Recovery Or Purification Patents (Class 423/488)
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Patent number: 4125593Abstract: Halogenated hydrocarbon materials are burned in an internally-fired horizontal fire-tube boiler and the heat of combustion directly produces saturated steam. Halogen values may be recovered from the combustion gases, e.g., by being absorbed in water. Thus halogenated hydrocarbon material which may need to be disposed of, is beneficially converted to energy and useful product.Type: GrantFiled: August 2, 1976Date of Patent: November 14, 1978Assignee: The Dow Chemical CompanyInventors: John C. Scheifley, Clark R. Shields, David E. Busby
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Patent number: 4119705Abstract: Hydrogen chloride and oxygen are contacted with a molten mixture of cuprous and cupric chloride in a oxidation reaction zone to enrich the cupric chloride content of the melt, and the melt introduced into a dechlorination zone wherein gaseous chlorine is removed from the melt. The oxidation reactor is operated at a pressure higher than the dechlorination reactor, and molten salt circulation rates are controlled in a manner such that the cupric chloride content and temperature of the salt introduced into the dechlorination reaction zone are higher than the cupric chloride concentration and temperature of the melt introduced into the oxidation reactor.Type: GrantFiled: April 6, 1977Date of Patent: October 10, 1978Assignee: The Lummus CompanyInventors: Herbert Riegel, Vincent A. Strangio
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Patent number: 4115531Abstract: Hydrochloric acid having a substantially constant HCl content of 20 to 36% is produced continuously by removing hydrogen chloride from hot combustion gas. To this end, hot combustion gas containing 1 to 10% by volume of HCl and steam, this gas being obtained by the joint combustion of off-gases containing chlorinated hydrocarbons and liquid residues of chlorinated hydrocarbons, is introduced into a quenching zone, and quenched therein, down to a temperature lower than its dew point, by means of cooled hydrochloric acid containing hydrogen chloride in a concentration of 20 to 36%, which concentration corresponds to the concentration of the hydrochloric acid which is to be produced. The resulting gas-liquid mixture is separated in an absorption cooling zone into cooled hydrochloric acid and cooled combustion gas containing 0.1 to 1% by volume of HCl.Type: GrantFiled: July 29, 1977Date of Patent: September 19, 1978Assignee: Hoechst AktiengesellschaftInventors: Wolfgang Opitz, Hans Hennen
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Patent number: 4115530Abstract: Process for the production of gaseous hydrogen chloride by extraction of dilute aqueous hydrochloric acid with amines.(a) The aqueous hydrochloric acid is extracted with an amine or with a mixture of an amine and an inert organic solvent which is immiscible with water and has a lower boiling point than the amine employed, the amines utilized being tertiary alkyl amines, tertiary aryl dialkyl amines, secondary arylalkyl amines, primary alkylaryl amines, or mixtures thereof, which contain 14-32 carbon atoms in the nitrogen-bound side chains, and among these at most one nitrogen-bound methyl group and at least one aliphatic residue containing at least 6 carbon atoms, and wherein the acid constant K.sub.a of the amine is smaller than 10.sup.-3.(b) An inert, water-immiscible organic solvent which has a lower boiling point than the amine employed is added to the extract, unless the solvent has already been added in stage (a).Type: GrantFiled: July 14, 1977Date of Patent: September 19, 1978Assignee: Chemische Werke Huls AGInventors: Alfred Coenen, Kurt Kosswig, Gunter Prominski
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Patent number: 4113786Abstract: Process for recovering hydrogen chloride from a gas withdrawn from an oxychlorination reaction zone which contains hydrogen chloride and water vapor wherein the gas is initially cooled, followed by contacting the gas with a small amount of water to absorb the hydrogen chloride from the gas. The water content is controlled to provide an aqueous hydrogen chloride stream having a hydrogen chloride concentration of from 10% to 20%, with the absorbed aqueous hydrogen chloride being recycled to the oxychlorination reaction. A dilute aqueous hydrogen chloride stream, obtained from another portion of the process, may be employed in the initial cooling step, as a direct quench, resulting in vaporization of the dilute aqueous hydrogen chloride stream and eliminating the necessity for a hydrogen chloride concentrator.Type: GrantFiled: April 2, 1976Date of Patent: September 12, 1978Assignee: The Lummus CompanyInventor: Utah Tsao
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Patent number: 4107267Abstract: A process for regenerating waste acid, such as waste hydrochloric acid pickling liquor by producing aqueous hydrochloric acid of pickling concentration and generating iron oxide including that of pigment grade, comprises the steps of (1) concentrating the waste liquor, (2) reacting the concentrated liquor at a temperature below 1000.degree. F.Type: GrantFiled: July 8, 1977Date of Patent: August 15, 1978Assignee: Toledo Pickling & Steel Service, Inc.Inventor: Lars J. Hansen
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Patent number: 4100255Abstract: Chlorinated hydrocarbons are separated from refuse, typically municipal refuse, and combusted in a separate combustion chamber within an incinerating furnace, the special combustion chamber being separated spatially, and the material containing the chlorinated hydrocarbons being separated from refuse, so that combustion gases arising from incineration of the chlorinated hydrocarbons are kept separate from the combustion gases arising from incineration of the refuse.Type: GrantFiled: May 12, 1975Date of Patent: July 11, 1978Assignee: Von Roll AGInventor: Walter Tschantre
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Patent number: 4092403Abstract: A process is disclosed for the purification of a by-product hydrogen chloride stream containing fluoride impurities including carbonyl fluorides comprising contacting said stream with activated alumina maintained at a temperature of at least 55.degree. C. to adsorb said impurities.Type: GrantFiled: August 12, 1976Date of Patent: May 30, 1978Assignee: Union Carbide CorporationInventors: Charles Edward Rectenwald, Henry Bishop Hinckley
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Patent number: 4086321Abstract: A method and apparatus for producing pre metallic oxides by dissolving the metal or oxide in heated dilute hydrochloric acid to form metallic chloride in a water solution (which solution may instead, be a waste product from a steel strip pickling line), reacting said solution in a reactor in the presence of heated oxygen to form metal oxide, part of which oxide being carried over in vapor form to a variable throat venturi where it is redissolved and reintroduced into the reactor to insure that only low chloride oxide will be discharged as a product. The system operates under negative pressure to prevent leakage tendency of HCl to the outside atmosphere.Type: GrantFiled: June 21, 1976Date of Patent: April 25, 1978Assignee: Carl A. HolleyInventors: Carl A. Holley, Russell J. McKinnon
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Patent number: 4083941Abstract: A process for preparing very high purity anhydrous hydrogen fluoride by contacting anhydrous hydrogen fluoride with at least 2.3% by weight of persulfuric acid based on the anhydrous hydrogen fluoride or at least 0.7% by weight of hydrogen peroxide based on the anhydrous hydrogen fluoride at ambient temperature and either at least 0.6% by weight of methanol based on the anhydrous hydrogen fluoride or at least one mole of sulfuric acid per mole of hydrogen peroxide at a temperature of from 0.degree. to 75.degree. C and distilling the resulting mixture to recover very high purity anhydrous hydrogen fluoride.Type: GrantFiled: April 18, 1977Date of Patent: April 11, 1978Assignee: E. I. Du Pont de Nemours and CompanyInventors: Madhusudan Dattatraya Jayawant, Geoffrey Walsh Meadows
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Patent number: 4078047Abstract: In the reaction of phosphate-containing fluorspar with sulphuric acid to produce gaseous hydrofluoric acid, withdrawing the hydrofluoric acid and condensing it, the improvement which comprises adding to the fluorspar a reactive iron compound in an amount approximately equivalent to the phosphate content whereby the phosphate content of the condensed hydrofluoric acid is markedly diminished. The reactive iron compound can be contained in another fluorspar which is blended in the first fluorspar in the requisite amount and/or it can be an iron oxide, fluoride or sulphate, or a hydrated or hydratable iron compound added to the phosphate-containing fluorspar in about 0.2 to 5% by weight calculated as Fe.sub.2 O.sub.3 content and based on the fluorspar.Type: GrantFiled: December 30, 1976Date of Patent: March 7, 1978Assignee: Bayer AktiengesellschaftInventor: Bernhard Spreckelmeyer
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Patent number: 4065551Abstract: Particles of solid carbonaceous waste material which contain fluorine are suspended in a stream of gas consisting of a mixture of steam and air to establish a fluidized bed in a retort. The particles are heated to a temperature of not less than 1000.degree. C to cause pyrohydrolysis and the recovery of fluorine as gaseous hydrogen fluoride at a very efficient rate.Type: GrantFiled: March 1, 1976Date of Patent: December 27, 1977Assignee: Elkem-Spigerverket A/SInventor: Erik Qvale Dahl
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Patent number: 4065513Abstract: By-product hydrogen chloride obtained from cracking of 1,2-dichloroethane is purified of minor concentrations of acetylene by contact with activated carbon at a temperature of at least 375.degree. F. (190.6.degree. C.).Type: GrantFiled: April 15, 1976Date of Patent: December 27, 1977Assignee: PPG Industries, Inc.Inventor: Richard H. Miller
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Patent number: 4059677Abstract: C.sub.2 -C.sub.4 halogenated, e.g., chlorinated and brominated, hydrocarbons, such as vinyl chloride, present in a gas stream are removed therefrom, e.g., incinerated, by contacting the gas stream with an oxygen-containing gas in the presence of metal oxide catalyst system consisting essentially of the oxides of manganese and cobalt at relatively low temperatures, e.g., 100.degree. C. Commonly, the halogenated hydrocarbon is present in the gas stream to be treated in small amounts, e.g., less than 0.05 weight percent. The temperature of treatment can vary, e.g., from 20.degree. C. to 500.degree. C., and can be adjusted within said range depending on the relative humidity of the gas stream treated to maintain catalytic activity. Preferably, treatment occurs under conditions of low relative humidity, e.g., less than 5 percent, and the metal oxides of the catalyst system are hydrated.Type: GrantFiled: December 23, 1976Date of Patent: November 22, 1977Assignee: PPG Industries, Inc.Inventors: Edward J. Sare, Jerome M. Lavanish
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Patent number: 4056605Abstract: A method for purification of hydrofluoric acid from silicofluoric acid and/or sulphuric acid which comprises contacting a mixture of said acids with an anion-exchange resin in the fluoride form. As a result, a purified hydrofluoric acid is obtained. The exhausted anion-exchange resin is treated with a regenerating solution which comprises an aqueous solution of ammonium fluoride with a concentration within the range of from 2 to 10% by weight and having a pH value ranging from 6 to 9.The method according to the present invention is technologically simple; it enables the use of tightly sealed and safe equipment; requires minimal operation costs and eliminates the formation of production wastes.Type: GrantFiled: November 23, 1976Date of Patent: November 1, 1977Inventors: Alexandr Ilich Vulikh, Maina Konstantinovna Zagorskaya, Izrail Zalmanovich Kofman, Inna Vasilievna Pavlovich, Boris Veniaminovich Levitan, Nikolai Vasilievich Troyan, Sergei Viktorovich Dubyaga
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Patent number: 4053558Abstract: Ferric chloride is removed from gas streams containing the same by passing the stream through a bed of activated alumina impregnated with potassium chloride or sodium chloride.Type: GrantFiled: December 6, 1976Date of Patent: October 11, 1977Assignee: Stauffer Chemical CompanyInventor: Ramsey G. Campbell
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Patent number: 4045538Abstract: Vinyl chloride is incinerated at relatively mild temperatures, e.g., 20.degree. to 300.degree.C., by contacting it in a combustion zone with an oxygen-containing gas in the presence of hydrated metal oxide catalyst selected from the group consisting of the oxides of manganese, copper, and mixtures of said oxides. The temperature of incineration is adjusted within the range of 20.degree.-300.degree.C. depending on the relative humidity of the gases in the combustion zone to maintain catalytic activity. Commonly, the vinyl chloride is contained in a gas stream in small amounts, e.g., less than 0.05 weight percent.Type: GrantFiled: September 1, 1976Date of Patent: August 30, 1977Assignee: PPG Industries, Inc.Inventors: Edward J. Sare, Jerome M. Lavanish
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Patent number: 4042639Abstract: Contacting the vapor product of an ethane oxychlorination reaction with relatively cold, liquid, aqueous hydrogen chloride to produce an absorbate containing substantial amounts of inorganic constituents, including hydrogen chloride and water, that were in the vapor product. At least a portion of the absorbate is then distilled at a first pressure, usually above atmospheric pressure, to produce an overhead, usually hydrogen chloride, and aqueous hydrogen chloride bottoms which are usually of substantially azeotropic concentration at the first pressure. These bottoms are then distilled at a second pressure, usually atmospheric pressure, to produce an overhead, usually water, and bottoms of aqueous hydrogen chloride, usually of substantially azeotropic concentration at the second pressure.Type: GrantFiled: November 20, 1974Date of Patent: August 16, 1977Assignee: Owens-Illinois, Inc.Inventors: Theodore H. Gordon, Herman Fred Kummerle
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Patent number: 4038332Abstract: An overall process for the separation of ethyl fluoride from a propane stream containing same is provided wherein said propane stream is extractively distilled using HF, as the extractive solvent producing a first mixture consisting essentially of propane and HF and a second mixture consisting essentially of ethylfluoride and HF, and wherein this second mixture is then mixed with water followed by phase separation.Type: GrantFiled: October 9, 1975Date of Patent: July 26, 1977Assignee: Phillips Petroleum CompanyInventor: C. O. Carter
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Patent number: 4036939Abstract: The method of recovery of hydrogen chloride in gaseous form from an organic solvent loaded with hydrochloric acid in a dilute aqueous solution consists in carrying out prior to distillation a dehydration of the loaded organic solvent in a dehydration extractor in which the solvent is circulated countercurrent to an aqueous solution having a high chloride concentration.Type: GrantFiled: April 24, 1974Date of Patent: July 19, 1977Assignee: Commissariat a l'Energie AtomiqueInventors: Jacques Duhayon, Michel Jean Jacques, Pierre Michel, Maurice Tarnero, Edmond Zellner
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Patent number: 4036776Abstract: A molten mixture containing the higher and lower valent forms of a multivalent metal chloride; in particular, cuprous and cupric chloride, is contacted with oxygen, and aqueous hydrogen chloride recycle, to recover the chlorine values by generation of the higher valent metal chloride and also effect oxidation of the melt by production of the oxychloride. The gas withdrawn from the oxidation contains hydrogen chloride, chlorine and water vapor, with the hydrogen chloride being separate from the gas as aqueous hydrogen chloride and recycle to the oxidation. The chlorine and water vapor in the gas are contacted with activated carbon to produce hydrogen chloride, which is separated as aqueous hydrogen chloride and recycled to the oxidation.Type: GrantFiled: February 10, 1976Date of Patent: July 19, 1977Assignee: The Lummus CompanyInventors: Herbert D. Riegel, Harvey D. Schindler, Vincent A. Strangio
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Patent number: 4036938Abstract: Method and apparatus for the production of high purity hydrogen fluoride by the flame hydrolysis of silicon tetrafluoride and the deliberate cooling of the silicon dioxide and hydrogen fluoride reaction products without appreciable dilution to promote agglomeration of the silicon dioxide and permit separation of the hydrogen fluoride with substantially no contamination.Type: GrantFiled: October 7, 1976Date of Patent: July 19, 1977Inventor: Richard S. Reed
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Patent number: 4035473Abstract: Small amounts of acetylene in anhydrous hydrogen chloride can be reduced by heating the gas to a temperature within the range of about 300.degree. C to 500.degree. C in the presence of oxygen, said oxygen being in molar excess to that of the acetylene present. The process converts up to 99+% of the acetylene to vinyl chloride, carbon monoxide, other oxidation and chlorinated products with minimal production of chlorine which is an undesirable by-product.Type: GrantFiled: July 16, 1976Date of Patent: July 12, 1977Assignee: The Dow Chemical CompanyInventors: German R. Urioste, David E. Busby, Garnet E. McConchie, Jimmy D. Orr
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Patent number: 4032621Abstract: A process for preparing pure anhydrous hydrogen fluoride with decreased levels of arsenic, iron and sulfite by treating anhydrous hydrogen fluoride sequentially with an oxidizing agent, and then a heavy metal free reducing agent, distilling the resulting mixture and recovering the pure hydrogen fluoride.Type: GrantFiled: November 24, 1975Date of Patent: June 28, 1977Assignee: E. I. Du Pont de Nemours and CompanyInventor: Geoffrey Walsh Meadows
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Patent number: 4031192Abstract: To dispose of high-polymer, chlorine-containing plastics, such as PVC, without liberating hydrochloric acid in the atmosphere, the material is placed in a closed vessel and contacted with super-heated steam to split off gaseous hydrochloric acid; the resulting mixture of water vapor, steam and hydrochloric acid is removed, cooled and condensed, so that hydrochloric acid can be derived therefrom; the residue of the material after the hydrochloric acid has been removed can then be safely incinerated with other refuse, etc.Type: GrantFiled: August 27, 1975Date of Patent: June 21, 1977Assignee: Von Roll AGInventor: Robert J. Hafeli
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Patent number: 4021312Abstract: The overhead stream of a deisobutanizer in an HF-alkylation plant is extracted with HF to produce a stream containing isobutane, HF and ethyl fluoride, which in turn is fractionated under a pressure of about 150 to 300 psig. The bottoms stream of this fractionation, then, is fractionated under a pressure of 50 to 145 psig to produce a relatively pure ethyl fluoride overhead stream and a relatively pure HF bottoms stream.Type: GrantFiled: June 24, 1976Date of Patent: May 3, 1977Assignee: Phillips Petroleum CompanyInventor: Cecil O. Carter
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Patent number: 4018880Abstract: The invention concerns a method of purifying hydrogen chloride gas containing small quantities of chlorine. The purifying method comprises passing impure hydrogen chloride over carbon, at a temperature from 30.degree. to 200.degree. C, in the presence of at least one olefin, possibly containing chlorine. The method of the invention applies particularly to the hydrogen chloride obtained from a chloroethane cracking operation initiated by chlorine.Type: GrantFiled: November 25, 1974Date of Patent: April 19, 1977Assignee: Rhone-ProgilInventors: Yves Correia, Jean Lesparre
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Patent number: 4009214Abstract: Hydrogen chloride gas, containing hydrogen fluoride and/or silicon tetrafluoride, is contacted with calcium chloride supported on activated alumina, to separate the hydrogen fluoride and/or silicon tetrafluoride therefrom.Type: GrantFiled: April 25, 1975Date of Patent: February 22, 1977Assignee: The Lummus CompanyInventors: Morgan C. Sze, John E. Paustian
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Patent number: 4003723Abstract: Crude hydrogen chloride gas obtained as a by-product in the production of chloroacetic acids by the catalytic chlorination of acetic acid with chlorine gas in contact with acetic anhydride and/or acetyl chloride, and contaminated with about 0.6 up to 3 % by volume of acetyl chloride is purified. To this end, crude hydrogen chloride gas is introduced into the base portion of a scrubbing zone and scrubbed countercurrently therein with 0.5 up to 20 liter, per normal cubic meter (S.T.P) of hydrogen chloride gas, of a cooled scrubbing liquid under circulation, consisting substantially of 20-80 weight % of concentrated H.sub.2 SO.sub.4, 15-60 weight % of acetic acid, and 5-50 weight % of water. The resulting purified moist hydrogen chloride gas issuing at the head of the scrubbing zone is introduced into the base portion of a drying zone and scrubbed countercurrently with precooled sulfuric acid under circulation.Type: GrantFiled: May 17, 1976Date of Patent: January 18, 1977Assignee: Hoechst AktiengesellschaftInventors: Stefan Schafer, Alexander Ohorodnik, Klaus Gehrmann, Albert Mainski
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Patent number: 4002717Abstract: This invention provides a method for treating manganese oxide ores in an aqueous medium, with hydrogen halide or sulfuric acid, and a hydrogen sulfide or a metal sulfide, e.g. an ore. A leach liquor containing the desirable metal halides is then separated from the solid, insoluble residue. Any iron value in either the manganese oxide ore or in any metal sulfide ore present is not dissolved or is converted to an insoluble iron oxide. Elemental sulfur is also obtained.The metal values in the leach liquor are recovered by crystallization of the manganese halide and liquid ion exchange extraction of the other metal values present.Type: GrantFiled: January 9, 1975Date of Patent: January 11, 1977Assignee: Deepsea Ventures, Inc.Inventors: Richard G. Sandberg, William S. Kane, Paul H. Cardwell
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Patent number: 4000205Abstract: Ferric chloride is removed from gas streams containing the same by passing the stream through a bed of activated alumina impregnated with potassium chloride or sodium chloride.Type: GrantFiled: July 14, 1975Date of Patent: December 28, 1976Assignee: Stauffer Chemical CompanyInventor: Ramsey G. Campbell
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Patent number: 3992507Abstract: This invention provides a halidation process for obtaining a high purity manganese oxide from a manganiferous ore, while reclaiming a substantial portion of the hydrogen halide reagent. The process comprises halidating the ore with a hydrogen halide and leaching to form the corresponding halogen and an aqueous solution comprising dissolved manganese halide and ferric halide. The hydrogen halide can be in the gaseous state and/or dissolved in the aqueous leach solution.The manganese halide and the ferric halide are preferably individually separated from the leach solution by crystallization and by selective extraction, respectively. The crystallized manganese halide is reacted with water at a temperature of from about 400.degree. C to about 700.degree. C to yield the corresponding hydrogen halide, which is recycled, and manganese oxide.In one embodiment, a concentrated leach solution is formed at a temperature of at least about 90.degree.Type: GrantFiled: April 26, 1974Date of Patent: November 16, 1976Assignee: Deepsea Ventures, Inc.Inventors: Paul H. Cardwell, William S. Kane
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Patent number: 3989806Abstract: Substantially all of the chlorine values, e.g., chlorine, are recovered from reactant feeds of chlorinated organic compounds, e.g., hexachlorobenzene and hexachlorobutadiene, by catalytic oxidation at temperatures below about 500.degree. C through the use of transition metal-containing supported catalysts, preferably copper-exchanged zeolite A, X or Y.Type: GrantFiled: February 10, 1975Date of Patent: November 2, 1976Assignee: Vulcan Materials CompanyInventor: David E. Hyatt
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Patent number: 3989807Abstract: Substantially all of the chlorine values, e.g., chlorine, are recovered from reactant feeds of chlorinated organic compounds, e.g., hexachlorobenzene and hexachlorobutadiene, by an improved process involving catalytic oxidation at temperatures below 500.degree. C and more typically below about 450.degree. C using a catalyst of a chromium salt or oxide impregnated on a support.Type: GrantFiled: February 10, 1975Date of Patent: November 2, 1976Assignee: Vulcan Materials CompanyInventor: Earnest L. Johnston
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Patent number: 3980758Abstract: A process for the combustion of chlorine containing residues and wastes with simultaneous recovery of the hydrogen chlorine thereby obtained, which comprises burning the chlorine containing residues with an excess of air and simultaneous addition of azeotropically boiling hydrochloric acid formed in the work-up of the combustion gases.Type: GrantFiled: April 29, 1975Date of Patent: September 14, 1976Assignee: Hoechst AktiengesellschaftInventors: Reinhard Krumbock, Wenzel Kuhn
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Patent number: 3979502Abstract: A method of eliminating chloroacetylenes present in small quantities in hydrogen chloride gas. The method comprises passing hydrogen chloride contaminated with chloroacetylenes over active carbon at a temperature from 50.degree. to 250.degree.C. The method of the invention can plainly be applied to the treatment of hydrogen chloride discharged from works where monochloroacetic acid is prepared, prior to compression of the hydrogen chloride.Type: GrantFiled: November 25, 1974Date of Patent: September 7, 1976Assignee: Rhone-ProgilInventors: Yves Correia, Francois Muller
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Patent number: 3976447Abstract: A gaseous mixture containing up to 20% of hydrogen fluoride and other gases inert to alkaline earth metal fluorides is passed in contact with particulate anhydrous alkaline earth metal fluoride prepared by the fluorination of anhydrous alkaline earth metal chloride in the absence of water. After the anhydrous alkaline earth metal fluoride has taken up the desired amount of hydrogen fluoride, up to its absorption capacity, the hydrogen fluoride is removed therefrom, e.g. by heat regeneration, and the alkaline earth metal fluoride is reused to absorb additional hydrogen fluoride from said gaseous mixtures.Type: GrantFiled: March 11, 1975Date of Patent: August 24, 1976Assignee: Pennwalt CorporationInventors: Dhirendra Ranchhoddas Merchant, Jimmie Ray Hodges
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Patent number: 3972982Abstract: Fluorine compounds are removed from aqueous phosphoric acid by extraction with a mixture of a silane and a long-chain hydrocarbyl amine.BACKGROUND OF THE INVENTIONThis invention relates to a process for removing fluorine from aqueous phosphoric acid.It is known that wet-process phosphoric acid obtained by acidulation of phosphate rock contains substantial amounts of fluorine, predominantly in the form of fluorine compounds such as fluorophosphates and various metal fluorides. Even following purification by known extraction processes, for example, extraction with various organic amines, ethers, etc., such phosphoric acid generally remains contaminated with undesirably high quantities of fluorine compounds with fluorine contents of 1,000 parts per million (ppm) by weight or more not being uncommon.Fluorine contents of this magnitude introduce complications relative to the use of the acid in various applications.Type: GrantFiled: March 3, 1975Date of Patent: August 3, 1976Assignee: Monsanto CompanyInventor: Louis F. Centofanti
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Patent number: 3971845Abstract: Recovery of hydrofluoric acid from aqueous fluosilicic acid by treating said aqueous fluosilicic acid at a temperature of from 100.degree. to 300.degree.C. and under a pressure of from 3 to 80 atmospheres and separating resulting hydrogen fluoride containing aqueous phase and silicon tetrafluoride containing gaseous phase and optionally hydrolyzing the silicon tetrafluoride containing gaseous phase in aqueous medium and recycling the aqueous fluosilicic acid to the process as starting material.Type: GrantFiled: September 26, 1973Date of Patent: July 27, 1976Assignee: Bayer AktiengesellschaftInventors: Wolf Becker, Wolfgang Weiss
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Patent number: 3969490Abstract: A process for the thermal dissociation of an organic substance containing chlorine in which substantially anhydrous hydrogen chloride is obtained. The substance containing chlorine is introduced in a first stage into a salt melt in the absence of oxygen, hydrogen chloride is discharged from the reaction mixture and then oxygen is supplied to the salt melt in a second stage.Type: GrantFiled: December 12, 1973Date of Patent: July 13, 1976Assignee: BASF AktiengesellschaftInventors: Gerard DE Beuckelaer, Gerd Krome, Jan Langens, Ferdinand Lockefeer, Paul Schaerlaekens
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Patent number: 3968200Abstract: Process for recovering hydrogen chloride from an aqueous hydrogen chloride off-gas from an oxychlorination reaction wherein hydrogen chloride is separated from the off-gas as an aqueous solution of hydrogen chloride and employed as feed to an oxychlorination reaction. The process is particularly applicable to the production of vinyl chloride.Type: GrantFiled: March 27, 1972Date of Patent: July 6, 1976Assignee: The Lummus CompanyInventor: Utah Tsao
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Patent number: 3968178Abstract: The invention is a process for the thermal substitution chlorination of methyl chloride at an elevated pressure and separation of the chlorinated hydrocarbons from the anhydrous hydrogen chloride by partial condensation at an elevated pressure to provide a hydrogen chloride gas stream containing only small quantities of chlorinated hydrocarbons.Type: GrantFiled: October 19, 1971Date of Patent: July 6, 1976Assignee: Stauffer Chemical CompanyInventors: Robert P. Obrecht, Marlin J. Bennett
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Patent number: 3959360Abstract: A process for preparing 1-hydroxy, ethylidene-1,1-diphosphonic acid, which comprises contacting a phosphorus trihalide such as phosphorus trichloride with glacial acetic acid in a reaction zone maintained at a temperature of from about 50.degree.C. to about 80.degree.C. while continuously removing by-product acetyl halide as formed from the said reaction zone to form a single-phase liquid reaction product, heating said reaction product to a temperature of from 90.degree.C. to 140.degree.C. and reacting therewith acetic anhydride to form a normally solid anhydrous reaction product, and hydrolyzing said product by steam treatment to recover the desired 1-hydroxy, ethylidene-1,1-diphosphonic acid and remove by-product acetic acid. The acetyl halide by-product is recovered by absorbing same in the aqueous by-product acetic acid recovered from the hydrolysis step and thereby recovering glacial acetic acid for storage and recycle to the process. The process is adapted for continuous operation.Type: GrantFiled: July 31, 1975Date of Patent: May 25, 1976Assignee: Monsanto CompanyInventor: Steve Vazopolos
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Patent number: 3959449Abstract: A method of recovering in highly pure states heavy metals such as cobalt, manganese, etc.Type: GrantFiled: April 1, 1974Date of Patent: May 25, 1976Assignee: Matsuyama Petrochemicals Inc.Inventors: Motoo Shigeyasu, Takeo Ozaki, Nobuo Kusano
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Patent number: 3947558Abstract: Hydrogen fluoride can be separated from an organic mixture of fluorinated C.sub.1 -C.sub.3 compounds and recovered for reuse by selectively absorbing the HF in a glycol in which the HF is soluble, but the fluorinated organic compound is substantially insoluble. If desired, HF can be obtained in anhydrous form.Type: GrantFiled: August 16, 1973Date of Patent: March 30, 1976Assignee: Dow Chemical (Nederland) B.V.Inventor: A. Theodorus van Eijl
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Patent number: 3933989Abstract: Waste synthetic high polymer, especially those containing polyvinyl chloride and the like chlorine-containing synthetic resins are heated at 200.degree.-500.degree.C to thereby form a hot molten bath of fusible materials contained in the waste resin mixture and the chlorine-containing resins are effectively decomposed in the molten bath kept at the temperature of 200.degree.-500.degree.C with the generation of hydrogen chloride gas which can be recovered as hydrochloric acid.Type: GrantFiled: January 11, 1974Date of Patent: January 20, 1976Assignee: Kawasaki Jukogyo Kabushiki KaishaInventors: Hayami Itoh, Mamoru Yamada, Yasuo Nozaki
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Patent number: 3933980Abstract: The invention is a method for reducing the amount of ethylenically unsaturated chlorinated hydrocarbons in gaseous mixtures. The method comprises providing a gas stream containing the ethylenically unsaturated chlorinated hydrocarbon and ozone by admixing ozone with a gas stream containing ethylenically unsaturated chlorinated hydrocarbons or introducing the ethylenically unsaturated chlorinated hydrocarbons into a gas stream containing ozone, and permitting the gas containing the ethylenically unsaturated chlorinated hydrocarbons and ozone to react for a sufficient length of time to reduce the amount of ethylenically unsaturated chlorinated hydrocarbon in the gas stream. The method is particularly useful for removing small amounts of vinyl chloride from gaseous streams thereby substantially reducing or eliminating the emission of such contaminants into the environment.Type: GrantFiled: December 19, 1974Date of Patent: January 20, 1976Assignee: Stauffer Chemical CompanyInventor: Lawrence A. Smalheiser
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Patent number: 3931294Abstract: Production of 2-phenyl-ethylene phosphonic acid by reacting styrene with phosphorus pentachloride in a molar ratio of about 1 : 2 in liquid phase and hydrolyzing the resulting complex 2-phenyl-ethylene phosphonic acid tetrachloride with water.Type: GrantFiled: June 21, 1974Date of Patent: January 6, 1976Assignee: Hoechst AktiengesellschaftInventors: Theodor Auel, Gero Heymer, Hans-Werner Stephan