Binary Fluorine Containing Compound Patents (Class 423/489)
  • Patent number: 5543120
    Abstract: Hazardous and carcinogenic asbestos waste characterized by a crystalline fibrous structure is transformed into non-carcinogenic, relatively nonhazardous, and non-crystalline solid compounds and gaseous compounds which have commercial utilization. The asbestos waste is so transformed by the complete fluorination of the crystalline fibrous silicate mineral defining the asbestos.
    Type: Grant
    Filed: July 21, 1994
    Date of Patent: August 6, 1996
    Assignee: The United States of America as represented by the United States Department of Energy
    Inventor: Thomas W. Selby
  • Patent number: 5470559
    Abstract: A process for recycling spent potlining material from aluminum reduction cells contaminated with fluoride and aluminum values. The process comprises first reducing the average particle size of the spent potlining material to smaller than 28 Tyler mesh to form a powder. The powder is then treated with an aqueous sodium hydroxide solution containing about 10 to 60 g/L of sodium hydroxide at a temperature in the range of between 60.degree. and 90.degree. C. to form a solution containing fluoride and sodium aluminate and a residual solid. The solution is removed from the residual solid and the content of NaOH is adjusted in the solution to the range of about 10 to 60 g/L of NaOH, if the content differs from this range, to produce a solution suitable for cyanide destruction. This solution is then heated to a temperature in the range of about 160.degree. to 220.degree. C. at a pressure in the range of about 150 to 350 p.s.i. for a time of between about 1/2 and 3 hours to destroy cyanide values in the solution.
    Type: Grant
    Filed: February 26, 1993
    Date of Patent: November 28, 1995
    Assignee: Alcan International Limited
    Inventors: Robert J. Grolman, George C. Holywell, Frank M. Kimmerle, Gilles R. Turcotte
  • Patent number: 5449503
    Abstract: The present invention provides a process for recovering arsenic acid from a starting mixture comprising sulfuric and arsenic acids and water. In step (a), the starting mixture is treated with a sulfur (IV) compound which will reduce the arsenic acid to arsenic (III) compound under conditions sufficient to substantially convert the arsenic acid to arsenic (III) wherein the resulting mixture comprises arsenic (III) compound, the sulfur (IV) compound, sulfuric acid, and water. In step (b), the resulting mixture is purged with gas to substantially remove the sulfur (IV) compound from the mixture wherein the purged mixture comprises the arsenic (III) compounds, sulfuric acid, and water. In step (c), the purged mixture is treated under conditions sufficient to substantially separate the arsenic (III) compounds from the purged mixture.
    Type: Grant
    Filed: August 26, 1994
    Date of Patent: September 12, 1995
    Assignee: AlliedSignal Inc.
    Inventors: Charles L. Redmon, Somanahalli N. Subbanna, Robert A. Smith
  • Patent number: 5417954
    Abstract: New crystalline phases of the fluoroaluminum compounds NH.sub.4 AlF.sub.4 and AlF.sub.3 and processes for their preparation are disclosed.
    Type: Grant
    Filed: March 2, 1994
    Date of Patent: May 23, 1995
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: Richard L. Harlow, Norman Herron
  • Patent number: 5417948
    Abstract: There is disclosed a process for cleaning a gas containing a nitrogen fluoride especially nitrogen trifluoride as the harmful component which comprises bringing the gas into contact with a cleaning agent comprising zirconium or a zirconium-based alloy such as Zr-Fe, Zr-Cu, Zr-Ni, Zr-Al, Zr-Mg, Zr-Ca, Zr-Zn, Zr-La and Zr-Ce to remove the harmful component at 100.degree. to 800.degree. C., especially 150.degree. to 500.degree. C. The process is capable of efficiently removing nitrogen fluoride, especially nitrogen trifluoride at a relatively low temperature without generating a harmful byproduct such as nitrogen oxide, and thus exhibits excellent effect on the cleaning of exhaust gas from semiconductor manufacturing process, etc.
    Type: Grant
    Filed: October 28, 1993
    Date of Patent: May 23, 1995
    Assignee: Japan Pionics Co., Ltd.
    Inventors: Keiichi Iwata, Toshiya Hatakeyama
  • Patent number: 5411726
    Abstract: The invention relates to a process for purifying industrial anhydrous hydrogen fluoride by means of oxygen difluoride.
    Type: Grant
    Filed: January 31, 1994
    Date of Patent: May 2, 1995
    Assignee: Bayer AG
    Inventors: Andreas Bulan, Rainer Weber, Hans-Dieter Block, Hans-Heinrich Moretto
  • Patent number: 5352419
    Abstract: Process for the recovery of aluminum and fluoride values from spent pot lining materials comprising the steps of calcining spent pot lining material to produce an ash having environmentally acceptable levels of cyanide contamination, subjecting the ash to a leaching step in a solution containing a mineral acid and a corresponding aluminum salt in such proportions as to dissolve the aluminum and fluoride values, and subjecting the leached liquid to thermal hydrolysis to cause precipitation of an aluminum fluoride product.
    Type: Grant
    Filed: June 15, 1993
    Date of Patent: October 4, 1994
    Assignee: Comalco Aluminium Limited
    Inventor: David H. Jenkins
  • Patent number: 5348723
    Abstract: Semiconductor grade tungsten hexafluoride (WF.sub.6) is produced by reacting tungsten metal with a recirculating flow of gaseous WF.sub.6 containing a small concentration of fluorine in a heated reactor. The high purity WF.sub.6 produced is useful for deposition of tungsten metallization in fabricating VLSI integrated circuitry.
    Type: Grant
    Filed: February 7, 1990
    Date of Patent: September 20, 1994
    Assignee: Bandgap Technology Corporation
    Inventors: Bruce J. Sabacky, Robert E. Doane
  • Patent number: 5346684
    Abstract: A method is provided for recovering an anhydrous hydrogen fluoride product from uranium hexafluoride gas by initially reacting the uranium hexafluoride in a primary reactor with steam to produce a uranyl fluoride intermediate and a gaseous mixture of hydrogen fluoride and water. The uranyl fluoride intermediate is fed to a secondary reactor and reacted with water to produce a triuranium octoxide product for disposal, and a gaseous mixture of water, hydrogen fluoride and oxygen. The two mixtures from the primary and secondary reactors are combined and subsequently separated in a distillation column to obtain an anhydrous hydrogen fluoride product stream and an aqueous azeotropic recycle stream containing water and hydrogen fluoride which is vaporized and returned to the primary reactor as the steam feed.
    Type: Grant
    Filed: January 21, 1993
    Date of Patent: September 13, 1994
    Assignee: Sequoyah Fuels Corporation
    Inventor: James H. Mestepey
  • Patent number: 5340585
    Abstract: Compositions and methods which are effective to treat benign gynecological disorders for extended periods of time in women in who the risk of endometrial stimulation is minimized or absent are described, wherein an effective amount of a gonadotropin hormone releasing hormone composition and an effective amount of an estrogenic composition are provided over a period of time, optionally with addition of an androgenic composition.
    Type: Grant
    Filed: May 17, 1993
    Date of Patent: August 23, 1994
    Assignee: University of Southern California
    Inventors: Malcolm C. Pike, Darcy V. Spicer
  • Patent number: 5336480
    Abstract: In a process utilizing steam, the method of producing at least a portion of said steam includes heating a solid substance so as to generate steam, followed by capturing the generated steam at a pressure greater than one atmosphere gage pressure for use in the process at a pressure greater than one atmosphere gage pressure. Suitable solid substances are aluminum hydrate or aluminum fluoride. New hydrated aluminum containing products and uses for those products are obtained by the use of the process.
    Type: Grant
    Filed: June 26, 1992
    Date of Patent: August 9, 1994
    Assignee: Aluminum Company of America
    Inventors: Chanakya Misra, Steven W. Sucech
  • Patent number: 5324498
    Abstract: A process is provided for purifying liquid tungsten hexafluoride containing volatile and non-volatile impurities. The process comprises the steps of evaporating tungsten hexafluoride from non-volatile impurities dissolved in liquid tungsten hexafluoride and condensing the evaporated tungsten hexafluoride. The condensed tungsten hexafluoride is subjected to freezing to solidify the tungsten hexafluoride. Volatile impurities are then evacuated from the solid tungsten hexafluoride. Thereafter, the solid tungsten hexafluoride is thawed to liquid tungsten hexafluoride to release trapped volatile impurities and then heated to a temperature above the boiling point of tungsten hexafluoride under pressure in a closed container. The volatile impurities dissolved in the thawed tungsten hexafluoride are removed and collected above the thawed tungsten hexafluoride and vented into an evacuated space.
    Type: Grant
    Filed: March 30, 1990
    Date of Patent: June 28, 1994
    Assignee: Bandgap Chemical Corporation
    Inventors: Barry J. Streusand, Don A. Almond, Robert E. Doane
  • Patent number: 5290730
    Abstract: A radiation wavelength conversion device is implemented in the form of a waveguide that includes a single crystal halide-based cladding layer, and a halide-based active layer. The active layer has a greater refractive index than the cladding layer, is approximately lattice matched with the cladding layer, and includes a dopant that causes it to respond to input radiation at one wavelength by emitting radiation at a different wavelength. The active layer can either form part of a laser resonator cavity, or can operate through spontaneous emission. It is preferably about 3.5-5 microns thick to induce single-mode propagation, and can be divided into separate waveguiding channels to limit beam fanning. The device is operable at room temperature, and can be fabricated using conventional microelectronics techniques.
    Type: Grant
    Filed: September 10, 1992
    Date of Patent: March 1, 1994
    Assignee: Hughes Aircraft Company
    Inventors: Ross A. McFarlane, Mark Lui
  • Patent number: 5277889
    Abstract: Metal halide compositions of enhanced purity are produced by vapor phase deposition via reactions involving organometallic starting materials in a process wherein a carbon getter is provided in the reaction zone and/or adjacent the developing metal halide deposit. The carbon getter reduces carbon contamination in the product which can result from side decomposition reactions involving the organometallic starting materials.
    Type: Grant
    Filed: May 13, 1985
    Date of Patent: January 11, 1994
    Assignee: Corning Incorporated
    Inventors: Joseph M. Power, Ahmad Sarhangi
  • Patent number: 5236690
    Abstract: A chemical vapor purification process for preparing metal fluorides. The process involves melting a metal selected from the metals forming fluorides suitable for use in fluoride glass and thermodynamically partitionable from cation contaminants, for example aluminum, gallium, or indium. Chlorine, bromine, or iodine is bubbled through a stoichiometric excess of the melt, under reaction conditions selected to result in generation of a gaseous halide of the metal. The gaseous halide is then isolated from the melt and reacted with a gaseous fluorinating agent to form a solid fluoride of the metal.
    Type: Grant
    Filed: January 31, 1991
    Date of Patent: August 17, 1993
    Assignee: GTE Laboratories Incorporated
    Inventors: Robert C. Folweiler, Barry C. Farnsworth
  • Patent number: 5234679
    Abstract: A method of refining tungsten hexafluoride containing molybdenum hexafluoride as an impurity includes the step of contacting the tungsten hexafluoride with at least one metal selected from the group consisting of Mo, W, Cu, Ni, Fe, Co, Zn, Ti, Al, Ca and Mg at a temperature ranging from 100.degree. to 500.degree. C. Molybdenum hexafluoride is efficiently removed from the tungsten hexafluoride by the method.
    Type: Grant
    Filed: April 10, 1992
    Date of Patent: August 10, 1993
    Assignee: Central Glass Company, Limited
    Inventors: Takashi Suenaga, Mitsuya Ohashi, Takashi Yoneda, Yoshiyuki Kobayashi
  • Patent number: 5207999
    Abstract: A compound MF.sub.n, where M is a metal and n is the valency of the metal and has a value between 1 and 6, is subjected to a thermal plasma at a temperature in excess of 3000 K to dissociate it into the metal and fluorine. Also present in the reactor is an added reactant that will react with the metal or the fluorine to prevent their recombination so that there is formed fluorine gas or a fluoride other than the fluoride of the metal M.
    Type: Grant
    Filed: August 13, 1991
    Date of Patent: May 4, 1993
    Assignee: Cameco Corporation
    Inventors: Robert C. Burk, Maher I. Boulos, Dennis G. Garratt, Tadeusz W. Zawidzki, Andrzej Huczko
  • Patent number: 5130146
    Abstract: A colloidal solution comprises a fluoride(s) being difficultly soluble in water comprises colloidal particles of the fluoride having a particle size of 0.005 to 1 micron, said fluoride having a fluoride ion concentration of 1 to 10,000 ppm in the state of saturation.
    Type: Grant
    Filed: June 10, 1991
    Date of Patent: July 14, 1992
    Assignee: Kao Corporation
    Inventors: Satoshi Tsujita, Manabu Tonomura, Shigeto Kayane, Takashi Imamura
  • Patent number: 5091168
    Abstract: A method of producing an anhydrous niobium or tantalum pentafluoride involving reacting the corresponding pentoxide or oxyhalide with an excess of anhydrous hydrogen fluoride in the presence of a sufficient dehydrating agent (e.g., COCl.sub.2, SOCl.sub.2 or SO.sub.2 Cl.sub.2) to react with any water formed. Such a process is useful to produce a catalyticallyactive anhydrous niobium or tantalum pentafluoride in essentially a single liquid phase reaction step.
    Type: Grant
    Filed: August 15, 1990
    Date of Patent: February 25, 1992
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Mario J. Nappa
  • Patent number: 5076839
    Abstract: Feed mixtures containing one or more platinum group metals are fluorinated to form at least one volatile fluoride product which is separated from the residual solid. Separations of different fluorides may be effected by collecting different fractions of volatile fluorides. Palladium does not form a volatile fluoride and is retained in the residual solid.
    Type: Grant
    Filed: June 12, 1990
    Date of Patent: December 31, 1991
    Assignee: Johnson Matthey Public Limited Company
    Inventors: David A. Boyd, John H. Holloway, Gillian Stanger
  • Patent number: 5069701
    Abstract: A fluoride glass is prepared by depositing a solid including a metal fluoride on a heated substrate, from a gaseous mixture of a nonmetallo-organic compound, carbon dioxide, and a source of carbonyl fluoride. The nonmetallo-organic compound contains the metallic cation of the metal fluoride bonded to an organic species through an electronegative element such as oxygen, but not directly to a carbon atom. The carbon dioxide, or optionally another species reactive with carbon to produce a gas, oxidizes solid carbon and other reduction products of the organic compound that could otherwise be present in the deposited metal fluoride to impair optical properties of the fluoride glass. The carbonyl fluoride, supplied by the gas itself or by reactants that produce the gas, reacts with the nonmetallo-organic compound without producing water, which would otherwise degrade the glass purity.
    Type: Grant
    Filed: February 23, 1990
    Date of Patent: December 3, 1991
    Assignee: Hughes Aircraft Company
    Inventors: Ricardo C. Pastor, Luisa E. Gorre
  • Patent number: 5045300
    Abstract: A process comprising the reaction of an amine.aluminum trichloride complex and a bifluoride compound to produce an aluminum fluoride compound. Exemplary processes include the reaction of AlCl.sub.3.N(CH.sub.2 CH.sub.3) and NH.sub.4 HF.sub.2 or NaHF.sub.2 to respectively produce NH.sub.4 AlF.sub.4 or Na.sub.5 Al.sub.3 F.sub.14.
    Type: Grant
    Filed: October 23, 1990
    Date of Patent: September 3, 1991
    Assignee: Ethyl Corporation
    Inventor: Everett M. Marlett
  • Patent number: 5013534
    Abstract: Morphologically improved, aggregated, monodispersed rare earth trifluoride particulates having a controlled and narrow grain size distribution, and a mean diameter of less than 1 .mu.m, are prepared by (i) reacting an aqueous solution of a rare earth salt with a solution of ammonium fluoride, (ii) separating the precipitate thus formed, and (iii) heat treating the separated precipitate.
    Type: Grant
    Filed: June 30, 1989
    Date of Patent: May 7, 1991
    Assignee: Rhone-Poulenc Chimie
    Inventors: Antoine Dissaux, Jean-Luc Le Loarer
  • Patent number: 4983373
    Abstract: High purity metal fluorides (ZrF.sub.4, HfF.sub.4, AlF.sub.3) are produced by incomplete reaction of metal or their compounds with elemental fluorine and subsequent elevated temperature sublimation of the metal fluoride from the reaction products wherein unreacted metal or metal compounds act as "getters" to convert volatile impurity metal fluorides to non-volatile metals or metal compounds.
    Type: Grant
    Filed: November 23, 1988
    Date of Patent: January 8, 1991
    Assignee: Air Products and Chemicals, Inc.
    Inventors: Howard P. Withers, Jr., Andrew J. Woytek, John T. Lileck
  • Patent number: 4965055
    Abstract: Metal halides are ultrapurified by selective complexation with a complexing gent to form a charged first complex. A ligand forms an oppositely charged second complex with metallic impurities in the metal halide to be purified. A solution containing these complexes is then passed through an ion exchange column and the desired purified metal halide collected. The present method is particularly useful in the production of ultrapure metal halides, such as zirconium fluorinate, for metallic glasses.
    Type: Grant
    Filed: March 27, 1990
    Date of Patent: October 23, 1990
    Assignee: The United States of America as represented by the Secretary of the Navy
    Inventors: Paul E. R. Nordquist, Jr., Arnold H. Singer
  • Patent number: 4960581
    Abstract: The method for preparing a gaseous metallic floride is here disclosed which comprises reacting a metal or its oxide with a fluorine gas or nitrogen trifluoride gas, the aforesaid method being characterized by comprising the steps of mixing the metal or its oxide with a molding auxiliary comprising a solid metallic fluoride which does not react with fluorine and nitrogen trifluoride; molding the resulting mixture under pressure; and contacting the molded pieces with the fluorine gas or nitrogen trifluoride gas, while the molded pieces are heated.
    Type: Grant
    Filed: March 13, 1989
    Date of Patent: October 2, 1990
    Assignee: Mitsui Toatsu Chemicals, Inc.
    Inventors: Isao Harada, Yukihiro Yoda, Naruyuki Iwanaga, Toshihiko Nishitsuji, Akio Kikkawa
  • Patent number: 4957661
    Abstract: Improved graphite fluoride fibers are produced by contact reaction between highly graphitized fibers and fluorine gas. It is preferable to intercalate the fibers with bromine or fluorine and metal fluoride prior to fluorination.These graphite fluoride fibers are bound by an epoxy. The resulting composites have high thermal conductivity, high electric resistivity, and high emissivity.
    Type: Grant
    Filed: September 30, 1988
    Date of Patent: September 18, 1990
    Assignee: The United States of America as represented by the United States National Aeronautics and Space Administration
    Inventor: Ching-Cheh Hung
  • Patent number: 4938945
    Abstract: Anhydrous ferric fluoride of 99.0% purity or greater, based upon F.sup.- analysis is afforded, as well as a process for its manufacture using anhydrous FeCl.sub.3 and liquid anhydrous HF, reacted in the substantial absence of O.sub.2, H.sub.2 O, or an oxidizing agent.
    Type: Grant
    Filed: October 18, 1988
    Date of Patent: July 3, 1990
    Assignee: Pennwalt Corporation
    Inventors: Tariq Mahmood, Charles B. Lindahl, Ronald E. Davis
  • Patent number: 4927616
    Abstract: A process is provided wherein tertiary ammonium trichlorosilyl, a complexing tertiary amine, and an alkali metal aluminum tetrahydride are reacted together in molar proportion of about 1:2:3, such that silane and tertiary amine alane are produced. Tertiary ammonium trichlorosilyl may be pre-formed or formed in situ by the reaction of trichlorosilane and tertiary amine. Yields are dramatically higher when the process is conducted in the presence of a tris(polyalkoxyalkyl)amine phase transfer catalyst.A sequential process is also provided for the preparation of silane and aluminum trifluoride. In the first part of this sequence, silane and tertiary amine alane are produced as described above. In the second part of the sequence, silicon tetrafluoride is reacted with the amine alane, producing additional silane and aluminum trifluoride.
    Type: Grant
    Filed: October 2, 1989
    Date of Patent: May 22, 1990
    Assignee: Ethyl Corporation
    Inventor: Everett M. Marlett
  • Patent number: 4923507
    Abstract: The subject of the invention is a process for opening ores, particularly ores containing tantalum, niobium, zirconium and titanium, of the kind that includes the stages of leaching with mineral acids, solvent extraction, purification and separation of the products obtained, characterized by the fact that initially, instead of leaching with sulfuric acid and hydrofluoric acid being performed as a first stage, the original ore concentrate is melted together with fluorite (CaF.sub.2), followed by milling of the melting product obtained and subsequently leaching with concentrated sulfuric acid, followed by extraction of the soluble species using solvents, separation and purification of the products obtained.
    Type: Grant
    Filed: May 19, 1988
    Date of Patent: May 8, 1990
    Assignee: Mamore Mineracao E Metalurgia S/A
    Inventor: Egberto Silva, Filho
  • Patent number: 4917872
    Abstract: 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: Grant
    Filed: November 25, 1988
    Date of Patent: April 17, 1990
    Assignee: NKK Corporation
    Inventors: Keisuke Nakahara, Hideyuki Yoshikoshi, Toshio Hinami, Takaho Kawawa
  • Patent number: 4889695
    Abstract: Disclosed in a process for recovering aluminum flouride, caustic, and carbon from spent potlining retrieved from an aluminum electrolytic reduction cell. Spent potlining is treated by leaching with a caustic solution to produce a fluoride-rich basic liquor and carbonaceous solid residue followed by contacting the carbonaceous solid with an acid bath of aluminum sulfate and sulfuric acid to produce a fluoride-rich acid liquor.
    Type: Grant
    Filed: February 20, 1985
    Date of Patent: December 26, 1989
    Assignee: Aluminum Company of America
    Inventor: J. Finley Bush
  • Patent number: 4859444
    Abstract: Graphite fluoride in the form of submicron particles is easily obtained at high yield by using, exclusively, acetylene black as the carbon material to be fluorinated with fluorine gas. Use of any other type of carbon black does not give comparable results. Graphite fluoride produced from acetylene black is superior in dispersibility.
    Type: Grant
    Filed: February 26, 1988
    Date of Patent: August 22, 1989
    Assignee: Central Glass Company, Limited
    Inventors: Yasushi Kita, Shirou Moroi
  • Patent number: 4857294
    Abstract: A process for the preparation of metal fluorides usable for the production of fluoride glasses consists of reacting in an organic liquid medium, such as toluene, (a) a compound of said metal chosen from among the gaseous compounds thereof, the compounds of said metal soluble in the organic liquid medium and the compounds of said metal in solution in an organic solvent miscible with said medium, and (b) a fluorinating agent chosen from among the gaseous fluorinating agents, the fluorinating agents which are partly soluble in the organic medium and the fluorinating agents which are partly soluble in an organic solvent miscible with said medium, to form a fluoride of said metal, the organic liquid medium being such that it reacts neither with the compound of the metal, nor with the fluorinating agent and does not dissolve the fluoride formed. To prepare the zirconium tetrafluoride, it is possible to introduce in toluene, gaseous Zr(BH.sub.4).sub.
    Type: Grant
    Filed: July 22, 1987
    Date of Patent: August 15, 1989
    Assignee: Commissariat A L'Energie Atomique
    Inventors: Martine Bridenne Alaux, Hubert Marquet-Ellis, Nelly Keller, Gerard Folcher, deceased
  • Patent number: 4857293
    Abstract: This invention provides a method for the preparation of ultrapure active metal fluorides of increased purity from their metal oxides by reacting an active metal with a predetermined amount of HF(aq) to form a solid reaction product which is dried under controlled heating to form a hydrated fluoride. This hydrated active metal fluoride is then subjected to reactive atmosphere processing comprising hydrofluoric acid vapor in a CO.sub.2 reactive carrier gas and a selected halide compound in the gas phase for a predetermined period of time to further increase anion purity.
    Type: Grant
    Filed: October 15, 1987
    Date of Patent: August 15, 1989
    Assignee: Hughes Aircraft Company
    Inventors: Ricardo C. Pastor, Luisa E. Gorre
  • Patent number: 4855121
    Abstract: This invention relates to a continuous process for the preparation of carbon polymonofluoride.The reaction of fluorine diluted with at least one inert gas with carbon particles is performed in a reaction zone in which the particles travel as a thin layer. Diluted fluorine is introduced into the reaction zone in the form of a plurality of gaseous mixtures delivered at a plurality of points close to the layer of the particles and distributed in the reaction zone. The weight content of fluorine and the flow rate of each of the gaseous mixtures are controlled independently and such that the volume content of fluorine in the gaseous phase at the gaseous phase/particles interface in the vicinity of each of the points is lower than the minimum content causing the inflammation of the particles.For a space time output higher than 10 kg.h.sup.-1 m.sup.
    Type: Grant
    Filed: December 23, 1987
    Date of Patent: August 8, 1989
    Assignee: Societe ATOCHEM
    Inventor: Jean Metzger
  • Patent number: 4853205
    Abstract: Process of using supercritical fluid to selectively separate, purify and recover metal halides.
    Type: Grant
    Filed: March 12, 1987
    Date of Patent: August 1, 1989
    Assignee: The United states of America as represented by the Secretary of the Interior
    Inventors: William K. Tolley, Alton B. Whitehead
  • Patent number: 4830842
    Abstract: A multistage process for preparing pure BF.sub.3 from hexafluorosilicic acid, H.sub.2 SiF.sub.6, comprises reacting H.sub.2 SiF.sub.6 with oxygen acids of boron and/or boron oxide in the first stage to give hydroxyfluoroboric acid and silica, filtering off the silica and concentrating the hydroxyfluoroboric acid, adding oleum to the concentrate and then heating to form gaseous BF.sub.3.
    Type: Grant
    Filed: February 5, 1988
    Date of Patent: May 16, 1989
    Assignee: BASF Aktiengesellschaft
    Inventors: Bernd Leutner, Hans H. Reich
  • Patent number: 4804390
    Abstract: A process for removing mineral impurities such as metal oxides from coal and shale oil structures is disclosed. The process is carried out by subjecting crushed coal or shale to a hydrocarbon fluoride leaching solution, separating the HF leach liquor from the coal or shale, washing the coal or shale with water, leaching the washed coal or shale with hydrogen chloride solution, separating the HCl leach liquor from the coal or shale, washing the coal or shale with water, and removing residual impurities from the treated coal or shale by heating under a vacuum. The process allows for the recovery of carbons and hydrocarbons of high purity from coal or shale which do not require expensive emission control equipment when combusted.
    Type: Grant
    Filed: July 30, 1984
    Date of Patent: February 14, 1989
    Inventors: Robert Lloyd, Maxwell J. Turner
  • Patent number: 4795624
    Abstract: The preparation of carbon fluoride and carbon fluoride chloride from a graphite intercalate is described. Treatment of group V-A pentahalide intercalates of graphite with fluorine or fluorine/chlorine gas mixtures at a temperature of about 300.degree. C. results in the production of highly fluorinated CF.sub.x ; X.gtoreq.1 or (C.sub.y F.sub.x Cl.sub.z).sub.n ;x.gtoreq.1.0, y=1.In the process, carbon fluoride or carbon fluoride chloride can be prepared from a highly ordered graphitic carbon at a temperature substantially lower than that of the decomposition temperature of the product, CF.sub.x or (C.sub.y F.sub.x Cl.sub.z).sub.n. In particular, carbon fluoride or carbon fluoride chloride is prepared from a group V-A pentahalogen intercalate and fluorine gas or fluorine/chlorine gas mixtures at temperatures in the order of 250.degree.-300.degree. C.
    Type: Grant
    Filed: April 28, 1988
    Date of Patent: January 3, 1989
    Assignee: Allied-Signal Inc.
    Inventor: David Nalewajek
  • Patent number: 4791038
    Abstract: Voltage suppression is an important problem in the Li/CF.sub.x battery system. The voltage that a Li/CF.sub.x battery will deliver just after the circuit has been closed can be as low as the voltage near the end of battery life. Electronic circuitry powered by Li/CF.sub.x batteries are complicated by the need to design around this problem.The processing of fluorinated carbon (CF.sub.x) to lower the initial voltage suppression is disclosed wherein fluorinated carbon is treated with a Group IA metal-alkyl or -aryl compound. The reaction between these compounds (e.g., n-butyl lithium) and the fluorinated carbon produces a battery grade product which undergoes reduced to almost no suppression of the initial closed circuit voltage.
    Type: Grant
    Filed: October 9, 1986
    Date of Patent: December 13, 1988
    Assignee: Allied-Signal Inc.
    Inventors: George A. Shia, David Nalewajek, Michael F. Pyszczek
  • Patent number: 4765968
    Abstract: A means to eliminate the suppression of the closed circuit voltage of a Li/CF.sub.x battery during the initial part of its discharge is effected by blending an additive CF.sub.x which does not show significant voltage suppression with the (bulk) CF.sub.x that is normally used in fabricating cathodes for such batteries. Blending is used to get a mixture which has substantially minimized voltage suppression and has good capacity.The closed circuit voltage of a Li/CF.sub.x battery during the initial 10% of discharge is known to be lower than the closed circuit voltage during the later stages. This characteristic adversely impacts applications since the voltage at beginning of life is as low as the voltage indicating end of life, complicating design of circuitry to indicate end of life.In the disclosure, the material with no significant voltage suppression discharges preferentially at the beginning of discharge leading to higher voltage and no suppression.
    Type: Grant
    Filed: June 8, 1987
    Date of Patent: August 23, 1988
    Assignee: Allied-Signal Inc.
    Inventors: George A. Shia, David J. Friedland
  • Patent number: 4757154
    Abstract: Process for the preparation of silane and a tertiary amine alane, said process comprising reacting:(a) an alkali metal aluminum tetrahydride having the formula MAlH.sub.4, wherein M is an alkali metal selected from the class consisting of lithium, sodium and potassium,(b) silicon tetrachloride, and(c) a complexing tertiary amine, such that the molar proportion of (a) to (b) to (c) is about 4:1:4.In this process, NaAlH.sub.4 and triethylamine are preferred reactants. The amine alane product can be reacted with additional silicon halide to prepare additional silane. This step can be conducted utilizing amine alane in the reaction mixture produced by the process above, and is preferably conducted using SiF.sub.4 as the silicon tetrahalide to produce AlF.sub.3 as a co-product. Both AlF.sub.3 and silane are valuable articles of commerce.
    Type: Grant
    Filed: November 4, 1986
    Date of Patent: July 12, 1988
    Assignee: Ethyl Corporation
    Inventors: Everett M. Marlett, Frederick W. Frey
  • Patent number: 4753786
    Abstract: There is disclosed a method for producing a graphite fluoride for use in an electrochemical cell of the type having as the negative electrode a light metal, such as an alkali metal, an electrolyte in which the negative electrode is not dissolved, and a positive electrode which has, as an active material, a graphite fluoride produced by fluorinating a decomposition residual carbon which has been obtained by decomposing a covalent intercalation compound. The electrochemical cell of the present invention exhibits high discharge potential and low overvoltage, and excellent discharge characteristics with respect to the flatness of discharge voltage, discharge capacity and shelf-life.
    Type: Grant
    Filed: February 3, 1987
    Date of Patent: June 28, 1988
    Assignee: Nobuatsu Watanabe
    Inventors: Nobuatsu Watanabe, Tsuyoshi Nakajima, Rika Hagiwara
  • Patent number: 4752454
    Abstract: This invention provides a method for the preparation of ultrapure active metal fluorides of increased purity from their metal oxides by reacting an active metal with a predetermined amount of HF(aq) to form a solid reaction product which is dried under controlled heating to form a hydrated fluoride. This hydrated active metal fluoride is then subjected to reactive atmosphere processing comprising hydrofluoric acid vapor in a CO.sub.2 reactive carrier gas and a selected fluoride compound in the gas phase for a predetermined period of time to further increase anion purity.
    Type: Grant
    Filed: December 27, 1984
    Date of Patent: June 21, 1988
    Assignee: Hughes Aircraft Company
    Inventors: Ricardo C. Pastor, Luisa E. Gorre
  • Patent number: 4741893
    Abstract: Process for producing fluorides of Mo, W, Nb, Ta, V, Re, Ti, Zr, Hf, Co, Ni, Cr, Sb, Sn, Zn, Pb, Al and rare earth metals comprising heating fluorine-containing ammonium salts of corresponding metals in a stream of an inert or reducing gas to convert them into fluorides of the metals.
    Type: Grant
    Filed: June 9, 1986
    Date of Patent: May 3, 1988
    Assignee: Solex Research Corporation of Japan
    Inventors: Morio Watanabe, Sanji Nishimura
  • Patent number: 4724200
    Abstract: Silver halide photographic emulsions are disclosed comprised of radiation sensitive silver halide grains of a cubic crystal lattice structure comprised of icositetrahedral crystal faces.
    Type: Grant
    Filed: July 3, 1986
    Date of Patent: February 9, 1988
    Assignee: Eastman Kodak Company
    Inventor: Joe E. Maskasky
  • Patent number: 4718929
    Abstract: A vapor phase method for making a metal halide material useful for the manufacture of an infrared transmitting optical waveguide fiber or other optical device, and the use of the method for making such a device, wherein a halogenated beta-diketonate of a metal to be incorporated in the device is converted to the corresponding metal halide by controlled decomposition of the halogenated diketonate, are described.
    Type: Grant
    Filed: October 21, 1983
    Date of Patent: January 12, 1988
    Assignee: Corning Glass Works
    Inventors: Joseph M. Power, Ahmad Sarhangi
  • Patent number: 4714604
    Abstract: A method of separating HF from a mixture including HF and HCl is disclosed wherein the mixture is contacted with silica causing the HF to react with the silica to form SiF.sub.4. The concentration of HCl is increased thereby increasing the relative volatility of SiF.sub.4 /HCl. The SiF.sub.4 is then removed as an aqueous distillate. The concentration of the HCl can be increased by various methods including adding gaseous or concentrated HCl to the mixture or by distilling off a portion of the water to thereby increase the concentration of the HCl. This method provides an efficient method of removing SiF.sub.4 and HF from HCl.
    Type: Grant
    Filed: August 13, 1986
    Date of Patent: December 22, 1987
    Assignee: The Dow Chemical Company
    Inventor: Robert S. Olson
  • Patent number: RE32777
    Abstract: A chemical vapor purification process for the preparation of high purity metal fluorides using the thermodynamic separation of cations by formation of a gaseous-metal-containing compound, vapor transport, and fluorination is disclosed.
    Type: Grant
    Filed: April 27, 1987
    Date of Patent: November 1, 1988
    Assignee: GTE Laboratories Incorporated
    Inventor: Robert C. Folweiler