Refractory Metal (ti, Zr, Hf, V, Nb, Ta, Cr, Mo, Or W) Patents (Class 423/492)
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Patent number: 4098868Abstract: Titanium metal values may be recovered from a titanium bearing source by roasting said source in a reducing atmosphere, leaching the source with aqueous hydrogen chloride at an elevated temperature, cooling and saturating the leached solution with gaseous hydrogen chloride to precipitate hydrated ferrous chloride, separating the precipitated ferrous chloride from the soluble titanium chloride, raising the temperature of the solution to precipitate the titanium, separating and recovering the crystallized titanium compound.Type: GrantFiled: April 27, 1977Date of Patent: July 4, 1978Assignee: UOP Inc.Inventor: William K. Tolley
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Patent number: 4070252Abstract: A method for separating niobium pentachloride and tantalum pentachloride contaminants from crude titanium chloride vehicle by addition of water to said vehicle to form substantially selectively solid hydration products of such contaminants which are readily separable.Type: GrantFiled: April 18, 1977Date of Patent: January 24, 1978Assignee: SCM CorporationInventor: James Paul Bonsack
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Patent number: 4069268Abstract: Deactivated or partially deactivated hydrocarbon conversion catalysts comprising (a) one or more Lewis acids of the formula MX.sub.n where M is a component selected from Group IIIA, IVB, V, VIB or VIII Elements of the Periodic Table or their mixtures, X is a halogen, and n is the atomic ratio of halogen to M and varies from 1 to 8, and (b) a strong Bronsted acid, may be regenerated by contacting said catalysts with a halogen selected from the group consisting of fluorine or chlorine. If a portion of the catalyst has been hydrolyzed, the catalyst may be regenerated via halogenation as above or by contact with a hydrogen halide selected from the group consisting of hydrogen fluoride or hydrogen chloride and then fluorine. The preferred Lewis acid is a metal halide, preferably tantalum pentafluoride, niobium pentafluoride or mixtures thereof. The preferred Bronsted acid is a hydrogen halide, preferably hydrogen fluoride.Type: GrantFiled: November 4, 1975Date of Patent: January 17, 1978Assignee: Exxon Research & Engineering Co.Inventors: Michael Siskin, Ronald J. Gillespie
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Patent number: 4066424Abstract: Process for selectively recovering metal chlorides from a gaseous mixture of metal chlorides by contacting the gaseous mixture at a temperature above the condensation point of the mixture with at least one stream of liquid to cool all the mixture to below the freezing point of at least one metal chloride in the mixture, the average velocity of the mixture being at least the pneumatic conveyance velocity at the point of contact. This process provides for recovery of metal chlorides without plugging the apparatus.Type: GrantFiled: October 13, 1976Date of Patent: January 3, 1978Assignee: E. I. Du Pont de Nemours and CompanyInventors: Arnold William Kilgren, David Nicholson Low, Robert Warwick Porter
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Patent number: 4065405Abstract: Tantalum and/or niobium pentafluorides may be recovered from a deactivated or partially deactivated hydrocarbon conversion catalyst comprising (a) a metal pentafluoride selected from the group consisting of tantalum pentafluoride, niobium pentafluoride and mixtures thereof and (b) hydrogen fluoride, by distilling said catalyst in the presence of a Lewis acid containing neither of these Group V metals, thereby displacing a pentahalide of tantalum and/or niobium into the vapor phase from which it can be condensed. Addition of hydrogen fluoride then converts the pentahalide to the pentafluoride.Type: GrantFiled: December 3, 1976Date of Patent: December 27, 1977Assignee: Exxon Research and Engineering CompanyInventor: Roger Hulme
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Patent number: 4060593Abstract: Solid titanium trichloride in the form of fine granules having low aluminum compound content, which is suitable as a catalyst for polymerization of .alpha.-olefins, especially, propylene is obtained as a precipitate by heating liquefied titanium trichloride in the presence of a liberating agent, and separating the thus formed precipitate. The liquefied titanium trichloride is preferably prepared with an reducing titanium tetrachloride by organic aluminium compound in the presence of ether and hydrocarbon.Type: GrantFiled: July 31, 1975Date of Patent: November 29, 1977Assignee: Mitsubishi Chemical IndustriesInventors: Yamaguchi Kazuo, Kakogawa Genjiro, Hasuo Masayoshi, Nobuaki Goko, Yasuo Maruyama
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Patent number: 4054686Abstract: Bulk coatings of Nb.sub.3 Ge superconductors having transition temperatures in excess of 20 K are readily formed by a chemical vapor deposition technique involving the coreduction of NbCl.sub.5 and GeCl.sub.4 in the presence of hydrogen. The NbCl.sub.5 vapor may advantageously be formed quantitatively in the temperature range of about 250.degree. to 260.degree. C by the chlorination of Nb metal provided the partial pressure of the product NbCl.sub.5 vapor is maintained at or below about 0.1 atm.Type: GrantFiled: June 26, 1975Date of Patent: October 18, 1977Assignee: The United States of America as represented by the United States Energy Research and Development AdministrationInventors: Lawrence R. Newkirk, Flavio A. Valencia
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Patent number: 4046853Abstract: The simultaneous chlorination of the iron and titanium values in an iron containing titaniferous ore such as ilmenite is advantageously conducted to convert the iron values to ferrous chloride but the resulting gaseous effluent is difficult to process to recover the titanium tetrachloride. The iron values in the effluent are partially oxidized according to the equation3FeCl.sub.2 + 3/4O.sub.2 .fwdarw. 1/2Fe.sub.2 O.sub.3 + 2FeCl.sub.3thereby reducing the vapor partial pressure of the ferrous chloride while maintaining the presence of some ferrous chloride to scavenge any chlorine emitted from the chlorination stage. The residual gaseous iron chlorides are condensed and chlorine-free titanium tetrachloride may be recovered from the remaining gases. If chlorine-free titanium tetrachloride is not required the mixture of gases resulting from the partial oxidation are reduced in temperature of from 500.degree. C to 800.degree.Type: GrantFiled: June 15, 1976Date of Patent: September 6, 1977Assignee: Laporte Industries LimitedInventor: Michael Robinson
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Patent number: 4021531Abstract: The invention relates to a process for the separation of zirconium, and hafnium tetrachlorides from mixtures thereof. The process according to the invention consists of selectively absorbing zirconium tetrachloride and hafnium tetrachloride vapors in a solvent medium circulating counter-current to these vapors in a distillation column, wherein the solvent consists of a molten chloroaluminate and/or chloroferrate of potassium. The process described may be used to obtain hafnium-free zirconium tetrachloride which may then be used to prepare nuclear-grade zirconium, and hafnium tetrachloride containing little zirconium.Type: GrantFiled: April 15, 1976Date of Patent: May 3, 1977Assignee: Ugine AciersInventors: Paul Besson, Jean Guerin, Pierre Brun, Michel Bakes
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Patent number: 4017304Abstract: A reduction/chlorination process is provided for the treatment of titaniferous materials such as ilmenite ores. The chlorination is selective in that the titanium constituent of the titaniferous material is chlorinated, but there is no appreciable net yield of iron chloride from the iron constituent. Where other metals such as vanadium are present they may be chlorinated with the titanium. The reduction utilizes as the reductant an amount of carbonaceous material which, based on oxygen in the titaniferous material, is at least stoichiometric to produce carbon monoxide. The selective chlorination utilizes as the chlorinating agent either ferrous chloride (FeCl.sub.2) alone or certain combinations of ferrous chloride and one or more other chlorine-containing members, notably molecular chlorine (Cl.sub.2) and hydrogen chloride (HCl). The use of ferric chloride (FeCl.sub.3) as a part or all of the chlorinating agent is the equivalent of using a FeCl.sub.2 /0.5 Cl.sub.2 mixture.Type: GrantFiled: September 18, 1973Date of Patent: April 12, 1977Assignee: E. I. Du Pont de Nemours and CompanyInventor: Hans Hellmut Glaeser
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Patent number: 4014976Abstract: Titanium tetrachloride is produced by reacting a titaniferous material having a particle size of 150 mesh or less (Tyler standard) as a median value with a chlorine-containing gas in the presence of a coarse carbonaceous substance in a dilute-phase fluidization system.Type: GrantFiled: March 24, 1976Date of Patent: March 29, 1977Assignee: Ishihara Sangyo Kaisha Ltd.Inventors: Masaaki Adachi, Takayoshi Shirai, Norio Nakasuzi
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Patent number: 3992159Abstract: A process is described for purifying liquids by cryogenic sublimation. This process involves solidifying the liquid by reducing the temperature and pressure to below the triple point. Purification is then carried out by direct transformation from the solid to the vapor phase. Because of increased differentials in vapor pressures at the low temperature at which the procedure is carried out, this purification process is highly efficient and is also particularly suitable for liquids that are susceptible to decomposition with ordinary purification procedures requiring elevated temperatures. The procedure is also advantageous in separating azeotropes, structurally similar compounds, as well as treating flammable, hydroscopic, corrosive and fuming compounds.Type: GrantFiled: June 23, 1975Date of Patent: November 16, 1976Assignee: Bell Telephone Laboratories, IncorporatedInventor: James Windfield Mitchell
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Patent number: 3991157Abstract: A chlorine-containing gas is introduced as an upward flow into a vertical, upwardly widening column-type reactor, and a titaniferous material and a solid carbonaceous reducing agent are charged into the reactor at its upper and lower parts to effect chlorination in a dilute-phase fluidization system accompanied by reflux of part of the solid materials and thereby yield titanium tetrachloride.Type: GrantFiled: March 20, 1975Date of Patent: November 9, 1976Assignee: Ishihara Sangyo Kaisha Ltd.Inventors: Masaaki Adachi, Kenichi Ichimura, Takayoshi Shirai
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Patent number: 3990891Abstract: This invention provides a process for obtaining the nonferrous metal values from a manganese oxide ore, by reacting the ore with an aluminum halide or a ferric halide at a temperature of at least about 50.degree. C and preferably, at least about 130.degree. C. The manganese oxide ore can be treated with or without reduction. If reduction of the manganese oxide ore is desired, it can be accomplished prior to, or simultaneously with, the reaction with the aluminum halide or ferric halide.The resulting nonferrous metal halides can be separated from the reacted ore residue by conventional methods such as leaching or evaporation.Type: GrantFiled: May 24, 1974Date of Patent: November 9, 1976Assignee: Deepsea Ventures, Inc.Inventors: Richard G. Sandberg, Paul H. Cardwell
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Patent number: 3989510Abstract: A reactor operating at a maximum temperature above 1535.degree. C and up to about 1950.degree. C is charged with a mixture of: (a) iron bearing titaniferous ore or its concentrate, or a residue from other operations containing iron and titanium, at least some of which is present as oxides, also (b) silica -- combined or separately added, also (c) one or more chlorides of a third metal of the alkaline or alkaline earth group, such as common salt and/or calcium chloride, also (d) a solid reductant as coke. Some impurities of the original material are removed as volatile chlorides or oxy-chlorides; the titanium also goes off as TiCl.sub.4 in the gas stream, the iron is withdrawn as molten metallic iron, and the third metal added as the chloride: e.g., the sodium of the common salt or the calcium of its chloride unites with the silica to give a silicate, such as sodium silicate (water glass) and/or calcium silicate which acts as a flux to remove the gangue from the iron.Type: GrantFiled: April 12, 1974Date of Patent: November 2, 1976Inventor: Donald F. Othmer
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Patent number: 3979372Abstract: It is known to prepare highly active catalyst components for a Ziegler polymerization catalyst by reduction of titanium tetrachloride with an aluminum alkyl. An improvement in the preparation of such catalysts which leads to production of highly sterospecific as well as highly active catalyst components consists of including in the preparation the step of washing the reaction mixture which contains the desired TiCl.sub.3 composition with an aliphatic hydrocarbon at temperatures above 40.degree.C and separating the washed solids from the wash liquid at a temperature above 40.degree.C. A heat treatment above 80.degree.C precedes, accompanies, or follows the washing and separation step. The washing step may be carried out in a single or in multiple stages.Type: GrantFiled: December 30, 1974Date of Patent: September 7, 1976Assignee: Shell Oil CompanyInventors: Herman Th. VAN DER Bend, Willem Sjardijn
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Patent number: 3966458Abstract: A process is provided for separating zirconium and hafnium tetrachlorides by the direct distillation from their solution in an eutectic mixture of sodium and potassium chlorides. Hafnium tetrachloride and zirconium tetrachloride are provided in adequate purity for direct introduction into reduction units for the production of the respective metals by virtue of controlled ratios of the salt eutectic solvent to the hafnium and zirconium tetrachlorides and by provision of a reflux of hafnium with added increments of the eutectic solvent salt mixture.Type: GrantFiled: September 6, 1974Date of Patent: June 29, 1976Assignee: Amax Speciality Metal CorporationInventor: Donald R. Spink
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Patent number: 3963585Abstract: In the purification of impure titanium tetrachloride comprising adding an agent to said titanium tetrachloride and thereafter distilling off purified titanium tetrachloride while leaving the impurity in the distillation residue, the improvement which comprises employing as said agent at least one amine of the formula ##EQU1## in which R.sub.1 and R.sub.2 each independently is hydrogen, alkyl or alkenyl of up to 6 carbon atoms, cycloalkyl of 5 to 7 carbon atoms, or aryl, andR.sub.3 is cycloalkyl of 5 to 7 ring carbon atoms, or aryl, orR.sub.2 together with R.sub.3 is butylene, pentylene or hexylene, in which eventR.sub.1 is hydrogen, alkyl of up to 6 carbon atoms or aryl.The preferred agents are aniline, cyclohexylamine, N,N-dimethyl-aniline, diphenylamine, 2,3-dimethyl-aniline and 2,6-dimethyl-aniline. The process serves to remove vanadium impurities.Type: GrantFiled: May 1, 1974Date of Patent: June 15, 1976Assignee: Bayer AktiengesellschaftInventors: Gerhard Winter, Walter Deissmann, Walter Gutsche, Peter Woditsch
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Patent number: 3954954Abstract: In the process of carrying out high temperature, chemical reactions including reductions for producing elemental metal powders, especially refractory metals; chlorinations for producing halogens and for chemical synthesis in general using a plasma generator, the reactant or reactants feed material is introduced into the reaction zone of the apparatus and the effluent from the reaction zone is directed into a quenching zone through a selectively variable passageway or orifice in a manner that permits in the reduction process separation of the desired reaction product from the effluent hot gas stream and the continuous collection of the reaction product in a collection zone wherein in some instances, the reaction product is of a selected characteristic, controlled by the maintenance of certain operational parameters, including a selected differential fluid pressure in the reaction and collection zone as well as reaction and collection zone temperatures.Type: GrantFiled: January 2, 1974Date of Patent: May 4, 1976Assignee: Plasmachem, Inc.Inventors: Robert D. Davis, Theodore N. Meyer, Roy L. Blizzard
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Patent number: 3950162Abstract: This invention provides a process for obtaining substantially pure manganese metal by the reduction of a manganese oxide or a manganese halide by reaction with a subhalide of a transport metal. The transport metal can be aluminum, silicon, or titanium. In preferred embodiments of this procedure, a continuous closed cycle process is carried out wherein the transport metal value is reconverted to its subhalide and recycled for reaction with additional manganese compound.Type: GrantFiled: May 20, 1974Date of Patent: April 13, 1976Assignee: Deepsea Ventures, Inc.Inventors: Harold H. Schobert, Roger C. Field, Paul H. Cardwell
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Patent number: 3939244Abstract: Process for the purification of titanium tetrachloride, in which the said titanium tetrachloride is brought into contact with a purifying agent consisting of an inert support in granular form on which metallic sodium or other reducing metal has been deposited in sub-divided form, the said contact taking place either on crude liquid titanium tetrachloride with subsequent distillation to recover the purified titanium tetrachloride or on crude vaporised titanium tetrachloride with subsequent condensation to recover the purified titanium tetrachloride.Type: GrantFiled: November 27, 1972Date of Patent: February 17, 1976Assignee: Societa Italiana Resine S.I.R. S.p.A.Inventors: Luigi Piccolo, Antonio Paolinelli, Marcello Ghirga
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Patent number: 3937794Abstract: An improved method of making finely divided, dry metal halides and sulfides, such as chromium chloride and chromium sulfide which are suitable for use as lubricants and wear-proof and corrosion-proof agents for metals.Type: GrantFiled: August 2, 1973Date of Patent: February 10, 1976Assignee: Kabushiki Kaisha KitoInventors: Norio Kanetake, Ikuo Maruyama, Katsuyuki Morita
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Patent number: 3935293Abstract: The raw material contains 80% by weight of an alloy of two at least of the metals of the group Fe, Ni, Cr, Cu, Co (and possibly sulphur), in the form of ingots, scrap-metal or mats, in pieces less than 200 mm in size. The alloys are firstly subjected to a chlorination operation at a temperature comprised between 600.degree.C and 1350.degree.C and then to the recovery operation for the chlorides formed. An enclosure, called a chlorination enclosure, is charged with (a) the alloy, (b) a gaseous mixture containing chlorine and HCl, (c) oxygen, and (d) at least one agent for regulating the temperature of the enclosure. The composition of the gaseous mixture, when it is constituted at the same time of Cl.sub.2 and of HCl, responds to the following conditions:5 % < the proportion of Cl.sub.2 < 90 %1 % < the proportion of HCl < 75 %1 % < the proportion of O.sub.2 < 35 %the partial pressures satisfying on their part the following conditions:2P.sub.Cl.sbsb.2 + P.sub.HCl > 0.2 atmosphere, andP.sub.Type: GrantFiled: June 29, 1973Date of Patent: January 27, 1976Assignee: Larco Societe Miniere et Metallurgique de Larymna S.A.Inventor: Constantin Tsirigotis