Reactor-distillation Patents (Class 203/DIG6)
  • Patent number: 4347321
    Abstract: A method and apparatus particularly suitable for the production of alcohol from fermentable substances such as grain. In this method, mash cooking, fermentation, and boiling are carried out sequentially in a single vessel. Boiling produces a first vapor rich in alcohol which is partially condensed to form a liquid condensate and a second vapor which is further enriched in alcohol. The liquid condensate is returned to the vessel and an alcohol product is recovered from the second vapor, preferably without the addition of external heat. Alcohol recovery is effected by passing the second vapor to a second vessel. Vapor from the second vessel is partially condensed to form a third vapor which is still further enriched in alcohol and a liquid condensate which is returned to the second vessel where it is contacted by the second vapor introduced thereto.
    Type: Grant
    Filed: October 7, 1980
    Date of Patent: August 31, 1982
    Assignee: Bio-Systems Research, Inc.
    Inventors: Joseph E. Lionelle, Jeffrey A. Staffa, William L. McCormick
  • Patent number: 4340574
    Abstract: Tri- and dichlorosilanes formed by hydrogenation in the course of the reaction of metallurgical silicon, hydrogen and recycle silicon tetrachloride are employed as feed into a separation column arrangement of sequential separation columns and redistribution reactors which processes the feed into ultrahigh purity silane and recycle silicon tetrachloride. A slip stream is removed from the bottom of two sequential columns and added to the recycle silicon tetrachloride process stream causing impurities in the slip streams to be subjected to reactions in the hydrogenation step whereby waste materials can be formed and readily separated.
    Type: Grant
    Filed: August 28, 1980
    Date of Patent: July 20, 1982
    Assignee: Union Carbide Corporation
    Inventor: Larry M. Coleman
  • Patent number: 4336407
    Abstract: A method for conducting chemical reactions and fractionation of the reaction mixture comprising feeding reactants to a distillation column reactor into a feed zone and concurrently contacting the reactants with a fixed bed catalytic packing to concurrently carry out the reaction and fractionate the reaction mixture.For example, a method for preparing methyl tertiary butyl ether in high purity from a mixed feed stream of isobutene and normal butene comprising feeding the mixed feed stream to a distillation column reactor into a feed zone at the lower end of a distillation reaction zone, and methanol into the upper end of said distillation reaction zone, which is packed with a properly supported cationic ion exchange resin, contacting the C.sub.4 feed and methanol with the catalytic distillation packing to react methanol and isobutene, and concurrently fractionating the ether from the column below the catalytic zone and removing normal butene overhead above the catalytic zone.
    Type: Grant
    Filed: February 17, 1981
    Date of Patent: June 22, 1982
    Assignee: Chemical Research & Licensing Company
    Inventor: Lawrence A. Smith, Jr.
  • Patent number: 4314947
    Abstract: A process for completing the esterification of aliphatic carboxylic acids of 1 to 8 carbon atoms with aliphatic or cycloaliphatic alcohols of 3 to 10 carbon atoms at the boiling point of the alcohol in a column operated with bottom heating, the lower space of the column being free from fitments, the middle space being provided with a packing and the upper space being provided with a packing or other fitments, in which process the water of esterification is driven off at the top of the column by azeotropic distillation, the starting mixture is fed into the side of the column from 5 to 10 m above the liquid level, the ester formed is taken off as liquid from the column bottom, and the column is operated with flooding such that the liquid level is from 6 to 10 m, with the liquid mixture filling the lower column space, which is free from fitments, and the lower part of the packed layer above the said space.
    Type: Grant
    Filed: December 21, 1978
    Date of Patent: February 9, 1982
    Assignee: BASF Aktiengesellschaft
    Inventors: Heinz Hohenschutz, Josef Gnad, Guenter Dinkhauser, Eberhard Schaefer
  • Patent number: 4307254
    Abstract: A method for conducting chemical reactions and fractionation of the reaction mixture comprising feeding reactants to a distillation column reactor into a feed zone and concurrently contacting the reactants with a fixed bed catalytic packing to concurrently carry out the reaction and fractionate the reaction mixture. For example, a method for preparing methyl tertiary butyl ether in high purity from a mixed feed stream of isobutene and normal butene comprising feeding the mixed feed stream to a distillation column reactor into a feed zone at the lower end of a distillation reaction zone, and methanol into the upper end of said distillation reaction zone, which is packed with a properly supported cationic ion exchange resin, contacting the C.sub.4 feed and methanol with the catalytic distillation packing to react methanol and isobutene, and concurrently fractionating the ether from the column below the catalytic zone and removing normal butene overhead above the catalytic zone.
    Type: Grant
    Filed: February 25, 1980
    Date of Patent: December 22, 1981
    Assignee: Chemical Research & Licensing Company
    Inventor: Lawrence A. Smith, Jr.
  • Patent number: 4302356
    Abstract: A catalyst system for use in a reaction-distillation column which is a cloth belt having a plurality of pockets therein containing acid cation exchange resin arranged and supported by wire mesh intimately associated with the cloth pockets, particularly by coiling the cloth belt with the wire mesh disposed between the coils, i.e., in a spiral.
    Type: Grant
    Filed: July 11, 1980
    Date of Patent: November 24, 1981
    Assignee: Chemical Research & Licensing Co.
    Inventor: Lawrence A. Smith, Jr.
  • Patent number: 4254246
    Abstract: A new process for use with continuously operated plants for the production of polyester polymers suitable for producing fibers, bottles and film, by reacting ethylene glycol and terephthalic acid in the presence of a catalyst so that the vapour by-products from the esterification, prepolycondensation and polycondensation stages are continuously rectified in two in-line columns yielding ethylene glycol of high purity (99.85%) which is returned to the process, waste water with 400 ppm ethylene glycol, and a heavy fraction containing oligomers, diethylene glycol, etc.Moreover, an improvement in the quality of the esterified product is attained as it contains less than 0.6% diethylene glycol without the use of diisopropylamine, a poisonous additive.
    Type: Grant
    Filed: March 26, 1979
    Date of Patent: March 3, 1981
    Assignee: Davy International AG
    Inventors: Ovidiu Dicoi, Hans Wewer
  • Patent number: 4250328
    Abstract: An improved method for separating an ester formed in a reaction mixture is disclosed. The method comprises controlling the ratio of organic acid and alcohol utilized and the removal of unreacted alcohol as an alcohol-ester azeotrope.
    Type: Grant
    Filed: February 6, 1979
    Date of Patent: February 10, 1981
    Assignee: Kyowa Yuka Co., Ltd.
    Inventors: Kiyoshi Fujita, Yukiyoshi Ito, Shigeru Kamimori
  • Patent number: 4233267
    Abstract: Volatile reactants are heated under reflux in a reactor and form volatile reaction by-products which are continuously removed in a vapor effluent from a reflux column and partial condenser. The effluent, which entrains some of the reactants, is condensed in a first total condenser and is fed to a distillation apparatus for separation of the volatile reactants and by-products and return of the separated reactants to the reactor. Before the condensate reaches the distillation apparatus, it is temporarily stored in a receiver from which it is controllably fed to a pre-heater where it is evaporated and then fed as a vapor to the distillation column of the distillation apparatus for separation. The distillation column includes at one end a reboiler which retains the reactants. The other end of the distillation column is coupled to a second total condenser in which the volatile by-products are condensed and withdrawn through a cooler for disposal.
    Type: Grant
    Filed: January 18, 1978
    Date of Patent: November 11, 1980
    Assignee: Fiberglas Canada Limited
    Inventors: Robert J. Coker, Gary W. Bate, Henk J. Deuzeman
  • Patent number: 4232177
    Abstract: A method for conducting chemical reactions and fractionation of the reaction mixture comprising feeding reactants to a distillation column reactor into a feed zone and concurrently contracting the reactants with a fixed bed catalytic packing to concurrently carry out the reaction and fractionate the reaction mixture.For example, a method for preparing methyl tertiary butyl ether in high purity from a mixed feed stream of isobutene and normal butene comprising feeding the mixed feed stream to a distillation column reactor into a feed zone at the lower end of a distillation reaction zone, and methanol into the upper end of said distillation reaction zone, which is packed with a properly supported cationic ion exchange resin, contacting the C.sub.4 feed and methanol with the catalytic distillation packing to react methanol and isobutene, and concurrently fractionating the ether from the column below the catalytic zone and removing normal butene overhead above the catalytic zone.
    Type: Grant
    Filed: February 21, 1979
    Date of Patent: November 4, 1980
    Assignee: Chemical Research & Licensing Company
    Inventor: Lawrence A. Smith, Jr.
  • Patent number: 4219680
    Abstract: 2-(perfluoroalkyl)-ethanols of the formula R.sub.f CH.sub.2 CH.sub.2 OH are obtained from 2-(perfluoroalkyl)-ethyl iodides of the formula R.sub.f CH.sub.2 CH.sub.2 I as a mixture with 2-(perfluoroalkyl)-ethylenes of the formula R.sub.f CH.dbd.CH.sub.2 and possibly also with 2-(perfluoroalkyl)-ethylcarboxylic acid esters of the formula R.sub.f CH.sub.2 CH.sub.2 OCOR. From these mixtures, the 2-(perfluoroalkyl)-ethanols are obtained with a high purity degree when adding during the distillation separation as entrainer an alkanol having from 1 to 8 carbon atoms or a monoalkyl ether of ethyleneglycol the alkyl radical of which contains 1 to 4 carbon atoms, or a mixture of such alkanols and/or alkylglycols, and in the presence of 2-(perfluoroalkyl)-ethylcarboxylic acid esters, furthermore an acidic ester interchange catalyst.
    Type: Grant
    Filed: July 25, 1979
    Date of Patent: August 26, 1980
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Inge Konig, Horst Streitberger, Engelbert Krempl, Ulrich Schwenk
  • Patent number: 4215011
    Abstract: A component of a distillation system having both a catalytic function and a distillation function.
    Type: Grant
    Filed: February 21, 1979
    Date of Patent: July 29, 1980
    Assignee: Chemical Research and Licensing Company
    Inventor: Lawrence A. Smith, Jr.
  • Patent number: 4213847
    Abstract: Heavy petroliferous stocks such as vacuum and atmospheric resids, tar sand oils, shale oils, liquids from conversion of coal and the like are concurrently distilled and hydroprocessed for removal of sulfur, nitrogen and metals and are hydrocracked or otherwise hydroprocessed in a packed distillation column under hydrogen pressure wherein the packing is constituted, at least to a substantial extent in both stripping and rectifying sections by catalyst suited to the desired conversions. In a specific application to catalytic hydrodewaxing of lubricating oil stocks, improvement of Viscosity Index (VI) of dewaxed product results.
    Type: Grant
    Filed: May 16, 1979
    Date of Patent: July 22, 1980
    Assignee: Mobil Oil Corporation
    Inventors: Nai Y. Chen, Ikai Wang
  • Patent number: 4194964
    Abstract: Heavy petroliferous stocks such as vacuum and atmospheric resids, tar sand oils, shale oils, liquids from conversion of coal and the like are concurrently distilled and hydroprocessed for removal of sulfur, nitrogen and metals and are hydrocracked or otherwise hydroprocessed in a packed distillation column under hydrogen pressure wherein the packing is constituted, at least to a substantial extent in both stripping and rectifying sections by catalyst suited to the desired conversions.
    Type: Grant
    Filed: July 10, 1978
    Date of Patent: March 25, 1980
    Assignee: Mobil Oil Corporation
    Inventors: Nai Y. Chen, Ikai Wang
  • Patent number: 4115460
    Abstract: Method for producing hexachlorocyclobutene from hexachlorobutadiene, wherein technical hexachlorobutadiene is rectified at a pressure of 2-10 mm Hg with a reflux ratio of 300-600, and the hexachlorobutadiene remaining in the sump during this procedure, after a heat treatment at 150.degree.-200.degree. C., is recycled into the rectifying column together with fresh, technical hexachlorobutadiene. The product rich in hexachlorocyclobutene, withdrawn overhead, is optionally subjected to a fractional crystallization.
    Type: Grant
    Filed: February 28, 1977
    Date of Patent: September 19, 1978
    Assignee: Chemische Werke Huls AG
    Inventor: Wolfgang Muller
  • Patent number: 4108866
    Abstract: An improved method of producing dialkyl-sulfoxides by oxidizing corresponding dialkyl-sulfides with hydrogen peroxide in aqueous acidic medium. It remedies the drawback of the similar prior art as concerns the separation of the sulfoxide formed from its reaction medium. The new method permits of easily recovering the sulfoxides in the state of good purity.The improvement consists in mixing the reaction medium with a large proportion of a solvent capable of yielding an azeotropic mixture with water. Then, after oxidization, the water is removed by distillation as azeotropic mixture. Preferably solvents are used which dissolve the dialkyl-sulfide but do not dissolve the sulfoxide formed; heptane is a particularly useful solvent. When an excess of the solvent is used, there is obtained, after distilling off the azeotropic mixture, a slurry of sulfoxide and solvent, easy to separate.
    Type: Grant
    Filed: June 8, 1977
    Date of Patent: August 22, 1978
    Assignee: Societe Nationale des Petroles d'Aquitaine
    Inventors: Bernard Tramier, Raymond Delourme, Philippe Fresnel
  • Patent number: 4089752
    Abstract: A distillation column reactor which provides a relatively long residence time with a minimum drop in pressure which comprises a distillation column containing standard trays with downcomers, a liquid reservoir between the trays, and vapor ports provided through said reservoir, whereby liquid from said downcomers enters said reservoir thereby providing increased liquid residence time in said column.
    Type: Grant
    Filed: August 30, 1976
    Date of Patent: May 16, 1978
    Assignee: Sun Ventures, Inc.
    Inventor: Allen W. Hancock, II
  • Patent number: 4088676
    Abstract: A process for the continuous preparation of organic solutions of percarboxylic acids by reaction of an aqueous solution of hydrogen peroxide with the corresponding carboxylic acid in the presence of an acid, water-soluble catalyst which boils above 160.degree. C., extraction of the percarboxylic acid from the resulting reaction mixture using an organic solvent which is immiscible with water, reconcentration of the raffinate, which essentially contains hydrogen peroxide and the acid catalyst, by distilling off water in a distillation column and recycle of the raffinate, concentrated in this way, into the reaction with the carboxylic acid. The raffinate is divided into two partial streams in a ratio of 1 to 25:1.
    Type: Grant
    Filed: April 28, 1976
    Date of Patent: May 9, 1978
    Assignees: Bayer Aktiengesellschaft, Deutsche Gold- und Silber-Scheideanstalt vormals Roessler
    Inventors: Willi Hofen, Gunter Prescher, Gerd Siekmann, Gunter Wolf
  • Patent number: 4087455
    Abstract: Process for the continuous preparation of organic solutions of percarboxylic acids by reaction of aqueous hydrogen peroxide with the corresponding carboxylic acid in the presence of an acid, water-soluble catalyst, extraction of the resulting reaction mixture with an organic solvent and recycle of the raffinate, containing hydrogen peroxide, after reconcentration by the removal of water by distillation into the reaction. The raffinate is fed, together with the whole of that amount of hydrogen peroxide which essentially to the consumption of hydrogen peroxide in the reaction or with a part thereof, into the distillation for the removal of water. The amount of water which essentially corresponds to the sum of the water of reaction formed during the reaction and the water introduced into the process with the feed products is distilled off under reduced pressure. The sump product, thus obtainable, from the distillation is recycled into the reaction.
    Type: Grant
    Filed: April 28, 1976
    Date of Patent: May 2, 1978
    Assignees: Bayer Aktiengesellschaft, Deutsche Gold-und Silber-Scheideanstalt Vormal Roessler
    Inventors: Gunter Prescher, Gerd Schreyer, Helmut Waldmann, Wulf Schwerdtel
  • Patent number: 3963446
    Abstract: Apparatus for conducting a continuous, pressurized liquid-state reaction while maintaining internal recycle. The apparatus has a perforated barrier plate which separates a reaction zone from a reboiler zone and has a by-pass conduit which connects these two zones. Control devices maintain the liquid levels in the reaction and reboiler zones. A heater in the reboiler zone evolves vapors in that zone, which vapors return to the reaction zone through the perforated barrier plate.
    Type: Grant
    Filed: January 14, 1975
    Date of Patent: June 15, 1976
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Donald Nelson Miller
  • Patent number: 3937616
    Abstract: Phosphorous acid is produced from PCl.sub.3 and water in an apparatus, the essential parts of which include a reactor and an evaporator, which are connected together by means of a conduit running from the bottom of the reactor to the head of the evaporator. The evaporator communicates with the lower end of a separator of which the upstream end terminates in an off-gas outlet. More particularly, the downstream end of the evaporator is connected to a stripping column which is provided with an off-gas outlet opening into the off-gas outlet associated with the evaporator.
    Type: Grant
    Filed: October 29, 1974
    Date of Patent: February 10, 1976
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Joseph Cremer, Willi Martin