titanium metal at this'stage, and then injecting at high velocity into the thus formed molten titanium subchloride a further amount of molten sodium suflicient to reduce the molten subchloride to the metallic state, said reductions being effected in a substantially non-contaminating atmosphere and at a temperature not greater than 950 C.
References Cited in the file of this patent UNITED STATES PATENTS 2,148,345 Frudenber Feb. 21, 1939 2,443,253 Kroll et al. June 15, 1948 2,586,134 Winter Feb. 19, 1952 2,607,674 Winter Aug. 19, 1952 2,616,800 Wartman Nov. 4,1952 2,618,549 Glasser et a1. .4. Nov. 18, 1952 2,618,550 Hampel et a1 Nov. 18, 1952 2,647,826 Jordan Aug. 4, 1953 2,667,413 Jordan Jan. 26, 1954 2,703,752 Glasser et al Mar. 8, 1955 2,753,256 Olson July 3, 1956 FOREIGN PATENTS 694,921 Great Britain July 29, 1953 1,094,987 France Dec. 15, 1954 OTHER REFERENCES Zeitschrift fur Anorganische und Allegemeine Chemie, vol. 23 4, 1937, pages 42-50, pages 43, 44 pertinent. Metal Industry, May 16, 1947, pages 363-364. Journal of Metals, April 1950, pages 634-640. Aagaard: Abstract of appl. S. N. 129,305, filed Nov. 25, 1949. Published Aug. 14, 1951, 649 0.76. 604.
Chemical Engineering Progress, vol. 50, No. 11, November 1954, pages 578-581.
Claims (1)
1. IN THE PRODUCTION OF TITANIUM METAL BY THE ALKALI METAL REDUCTION OF TITANIUM TETRACHLORIDE, THE IMPROVEMENT WHICH COMPRISES FIRST REDUCING SUBSTANTIALLY ALL OF THE TITANIUM TETRACHLORIDE TO MOLTEN TITANIUM SUBCHLORIDE BY DIRECTING A STREAM OF TITANIUM TETRACHLORIDE AT HIGH VELOCITY INTO A BATH OF MOLTEN ALKALI METAL AT A RATE AND IN AMOUNT IN EXCESS OF THAT WHICH THE ALKALI METAL CAN REDUCE TO TITANIUM SO AS TO AVOID THE FORMATION OF TITANIUM METAL AT THIS STAGE, AND THE INJECTING AT HIGH VELOCITY INTO THE THUS FORMED MOLTEN TITANIUM SUBCHLORIDE A FURTHER AMOUNT OF MOLTEN ALKALI METAL
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| BE546236D BE546236A (en) | 1955-03-28 | ||
| US497322A US2826493A (en) | 1955-03-28 | 1955-03-28 | Method of producing titanium |
| FR1144500D FR1144500A (en) | 1955-03-28 | 1956-03-23 | Process for the production of refractory metals |
| DEU3819A DE1041254B (en) | 1955-03-28 | 1956-03-27 | Multi-stage reduction process for the production of heat-resistant metals of IV., V. and VI. Group of the Periodic Table by reducing their halides with alkali metal in a molten state under a reducing atmosphere |
| GB9461/56A GB824298A (en) | 1955-03-28 | 1956-03-27 | Refractory metal production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US497322A US2826493A (en) | 1955-03-28 | 1955-03-28 | Method of producing titanium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2826493A true US2826493A (en) | 1958-03-11 |
Family
ID=23976387
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US497322A Expired - Lifetime US2826493A (en) | 1955-03-28 | 1955-03-28 | Method of producing titanium |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US2826493A (en) |
| BE (1) | BE546236A (en) |
| DE (1) | DE1041254B (en) |
| FR (1) | FR1144500A (en) |
| GB (1) | GB824298A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2950963A (en) * | 1957-05-02 | 1960-08-30 | Nat Distillers Chem Corp | Production of metals |
| US2963362A (en) * | 1956-02-27 | 1960-12-06 | Nat Distillers Chem Corp | Process for reducing higher halides |
| US2986462A (en) * | 1957-10-10 | 1961-05-30 | Cons Mining & Smelting Co | Process for the production of metals |
| US2995440A (en) * | 1958-04-23 | 1961-08-08 | Union Carbide Corp | Process for producing reactive metals |
| US3004848A (en) * | 1958-10-02 | 1961-10-17 | Nat Distillers Chem Corp | Method of making titanium and zirconium alloys |
| US3069255A (en) * | 1957-11-25 | 1962-12-18 | Jr Don H Baker | Production of high purity titanium by metallic sodium reduction of titanic halide |
| US20220008993A1 (en) * | 2015-02-23 | 2022-01-13 | Nanoscale Powders LLC | Methods for Producing Metal Powders |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2148345A (en) * | 1936-09-10 | 1939-02-21 | Degussa | Preparation of metallic titanium |
| US2443253A (en) * | 1944-04-12 | 1948-06-15 | Electro Metallurg Co | Process for producing zirconium chloride |
| US2586134A (en) * | 1948-12-24 | 1952-02-19 | Du Pont | Production of metals |
| US2607674A (en) * | 1949-05-25 | 1952-08-19 | Du Pont | Production of metals |
| US2616800A (en) * | 1949-11-22 | 1952-11-04 | Frank S Wartman | Method of making cupro-titanium |
| US2618550A (en) * | 1952-01-04 | 1952-11-18 | Kennecott Copper Corp | Method for the production of titanium |
| US2618549A (en) * | 1949-05-02 | 1952-11-18 | Kennecott Copper Corp | Method for the production of titanium |
| GB694921A (en) * | 1950-08-10 | 1953-07-29 | Titan Co Inc | A method for the production of titanium metal or a fused salt mixture from titanium tetrachloride |
| US2647826A (en) * | 1950-02-08 | 1953-08-04 | Jordan James Fernando | Titanium smelting process |
| US2667413A (en) * | 1951-01-15 | 1954-01-26 | Jordan James Fernando | Vapor-phase smelting process |
| US2703752A (en) * | 1951-01-20 | 1955-03-08 | Kennecott Copper Corp | Method for production of refractory metals |
| FR1094987A (en) * | 1953-11-30 | 1955-05-25 | Brevets D Etudes Et De Rech S | Preparation of metals such as titanium and zirconium |
| US2753256A (en) * | 1950-10-11 | 1956-07-03 | Du Pont | Method of producing titanium |
-
0
- BE BE546236D patent/BE546236A/xx unknown
-
1955
- 1955-03-28 US US497322A patent/US2826493A/en not_active Expired - Lifetime
-
1956
- 1956-03-23 FR FR1144500D patent/FR1144500A/en not_active Expired
- 1956-03-27 DE DEU3819A patent/DE1041254B/en active Pending
- 1956-03-27 GB GB9461/56A patent/GB824298A/en not_active Expired
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2148345A (en) * | 1936-09-10 | 1939-02-21 | Degussa | Preparation of metallic titanium |
| US2443253A (en) * | 1944-04-12 | 1948-06-15 | Electro Metallurg Co | Process for producing zirconium chloride |
| US2586134A (en) * | 1948-12-24 | 1952-02-19 | Du Pont | Production of metals |
| US2618549A (en) * | 1949-05-02 | 1952-11-18 | Kennecott Copper Corp | Method for the production of titanium |
| US2607674A (en) * | 1949-05-25 | 1952-08-19 | Du Pont | Production of metals |
| US2616800A (en) * | 1949-11-22 | 1952-11-04 | Frank S Wartman | Method of making cupro-titanium |
| US2647826A (en) * | 1950-02-08 | 1953-08-04 | Jordan James Fernando | Titanium smelting process |
| GB694921A (en) * | 1950-08-10 | 1953-07-29 | Titan Co Inc | A method for the production of titanium metal or a fused salt mixture from titanium tetrachloride |
| US2753256A (en) * | 1950-10-11 | 1956-07-03 | Du Pont | Method of producing titanium |
| US2667413A (en) * | 1951-01-15 | 1954-01-26 | Jordan James Fernando | Vapor-phase smelting process |
| US2703752A (en) * | 1951-01-20 | 1955-03-08 | Kennecott Copper Corp | Method for production of refractory metals |
| US2618550A (en) * | 1952-01-04 | 1952-11-18 | Kennecott Copper Corp | Method for the production of titanium |
| FR1094987A (en) * | 1953-11-30 | 1955-05-25 | Brevets D Etudes Et De Rech S | Preparation of metals such as titanium and zirconium |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2963362A (en) * | 1956-02-27 | 1960-12-06 | Nat Distillers Chem Corp | Process for reducing higher halides |
| US2950963A (en) * | 1957-05-02 | 1960-08-30 | Nat Distillers Chem Corp | Production of metals |
| US2986462A (en) * | 1957-10-10 | 1961-05-30 | Cons Mining & Smelting Co | Process for the production of metals |
| US3069255A (en) * | 1957-11-25 | 1962-12-18 | Jr Don H Baker | Production of high purity titanium by metallic sodium reduction of titanic halide |
| US2995440A (en) * | 1958-04-23 | 1961-08-08 | Union Carbide Corp | Process for producing reactive metals |
| US3004848A (en) * | 1958-10-02 | 1961-10-17 | Nat Distillers Chem Corp | Method of making titanium and zirconium alloys |
| US20220008993A1 (en) * | 2015-02-23 | 2022-01-13 | Nanoscale Powders LLC | Methods for Producing Metal Powders |
| US11858046B2 (en) * | 2015-02-23 | 2024-01-02 | Nanoscale Powders LLC | Methods for producing metal powders |
Also Published As
| Publication number | Publication date |
|---|---|
| FR1144500A (en) | 1957-10-14 |
| BE546236A (en) | |
| GB824298A (en) | 1959-11-25 |
| DE1041254B (en) | 1958-10-16 |
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