Titanium, Zirconium, Or Hafnium Patents (Class 423/76)
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Patent number: 11213765Abstract: The present invention provides a process for recovering transition metal tetrahalides from a waste stream coming from a catalyst manufacturing process by (a) establishing a mixed stream comprising transition metal tetrahalide and transition metal alkoxyhalides; (b) forming a falling liquid film from the mixed stream of step (a) at a temperature of from 25 to 85° C. and an absolute pressure of from 0.05 to 0.6 bar; and (c) establishing from the film of step (b) a first vapour stream containing from 90 to 100% of recoverable components and a second liquid stream containing about 10 to 80% of titanium haloalkoxides.Type: GrantFiled: July 30, 2019Date of Patent: January 4, 2022Assignee: Borealis AGInventors: Mikko Lylykangas, Jukka Räsänen, Klaus Nyfors, Pekka Malinen
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Patent number: 8399529Abstract: For processing of noble metal-containing, moist recycling materials with an unknown noble metal content (hereinafter called “batch”), a moisture-binding agent is added for homogenisation and the batch is mixed with comminution of optionally pre-sent agglomerates to form a free-flowing and homogenous powder. Optionally, the following takes place subsequently for analysis: A at least one representative, volume-reduced sample is taken first of all, B the sample is dried, C the sample is optionally divided further and D the sample is analyzed and the noble metal content of the batch is calculated on the basis of the data a previously known or pre-calculated quantity of the moisture-binding agent being added before sampling (step A).Type: GrantFiled: September 7, 2006Date of Patent: March 19, 2013Assignee: W.C. Heraeus GmbHInventors: Christian Mock, Horst Meyer, Matthias Grehl, Jochen Schleβmann, Martin Stettner
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Patent number: 8309042Abstract: The disclosure provides a process for recycling ore in the chloride process, without the build-up of silica-containing gangue in the chlorination reactor.Type: GrantFiled: January 23, 2008Date of Patent: November 13, 2012Assignee: E I du Pont de Nemours and CompanyInventors: Matthew Donnel Eisenmann, Jorge Lavastida, Timothy Josiah McKeon, James Elliott Merkle, Jr.
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Patent number: 7976818Abstract: A method for continuously recovering titanium tetrachloride TiCl4 from a waste liquid comprising TiCl4 and by-products, wherein said waste liquid is subjected, as a flowing liquid film, to an evaporation step for a residence time of less than 15 minutes at a temperature higher than 90° C.Type: GrantFiled: November 21, 2005Date of Patent: July 12, 2011Assignee: Basell Poliolefine Italia s.r.l.Inventors: Paolo Vincenzi, Rosa Spoto, Matteo Badalocchi
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Patent number: 7927879Abstract: Proposed is a zirconium crucible used for melting an analytical sample in the pretreatment of the analytical sample, wherein the purity of the zirconium crucible is 99.99 wt % or higher. In light of the recent analytical technology demanded of fast and accurate measurement of high purity materials, the present invention provides a zirconium crucible for melting an analytical sample, a method of preparing such analytical sample, and a method of analysis that enables the analysis of high purity materials by inhibiting the inclusion of impurities from the crucible regardless of difference in the analysts and their skill.Type: GrantFiled: February 20, 2007Date of Patent: April 19, 2011Assignee: JX Nippon Mining & Metals CorporationInventors: Masahiro Sakaguchi, Mitsuru Yamaguchi, Tomio Takahashi, Kouichi Takemoto
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Patent number: 7824487Abstract: The invention covers a fine-particle, brilliant and strongly hiding rutile-based pigment that is devoid of any metal or reactive metal compounds relevant to mill abrasion detectable by application technology but whose particle-size in terms of particle diameters ranges from 50 to 1000 nm, for mono-, bi-, tri- or oligo-modal size distribution and a primary maximum ranges from 230 to 400 nm, wherein optionally for a bi- or poly-modal frequency distribution, a secondary maximum is less than 25% of the primary maximum between 400 and 1000 nm. The process for producing said pigment comprises treating an inorganic mixed-phase rutile structured oxide pigment by high-speed grinding in suspension in a ball grinding mill provided with a mechanically and chemically resistant coating until said particle-size and a substantially isometric rounded particle shape are attained. The invention optionally provides for viscosity adjustment and surface conditioning of the pigment.Type: GrantFiled: February 20, 2007Date of Patent: November 2, 2010Assignee: Heubach GmbHInventor: Rainer Heubach
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Patent number: 7824486Abstract: The present disclosure relates to a process for making a decorative base paper for a paper laminate comprising impregnating a base paper with a pigment mixture of titanium dioxide and water wherein the titanium dioxide pigment is made by treating a mixture of titanium dioxide pigment and water with a source of phosphorus and a source of aluminum; drying the treated mixture to form a treated pigment, the treated pigment having surface hydroxyl groups; and removing a major proportion of the surface hydroxyl groups of the treated pigment. Preferably the surface hydroxyl groups are removed by thermal treatment, for example at temperatures ranging from 300° C. to 800° C. The source of phosphorus is typically phosphoric acid and the source of aluminum is typically sodium aluminate. The pigment can be characterized by an isoelectric point which is greater than pH 6 and a negative zeta potential of at least 20 mV at a pH of 7.5 or more and wherein the pigment has improved light fastness.Type: GrantFiled: September 27, 2005Date of Patent: November 2, 2010Assignee: E. I. du Pont de Nemours and CompanyInventor: Erik Shepard Thiele
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Patent number: 7780931Abstract: Process for preparing TiO2 powders starting from a liquid comprising chlorinated titanium compounds, the process comprising: a) atomizing said liquid and reacting the atomized liquid with a flow of steam and air at a temperature of 100-250° C. for converting said chlorinated titanium compounds to titanium dioxide TiO2; b) the gaseous phase and the entrained TiO2 powders obtained from step a) are then fed to an oven operated at a temperature in the range 400-900° C. to remove the residual organic compounds and hydrochloridic acid from said powders.Type: GrantFiled: November 3, 2005Date of Patent: August 24, 2010Assignee: Basell Poliolefine Italia s.r.l.Inventors: Anna Fait, Arrigo Arletti, Lucia Caiazzo
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Patent number: 7713662Abstract: The invention provides a lithium-manganese-based composite oxide containing Ti and Ni, which is represented by the compositional formula: Li1+x(Mn1?n?mNimTin)1?xO2, wherein 0<x?0.33, 0.05<m<0.3, and 0.3<n<0.5, and includes a crystal phase of layered rock-salt type structure. The composite oxide is a novel material that is capable of maintaining an average discharge voltage of 3 V or more over long charge/discharge cycles, while providing a discharge capacity equal to or higher than those of lithium-cobalt-oxide-based positive electrode materials, and that can be prepared using starting materials that are inexpensive and less limited as natural resources, while exhibiting improved charge/discharge characteristics over known low-cost positive electrode materials.Type: GrantFiled: November 13, 2007Date of Patent: May 11, 2010Assignee: National Institute of Advanced Industrial Science and TechnologyInventors: Mitsuharu Tabuchi, Yuko Oka, Tomonari Takeuchi, Kuniaki Tatsumi
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Patent number: 7585488Abstract: An anatase-type titanium oxide powder having a ratio of rutile to anatase of 10% or less and a BET specific surface area of 20 to 80 m2/g. Since the titanium oxide powder has a large specific surface area and a low ratio of rutile to anatase in comparison with a conventional titanium oxide powder and excels in dispersibility, the titanium oxide powder is suitable for various applications.Type: GrantFiled: March 10, 2005Date of Patent: September 8, 2009Assignee: Toho Titanium Co., Ltd.Inventor: Hideki Sakai
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Patent number: 7476378Abstract: This disclosure relates to a process for producing titanium dioxide, comprising: a) providing a quantity of liquid titanium tetrahalide for reacting with an oxygen-containing gas; b) vaporizing a first portion of the liquid titanium tetrahalide and reacting the titanium tetrahalide vapor and the oxygen-containing gas, in a first stage of a reaction zone, the reaction zone temperature ranging from at least about 650° C.—to form a reaction product at least containing titanium dioxide and oxygen-containing gas and passing the reaction product, more typically in the vapor phase, to at least one additional stage of the reaction zone; and c) charging at least one additional portion of the liquid titanium tetrahalide to the at least one additional stage of the reaction zone to cool the titanium dioxide and to react with the oxygen-containing gas to form additional titanium dioxide.Type: GrantFiled: October 27, 2005Date of Patent: January 13, 2009Assignee: E.I. DuPont deNemours & CompanyInventors: Narayanan Sankara Subramanian, Richard P. Bernard, Yung-Hsing Samson Hsu, Charles David Musick, Kunle Ogunde, James Nelson Tilton
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Patent number: 7452389Abstract: The incorporation or blending of from about 1 to about 10% by volume of a “carbide precursor” powder, preferably on the order of <100 microns in size, with a coal particulate starting material and the subsequent production of carbon foam in accordance with the method described herein, results in a carbon foam that exhibits significantly enhanced abrasive characteristics typical of those required in the polishing of, for example glass, in the manufacture of cathode ray tubes.Type: GrantFiled: March 29, 2004Date of Patent: November 18, 2008Assignee: Touchstone Research Laboratory, Ltd.Inventors: Darren Kenneth Rogers, Janusz Wladyslaw Plucinski
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Patent number: 7413726Abstract: The present invention provides a low temperature process for the synthesis of ultrafine rutile phase titanium dioxide particles through vapor phase hydrolysis of titanium tetra chloride.Type: GrantFiled: March 26, 2004Date of Patent: August 19, 2008Assignee: Council of Scientific and Industrial ResearchInventors: Gerald D. Surender, Ani K. John, Kumara P. Rajendra Prasad, Savithri Sivaraman
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Patent number: 7368096Abstract: The disclosure is directed to a process for isolating solids from a purification purge stream comprising an impurity present as a solid, wherein the purification purge stream is substantially free of chlorides other than titanium tetrachloride and vanadium chloride, the process comprising the steps of: (a) atomizing the purification purge stream comprising titanium tetrachloride as a liquid and an impurity present as a solid; (b) drying solids in the atomized purification purge stream by contacting the atomized stream with a titanium tetrachloride vapor stream such that the combined streams reach a temperature of at least about 140° C. to vaporize the liquid titanium tetrachloride, wherein the titanium tetrachloride vapor is substantially free of chlorides other than those of titanium and vanadium, and substantially free of non-condensable gases comprising CO, CO2, N2, or mixtures thereof; and (c) separating the impurity present as a solid from the vaporized titanium tetrachloride.Type: GrantFiled: June 7, 2005Date of Patent: May 6, 2008Assignee: E.I. du Pont de Nemours and CompanyInventors: Xuqing Gu, Stephen Erwin Lyke, Steve Mirabella, Joseph M. Shekiro, Jr., Jodi Lynn Witt
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Patent number: 7326399Abstract: Titanium dioxide nanoparticles are formed using a dispersing agent to form nanoparticles with desired size, shape, and uniformity. The titanium dioxide nanoparticles are formed by reacting an inorganic titanium compound with water or ice to form an aqueous titanium compound. The aqueous titanium compound is reacted or combined with a dispersing agent. Titanium dioxide nanoparticles are precipitated to form a suspension. The formation of the titanium dioxide nanoparticles is influenced by the presence of bonding of the dispersing agent. The size of the nanoparticles can be advantageously controlled by selecting the ratio of titanium to dispersing agent. In addition, the titanium dioxide nanoparticles can be used in suspension form or filtered and dried to form a powder.Type: GrantFiled: April 15, 2005Date of Patent: February 5, 2008Assignee: Headwaters Technology Innovation, LLCInventors: Bing Zhou, Sukesh Parasher, Zhihua Wu, Zhenhua Zhou
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Patent number: 7041150Abstract: A method and apparatus for making alloys or ceramics by the subsurface injection of an equilibrium vapor of a boiling liquid of the ceramic or alloys constituents is disclosed. Various powders and products are disclosed.Type: GrantFiled: September 3, 2003Date of Patent: May 9, 2006Assignee: The University of ChicagoInventors: Donn Reynolds Armstrong, Richard Paul Anderson, Lance E. Jacobsen
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Patent number: 6929786Abstract: A method of separating zirconium and hafnium tetrachlorides using a solvent comprising firstly an alkaline metallic solvent comprising a salt made up of an alkali metal chloride and an acidic metal chloride A, for example a chloroaluminate or an alkaline chloroferrate, and secondly an acidic metal or metalloid chloride B of acidity that is less than that of the acidic metal chloride A. The acidic metal or metalloid chloride B may be selected from chlorides of Mg, Zn, and Cu. The method may be a continuous separation method by selective absorption of the tetrachloride vapors by the solvent in the substantially or totally molten state.Type: GrantFiled: April 12, 2002Date of Patent: August 16, 2005Assignee: Compagnie Europeenne du Zirconium CEZUSInventors: Laurence Delons, Gérard Picard, Delphine Tigreat
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Patent number: 6869455Abstract: The incorporation or blending of from about 1 to about 10% by volume of a “carbide precursor” powder, preferably on the order of <100 microns in size, with a coal particulate starting material and the subsequent production of carbon foam in accordance with the method described herein, results in a carbon foam that exhibits significantly enhanced abrasive characteristics typical of those required in the polishing of, for example glass, in the manufacture of cathode ray tubes.Type: GrantFiled: February 5, 2002Date of Patent: March 22, 2005Assignee: Touchstone Research Laboratory, Ltd.Inventors: Darren Kenneth Rogers, Janusz Wladyslaw Plucinski
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Patent number: 6860910Abstract: The incorporation or blending of from about 1 to about 10% by volume of a “carbide precursor” powder, preferably on the order of <100 microns in size, with a coal particulate starting material and the subsequent production of carbon foam in accordance with the method described herein, results in a carbon foam that exhibits significantly enhanced abrasive characteristics typical of those required in the polishing of, for example glass, in the manufacture of cathode ray tubes.Type: GrantFiled: October 12, 2001Date of Patent: March 1, 2005Assignee: Touchstone Research Laboratories, Ltd.Inventors: Darren Kenneth Rogers, Janusz Wladyslaw Plucinski
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Patent number: 6790319Abstract: A method for recovering a titanium compound includes bringing a waste solution containing a titanium alkoxide into contact with a halogenating agent to convert at least a part of the titanium alkoxide to a titanium halide, and then distilling the solution containing the titanium halide to recover the titanium halide from the solution, or the method includes distilling a waste solution containing a titanium alkoxide and a titanium halide to recover at least a part of the titanium halide from the waste solution, bringing a residue in a distiller after the distillation into contact with a halogenating agent to convert at least a part of the titanium alkoxide to a titanium halide, and distilling the solution containing the titanium halide to recover the titanium halide from the solution. The method can recover an increased amount of a titanium compound from a waste solution containing a titanium alkoxide.Type: GrantFiled: November 28, 2001Date of Patent: September 14, 2004Assignee: Mitsui Chemicals, Inc.Inventors: Takumi Kitahara, Tetsuya Nakano
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Patent number: 6770254Abstract: This invention relates to an improved process for removing trace levels of Group IVb contaminants from a Group IVb metal tetrahalide of and particularly to a process for removing zirconium tetrachloride from titanium tetrachloride. The improvement resides in contacting a titanium tetrachloride feedstock containing trace impurities of zirconium tetrachloride or hafnium tetrachloride with a sufficient amount of titanium hydride to convert any zirconium tetrachloride or hafnium tetrachloride to a lower volatile compound. The resultant mixture is distilled and the titanium tetrachloride separated from the lower volatile zirconium or hafnium compounds.Type: GrantFiled: January 17, 2002Date of Patent: August 3, 2004Assignee: Air Products and Chemicals, Inc.Inventors: Heather Regina Bowen, David Allen Roberts
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Patent number: 6627120Abstract: In order to achieve miniaturization and an increase in the capacitance of a monolithic ceramic capacitor, a conductive paste suitable for forming an internal conductor film is provided, the layer thickness of the internal conductor film being decreased with a decrease in the layer thickness of a dielectric ceramic layer. The conductive paste contains a conductive powder, such as a nickel powder, an organic vehicle, an organic acid barium salt and an organic zirconium compound. Each of the organic acid barium salt in terms of barium atom and the organic zirconium compound in terms of zirconium atom is about 0.05 to 1.00 mol per mol of the conductive powder, and the content of the organic zirconium compound in terms of zirconium atom is about 0.98 to 1.02 mol per mol of the organic acid barium salt in terms of barium atom.Type: GrantFiled: January 30, 2003Date of Patent: September 30, 2003Assignee: Murata Manufacturing Co. Ltd.Inventor: Motohiro Shimizu
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Patent number: 6572793Abstract: A method of producing an electronic device including a dielectric layer includes a dielectric ceramic composition containing a main component expressed by a formula of {(Sr1−xCax)O}m.(Ti1−yZry)O2, wherein x fulfills 0≦x≦1.00 and y fulfills 0≦y≦0.20, and producing said dielectric ceramic composition by using a material expressed by a formula of {(Sr1−xCax)O}m′.(Ti1−yZry)O2 wherein the mole ratio m′ fulfills m′<m. It is possible to produce an electronic device, such as a chip capacitor, having excellent resistance to reducing during firing and excellent capacity-temperature characteristics after firing, wherein the insulation resistance is hard to be deteriorated particularly when made to be a thin layer and defect rate of the initial insulation resistance is low.Type: GrantFiled: March 19, 2001Date of Patent: June 3, 2003Assignee: TDK CorporationInventors: Takashi Fukui, Yasuo Watanabe, Mikio Takahashi, Akira Sato
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Patent number: 6500396Abstract: A method for the production of titanium metal from titanium-bearing ore. The method comprises leaching said ore or a concentrate thereof with an aqueous solution of a hydrogen halide; separating solids from the leach solution, to provide a leachate solution. The leachate solution may be subjected to extraction with an immiscible organic phase. Titanium halide is separated from the organic phase by stripping. Preferably, the titanium halide is titanium tetrachloride.Type: GrantFiled: November 17, 1999Date of Patent: December 31, 2002Inventors: Vaikuntam Iyer Lakshmanan, Ramamritham Sridhar, Marc Murray Rishea, Robert Joseph de Laat
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Patent number: 6440383Abstract: A hydrometallurgical process is provided for producing ultrafine or nano-sized titanium dioxide from titanium containing solutions, particularly titanium chloride solutions. The process is conducted by total evaporation of the solution, above the boiling point of the solution and below the temperature where there is significant crystal growth. Chemical control additives may be added to control particle size. Nano-sized elemental particles are formed after calcination. The titanium dioxide can be either anatase or rutile. Following calcination, the titanium dioxide is milled to liberate the elemental particles and provide a high quality nano-sized TiO2 with a narrow particle size distribution.Type: GrantFiled: February 14, 2000Date of Patent: August 27, 2002Assignee: Altair Nanomaterials Inc.Inventors: Willem P. C. Duyvesteyn, Timothy Malcome Spitler, Bruce James Sabacky, Jan Prochazka
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Patent number: 6423291Abstract: The invention provides a process for the production of titanium tetrachloride (TiCl4) by the chlorination of titanium values in a titanium-containing starting material. The process includes exposing the starting material to a chlorinating agent and contacting the starting material with an inert liquid while the starting material is exposed to the chlorinating agent. The inert liquid is at a temperature of 200-350° C. and is at a pressure of 5-100 atmospheres (1 atmosphere=101.325 kN/m2). This causes the starting material to react with the chlorinating agent to form TiCl4. The invention also extends to TiCl4 whenever made in accordance with the method.Type: GrantFiled: August 10, 2000Date of Patent: July 23, 2002Inventors: Andrew Kenneth Stone, David Steyn Van Vuuren, Kevin Frans Pieter Cilliers
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Patent number: 6399033Abstract: An improvement to the chloride process of making titanium dioxide. By recycling some of the cyclone dust, the yield in the chlorination of titanium-containing raw materials can be increased. In order to prevent silica accumulation in the fluidized bed, the cyclone dust is divided into two fractions. An economic solution is described of a single-stage separation of the cyclone dust in a hydrocyclone, the majority of the titanium dioxide occurring in the hydrocyclone underflow, although the separation is not sharp. By grinding and drying the solids from the hydrocyclone underflow, the titanium dioxide particles returned to the lower region of the fluidized-bed reactor are rapidly chlorinated, while the quartz and coke particles are rapidly discharged again from the fluid bed, so that no silica contamination occurs.Type: GrantFiled: November 3, 1995Date of Patent: June 4, 2002Assignee: Kronos, Inc.Inventor: Achim Hartmann
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Patent number: 5948212Abstract: A process for the separation of a mixture of a titanium tetrahalide, a reaction diluent of an intermediate boiling point and at least one of a titanium alkoxide, ester or complex thereof without the aid of a distinct separation solvent by subjecting the mixture to a first distillation step to separate the titanium tetrahalide as the lights component and subjecting the heavies product to a second distillation step to recover a portion of the reaction diluent as the lights component.Type: GrantFiled: October 21, 1996Date of Patent: September 7, 1999Assignee: Union Carbide Chemicals & Plastics Technology CorporationInventors: Peter Anthony Kilty, Michael Philip Zum-Mallen, Michael Wayne Potter
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Patent number: 5437854Abstract: Zirconium tetrachloride containing hafnium tetrachloride is selectively reduced with liquid metallic tin to produce zirconium trichloride. The hafnium tetrachloride is then separated as a vapor from a slurry of zirconium trichloride and other solids, including stannous dichloride, in liquid metallic tin.Type: GrantFiled: June 27, 1994Date of Patent: August 1, 1995Assignee: Westinghouse Electric CorporationInventors: Roy G. Walker, Carlos L. Aguilar
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Patent number: 5242549Abstract: An improved process for separation of valuable components of a waste stream resulting from production of an olefin polymerization procatalyst by the addition to the waste stream of a separation solvent of intermediate boiling point, subjecting the resulting mixture to a first distillation zone to separate the desired waste stream components from the upper portion of the zone and passing the bottoms product to a second distillation zone wherein separation solvent is recovered from the upper portion of the zone for recycle and passing the bottoms product to disposal or further processing.Type: GrantFiled: December 6, 1991Date of Patent: September 7, 1993Assignee: Shell Oil CompanyInventors: Michael W. Potter, Stephen W. Cowan, Robert S. Tomaskovic
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Patent number: 5171549Abstract: An improved halogenator process and system is provided which significantly and economically decreases the level of impurities in the processing of various refractory metals and their halides and particularly hafnium tetrachloride which is condensed from gases produced by the chlorination of Zircon.Type: GrantFiled: May 22, 1991Date of Patent: December 15, 1992Assignee: Teledyne Wah Chang AlbanyInventors: Ronald E. Walsh, Jr., Peter W. Krag, Roy E. Blackstone, Duane L. Hug
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Patent number: 5158651Abstract: A process for removing inorganic compounds from glycol recovery still bottoms resulting from the manufacture of poly(ethylene terephthalate), the novel process using a small amount of phosphoric acid to precipitate the antimony and then removing the titanium dioxide and antimony compound by a centrifuge. The novel process for removing the inorganic compounds from the recovery polyester bottoms includes the steps of distilling ethylene glycol from the spent glycol until the remaining bottoms have a solids concentration from about 15% to about 45%; adding phosphoric acid to the bottoms to form an antimony compound and removing the antimony and titanium precipitates from the bottoms by a centrifuge.Type: GrantFiled: June 11, 1990Date of Patent: October 27, 1992Assignee: Hoechst Celanese CorporationInventor: Marvin L. Doerr
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Patent number: 5110566Abstract: The isotopes of zirconium can be partially or completely separated by loading an aqueous solution of an ionic compound of zirconium onto a cationic exchange resin with pentavalent phosphorus derived active groups which serves as the stationary phase of a chromatograph, eluting the compound with an aqueous acid and collecting distinct elution volumes representative of each isotope. In a preferred embodiment, the eluant is a strong mineral acid, such as hydrochloric acid and the chromatograph is of a type, such as a continuous annular chromatograph, that it can be operated in a continuous, steady state manner.Type: GrantFiled: July 19, 1990Date of Patent: May 5, 1992Assignee: Westinghouse Electric Corp.Inventors: Thomas S. Snyder, Ernest D. Lee
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Patent number: 5098678Abstract: The isotopes of zirconium can be partially or completely separated by loading an aqueous solution of an ionic compound of zirconium onto a cationic exchange resin which serves as the stationary phase of a chromatograph, eluting the compound with an aqueous acid and collecting distinct elution volumes representative of each isotope. In a preferred embodiment, the eluant is a strong mineral acid, such as hydrochloric acid and the chromatograph is of a type, such as a continuous annular chromatograph that it can be operated in a continuous, steady state manner.Type: GrantFiled: April 27, 1990Date of Patent: March 24, 1992Assignee: Westinghouse Electric Corp.Inventors: Ernest D. Lee, Thomas S. Snyder, Edward J. Lahoda
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Patent number: 5063032Abstract: Synthetic rutile is prepared from titaniferous slags containing alkaline-earth metal impurities, such as magnesium oxide, by a method comprising contacting the slag with chlorine at a temperature of at least about 800.degree. C., and then leaching the chlorine-treated slag with hydrochloric acid at a temperature of at least about 140.degree. C.Type: GrantFiled: March 27, 1990Date of Patent: November 5, 1991Assignee: QIT-Fer et Titane, Inc.Inventor: Michel Gueguin
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Patent number: 5049363Abstract: A process for extracting scandium from titanium ore includes the steps of: feeding the titanium ore to a fluidized bed chlorinator at about 1000.degree. C. to produce a vaporous (generally titanium and possible iron chlorides) phase and a scandium-containing residue; and recovering the scandium from the residue.In one practice, the scandium is recovered by leaching the residue with aqueous acid (e.g. HCl) to produce a scandium-containing aqueous solution, followed by contacting the aqueous solution with a polyalkyl phosphate-containing organic phase, the polyalkyl phosphate (e.g. tributyl phosphate) extracting scandium into the organic phase, followed by scandium precipitation by an ammonium addition to produce a scandium hydroxide precipitate and the scandium hydroxide is calcined, whereby scandium is recovered as an oxide. The residue generally also contains yttrium and lanthanides, and the yttrium and lanthanides can also be recovered from the residue as a part of the scandium recovery process.Type: GrantFiled: August 3, 1989Date of Patent: September 17, 1991Assignee: Westinghouse Electric Corp.Inventor: Robert J. Feuling
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Patent number: 5032556Abstract: A preparation method for zircon powder, which comprises heating a feed powder mixture comprising:(1) silica and zirconia obtained by subjecting a liquid having a pH of not higher than 8 and containing silica and zirconia in a SiO.sub.2 /ZrO.sub.2 molar ratio of substantially 1/1, to liquid-removing treatment, and(2) zircon in an amount of at least 0.1% by weight based on the total amount of said silica and zirconia,at a heating rate of not higher than 5.degree. C./min from 1,200.degree. C. to a calcination temperature, and maintaining it at a calcination temperature of from 1,300.degree. to 1,700.degree. C. for from 1.0 to 24 hours.Type: GrantFiled: February 20, 1990Date of Patent: July 16, 1991Assignee: Tosoh CorporationInventors: Toshiyuki Mori, Yoshitaka Kubota, Takashi Mitamura, Hidehiko Kobayashi
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Patent number: 5024740Abstract: A method and apparatus for the elimination of unwanted impurities and inclusions from a variety of non-conductive base materials by the application of high power, variable frequency RF energies in selective of rarefied atmospheres. Refined natural quartz is a product acquired by the method using the apparatus herein described.Type: GrantFiled: October 28, 1989Date of Patent: June 18, 1991Inventors: Stephen M. Birken, Karl Birken
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Patent number: 5009866Abstract: Continuous production of zirconium and/or hafnium metal from a fused salt bath in which one of the salts is zirconium and/or hafnium tetrachloride is carried out by feeding additional, make-up zirconium and/or hafnium tetrachloride powder into a zirconium and/or hafnium dissolution area of the bath maintained at a dissolution temperature below which the tetrachloride will vaporize, by circulating portions of the bath into and through a separate but contiguous area maintained at a temperature at which the tetrachloride will vaporize, and by recovering the vaporized tetrachloride. It is preferred that the vaporization area of the bath be wholly surrounded by and insulated from the dissolution area of the bath.Type: GrantFiled: November 16, 1989Date of Patent: April 23, 1991Assignee: Westinghouse Electric Corp.Inventor: Ernest D. Lee
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Patent number: 4941916Abstract: The invention relates to a process and apparatus for the supply of a Kroll reactor with zirconium tetrachloride vapor, in which zirconium chloride powder is vaporized in a sublimator by heating power and the vapor obtained is passed into the reactor. Part of the heating power applied in the sublimator is supplied to the powder by an internal heating means, and the remainder of the heating power is supplied to the wall of the sublimator by an external heating means. The heating power of the internal heating means is used for the sublimation of the zirconium tetrachloride powder and the heating power of the external means is applied in order to compensate the heat losses of the wall of the sublimator.Type: GrantFiled: March 21, 1988Date of Patent: July 17, 1990Assignee: Compagnie Europeenne Du Zirconium CezusInventors: Jean Boutin, Pierre Brun, Airy-Pierre Lamaze
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Patent number: 4933154Abstract: A ZrO.sub.2 powder of very fine particle size adapted especially for the making of high density ceramics is produced by chlorinating a zirconium source material, such as zircon sand, to produce crude ZrCl.sub.4 solids; the solids are dissolved to form a ZrOCl.sub.2 solution from which ZrOCl.sub.2 crystals are precipitated; the crystals are dried and milled to a desired particle size; and the crystal particles are subjected to direct oxidation under controlled conditions to produce a very fine ZrO.sub.2 powder especially adapted to the making of high density ceramics.Type: GrantFiled: January 30, 1987Date of Patent: June 12, 1990Assignee: Westinghouse Electric Corp.Inventor: Young J. Kwon
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Patent number: 4923577Abstract: This is a method of reducing zirconium chloride to a metal product by introducing zirconium chloride into a molten salt bath containing at least one alkali metal chloride and at least one alkaline earth metal chloride; and electrochemically reducing alkaline earth metal chloride to a metallic alkaline earth metal in the molten salt bath, with the reduced alkaline earth metal reacting with the zirconium chloride to produce zirconium metal. By using this electrochemical-metallothermic reduction, zirconium metal is produced and insoluble subchlorides of zirconium in the metal product are generally avoided.Preferably, the molten salt in the molten salt bath consists essentially of a mixture of lithium chloride, potassium chloride, magnesium chloride and zirconium or hafnium chloride.Type: GrantFiled: September 12, 1988Date of Patent: May 8, 1990Assignee: Westinghouse Electric Corp.Inventors: David F. McLaughlin, Francis Talko
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Patent number: 4917773Abstract: The process and the device according to the invention relate to the introduction, at a stable, known flow rate, of sublimable tetrachloride into a column for continuous extractive distillation under pressure of the chlorides. The sublimable tetrachloride is dissolved in a hot dissolver in a liquid solvent such as KAlCl.sub.4, and is then recirculated by pump at a stable, known flow rate into an evaporator connected to the column. The solution is then heated in an evaporator in order to sublime the majority of the product which it contains, the sublimed vapors thus passing into the column at a stable, known flow rate. The process according to the invention is adapted, in particular, to a plant for the production of ArCl.sub.4 of nulear purity and of HfCl.sub.4.Type: GrantFiled: March 6, 1989Date of Patent: April 17, 1990Assignee: Compagnie Europeenne Du Zirconium CezusInventors: Pierre Brun, Jean Guerin
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Patent number: 4917872Abstract: A method for producing titanium fluoride comprises: a dissolution process, wherein iron-containing titanium material is dissolved in solutions containing hydrofluoric acid, fluoride solutions being produced; a first crystallization and separation process, wherein ferric fluoride is crystallized and ferric fluoride crystals thus obtained are separated from the fluoride solutions by cooling the fluoride solutions, crude titanium fluoride solutions being produced; a second crystallization and separation process, wherein a mixed salt of (NH.sub.4).sub.2 TiF.sub.6 and (NH).sub.3 FeF.sub.6 is crystallized and separated by mixing ammonium fluoride solutions with the crude titanium fluoride solutions to obtain a mixture and concentrating the mixture; a first pyrolysis process, wherein the ammonium fluoride salt is pyrolyzed at a temperature of from 300.degree. to 800.degree. C. in a stream of dry gas after having dried the ammonium fluoride, solid ferric fluoride (FeF.sub.3) and gaseous TF.sub.4, HF and NH.sub.Type: GrantFiled: November 25, 1988Date of Patent: April 17, 1990Assignee: NKK CorporationInventors: Keisuke Nakahara, Hideyuki Yoshikoshi, Toshio Hinami, Takaho Kawawa
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Patent number: 4910009Abstract: The process for purifying a contaminated chloro, bromo or iodo precursor salt of zirconium, hafnium or aluminum by means of providing a molten thermal body of one or more alkali or alkaline earth metal halides and the precursor salt containing impurities, maintaining the body at a temperature sufficient to volatilize the precursor salt away from its impurities while effecting a reducing condition in the body by means of a fluid, mobile reducing agent which is non-reducing of said precursor salt, and isolating the purified volatilized precursor salt from the body. The ultra purified isolated volatilized precursor salt can then be reacted with a fluorinating agent to produce the highly purified fluoride for use in optical fiber grade glass or the like.Type: GrantFiled: May 6, 1988Date of Patent: March 20, 1990Assignee: Teledyne Industries, Inc.Inventor: James A. Sommers
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Patent number: 4897116Abstract: The process for preparing zirconium, hafnium, vanadium, tantalum, or niobium metal comprising providing in first vessel means a eutectic solution of a chloro, bromo or iodo salt of zirconium or hafnium in a molten thermal body of one or more alkali or alkaline earth metal halides at a non-vaporizing temperature, transferring said eutectic solution to second vessel means, maintaining said second vessel means at a temperature sufficient to vaporize said salt, transferring the salt vapor independently to a bank of separately fed reduction crucibles, the supply of said eutectic solution to said second vessel means being maintained such that said salt vapor can be supplied substantially continuously to said crucibles in a selective manner dependent upon the operating status of each crucible.Type: GrantFiled: May 25, 1988Date of Patent: January 30, 1990Assignee: Teledyne Industries, Inc.Inventor: Randall L. Scheel
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Patent number: 4885019Abstract: Heavy metal fluoride glasses are made by a process that requires high purity fluoride constituent compounds fluorinated oxides, or premelted glass cullet. The charge is placed in an enclosed furnace chamber having the ability of atmosphere control, heat control and position control of the charge. In particular, an inert, or nonreactive atmosphere or air is used in the furnace chamber as well as an oxygen-scavenging metal therein. The oxygen-scavenging metal at the high temperature produces a controlled oxygen partial pressure so that the air is essentially inert and non-reactive although the presence of a slightly oxidizing atmosphere is still required to produce the glass. The charge is rapidly raised to its fusion temperature and held at the temperature for a short time in proximity to an oxygen-scavenging material. The charge is immediately removed from the heating source and quickly cooled through the critical crystallization region. The total heating and cooling time being less than one hour.Type: GrantFiled: January 28, 1988Date of Patent: December 5, 1989Assignee: The United States of America as represented by the Secretary of the Air ForceInventor: Joseph J. Hutta
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Patent number: 4865696Abstract: This is a process for removing phosphorus oxychloride from a complex of zirconium or hafnium chloride and phosphorus oxychloride utilizing a lithium-potassium chloride molten salt absorber vessel displacing phosphorous oxychloride from the complex, with a condenser which has the complex of zirconium or hafnium chloride and phosphorus oxychloride as the condensing fluid to scrub zirconium or hafnium chloride from the phosphorus oxychloride vapor released from the complex. The process uses at least one separate vessel to strip the zirconium or hafnium chloride from the lithium-potassium chloride molten salt.Type: GrantFiled: September 12, 1988Date of Patent: September 12, 1989Assignee: Westinghouse Electric Corp.Inventors: David F. McLaughlin, Richard A. Stoltz
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Patent number: 4842832Abstract: Ultra-fine spherical particles of a metal oxide having an average particle diameter of 40 nm or smaller can be prepared by a method in which a vaporizable metal compound is vaporized and decomposed under heating to give ultra-fine particles of a metal oxide followed by immediate cooling down to a temperature at which coalescence of the fine particles are prevented from coalescence. The fine particles have characteristics such as an excellent power of ultraviolet scattering.Type: GrantFiled: March 21, 1988Date of Patent: June 27, 1989Assignee: Idemitsu Kosan Company LimitedInventors: Hakuai Inoue, Hiroshi Komiyama
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Patent number: 4840774Abstract: A process for the production of zirconium tetrachloride from dissociated zircon in which gaseous chlorine is passed through pellets consisting of ground dissociated zircon, carbon and a binder at a temperature in the range of from 450.degree. to 800.degree. C. The zirconium tetrachloride produced contains less than about 0.22% by weight, calculated as SiO.sub.2, of silicon tetrachloride.Type: GrantFiled: June 26, 1987Date of Patent: June 20, 1989Assignee: Tam Ceramics Inc.Inventors: John S. Campbell, Brian N. Baker, Anil Katyal