Reactor-distillation Patents (Class 203/DIG6)
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Patent number: 4847430Abstract: The invention concerns a process for manufacturing methyl tert-butyl ether (MTBE) by reacting methanol with an isobutene-containing hydrocarbon mixture.This process is characterized by the steps of:introducing the reactants into a reaction-distillation zone containing at least two superposed and non-contiguous fixed beds (2a, 2b) of catalyst of the sulfonated resin type, wherein passage-ways are provided for a vapor phase, at least one distillation tray (4a), at least one liquid redistribution tray (5),maintaining distillation conditions in said zone so as to have a descending liquid phase and an ascending vapor phase,maintaining a continuous liquid phase in the lower part of said beds,discharging a vapor phase containing a high proportion of unconverted hydrocarbons from the top (8) of said zone, andwithdrawing a liquid phase of high MTBE content from the bottom (10) of said zone.Type: GrantFiled: March 21, 1988Date of Patent: July 11, 1989Assignees: Institut Francais Du Petrole, Elf FranceInventors: Dang Vu Quang, Pierre Amigues, Jean-Ferdinand Gaillard, Jacques Leonard, Jean-Luc Nocca
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Patent number: 4836989Abstract: A distributor system for use in multiple bed, downflow reactors which provides improved distribution across the reactor and improved vapor/liquid contact and distribution. The system comprises a collection tray arranged below the first catalyst bed in the reactor, a first, rough distributor tray which is arranged below the collection tray and which is fed from the collection tray by means of spillways in the tray and a mixing chamber beneath the spillways. The first distributor tray provides for separate vapor and liquid flow by means of apertures in the tray or downward flow of liquid and vapor chimneys for downward flow of vapor. After the first distributor tray, a second, final distributor tray is provided with downcomers for flow of liquid and vapor onto the lower catalyst bed. Each downcomer comprises an open-topped tube with a side aperture for entry of liquid into the tube, vapor entering through the open top of the tube.Type: GrantFiled: July 2, 1987Date of Patent: June 6, 1989Assignee: Mobil Oil CorporationInventors: Fouad A. Aly, Richard G. Graven, David W. Lewis
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Patent number: 4832920Abstract: A continuous catalytic system for converting an olefinic feedstock comprising ethylene and C.sub.3.sup.+ olefins to heavier liquid hydrocarbon product comprising apparatus for(a) prefractionating the olefinic feedstock to obtain a gaseous stream rich in ethylene and a liquid stream containing C.sub.3.sup.+ olefins;(b) vaporizing and contacting the liquid stream from the prefractionating step with hydrocarbon conversion oligomerization catalyst in a catalytic reactor system to provide a heavier hydrocarbon effluent stream comprising distillate, gasoline and lighter hydrocarbons;(c) fractionating the effluent stream to recover distillate, gasoline and lighter hydrocarbons separately;(d) recycling at least a portion of the recovered gasoline as a liquid sorption stream to prefractionating step (a); and(e) further reacting the recycled gasoline together with sorbed C.sub.3.sup.+ olefins in the catalytic reactor system of step (b).Type: GrantFiled: June 13, 1984Date of Patent: May 23, 1989Assignee: Mobil Oil CorporationInventors: Hartley Owen, Chung H. Hsia, Bernard S. Wright
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Patent number: 4832796Abstract: A process for improving the quality of phenol which comprises(a) introducing a liquid phenol composition comprising above about 95 weight percent phenol on a dry basis, organic acid contaminants, and organic ketone contaminants;(b) introducing water into the distillation tower, together with the phenol stream or in a separate stream;(c) heating the phenol composition and water to a temperature sufficiently high to vaporize the water;(d) allowing the organic acid contaminant to build to a concentration whereby sufficient acid is present to catalyze a reaction between an organic ketone contaminant and phenol, thereby forming a new compound(s) and;(e) removing the said formed compound(s) from the distillation tower by hydroextractive steam distillation.Type: GrantFiled: July 16, 1987Date of Patent: May 23, 1989Assignee: General Electric CompanyInventor: John W. Fulmer
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Patent number: 4830712Abstract: A process is described for recovering polyester-grade ethylene glycol from crude ethylene glycol containing at least one component which has a normal boiling point below that of ethylene glycol, and which can form a UV absorber in the presence of ethylene glycol which comprises supplying to an ethylene glycol distillation system, preferably comprising a fractional distillation zone having an upper portion, a lower portion and an intermediate portion a crude ethylene glycol stream at a determined pH of less than about 7.Type: GrantFiled: September 29, 1987Date of Patent: May 16, 1989Assignee: Union Carbide CorporationInventors: John W. Crandall, Bernard C. Ream
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Patent number: 4826662Abstract: Apparatus for reducing the amount of water in the feed to a methanol-to-gasoline (MTG) conversion reactor is described. The output products of a dehydration reactor and an aqueous methanol feed are supplied to a primary distillation tower or separator. A dimethylether (DME)/methanol mixture is taken as overhead from the primary tower and can be sent to the MTG conversion reactor to produce hydrocarbons boiling in the gasoline range. Bottoms from the primary tower, containing methanol and water, are supplied to a secondary distillation tower or separator. A methanol stream is drawn as overhead from the secondary tower and is passed to an acid catalyzed dehydration reactor where an equilibrium mixture of dimethylether, methanol, and water is produced. The equilibrium mixture is passed from the dehydration reactor to the primary distillation tower. In preferred embodiments, the conversion reactor feed from the primary distillation tower may be of a gaseous or liquid phase.Type: GrantFiled: May 6, 1987Date of Patent: May 2, 1989Assignee: Mobil Oil CorporationInventors: Cheng-How Mao, Max Schreiner, Jr.
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Patent number: 4791227Abstract: What is disclosed is the use of metallic vessels having particularly high corrosion resistance which are made of(a) aluminum or alloys containing more than 95% aluminum, or of(b) nickel-chromium-iron alloys containing from 30 to 50% of nickel, from 20 to 30% of chromium, and from 18 to 50% of iron, by weight, in reacting or working up mixtures containing substantial amounts of hydrogen fluoride in addition to organic carboxylic acids and/or carbon monoxide and/or water.Type: GrantFiled: September 23, 1982Date of Patent: December 13, 1988Assignee: Rohm GmbHInventors: Alfred Neumann, Willi Ploesser, Hermann-Josef Siegert
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Patent number: 4778568Abstract: Isomer mixtures of 1,3- and 1,4-bis-(2-hydroxyhexafluoroprop-2-yl)-benzene are separated by a steam distillation in the presence of CS.sub.2. On cooling of the steam distillate, a solid precipitates which is composed mainly of the 1,4-isomer. After the solid has been separated off, an aqueous-organic liquid-phase mixture remains, the organic phase of which mainly contains the 1,3-isomer. The pure isomers are obtained by recrystallization or distillation respectively. These are mainly intermediates in the polymer field.Type: GrantFiled: July 21, 1987Date of Patent: October 18, 1988Assignee: Hoechst AktiengesellschaftInventors: Klaus-Albert Schneider, Gunter Siegemund
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Patent number: 4759826Abstract: An improved process for purifying thionyl chloride by the double distillation of an impure mixture of thionyl chloride, sulfuryl chloride, sulfur monochloride, sulfur dichloride and sulfur dioxide is disclosed. The double distillation process is conducted in the presence of sulfur to convert sulfur dichloride into sulfur monochloride. The sulfuryl chloride content of the mixture is reduced by contacting the vapor from the reboiler in the first stage distillation with activated carbon prior to fractional distillation in the column. The product of the first stage distillation is then redistilled to produce a thionyl chloride product of high purity.Type: GrantFiled: October 23, 1986Date of Patent: July 26, 1988Assignee: Occidental Chemical CorporationInventor: Gary M. Sellers
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Patent number: 4730082Abstract: A process for the preparation of methyltrifluoroacetate. Trifluoroacetic acid is contacted with an excess of methanol and distilled to form a methyltrifluoroacetate/methanol azeotrope. The azeotrope is contacted with trifluoroacetic acid in the presence of a catalytic quantity of a strong acid followed by distillation to obtain methyltrifluoroacetate. The methyltrifluoroacetate can be used as a synthesis intermediate in the pharmaceutical industry.Type: GrantFiled: June 12, 1986Date of Patent: March 8, 1988Assignee: Rhone-Poulenc Specialties ChimiquesInventor: Louis Amiet
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Patent number: 4725338Abstract: A process for purifying a solvent suitable for use in the polymerization of an olefin in the presence of a Ziegler-Natta catalyst, which comprises feeding the polymerization solvent to a stage lower than a chimney tray of a multi-stage distillation column, said chimney tray being provided at a height between the top and bottom of the column, feeding an organoaluminum compound to a stage higher than the chimney tray, drawing out a condensate from the chimney tray, heating the condensate to produce heated vapor, introducing the heated vapor to the chimney tray or to a stage higher than the chimney tray but lower than the stage to which the organoaluminum compound has been fed, and drawing the solvent in a purified state from the top.Type: GrantFiled: February 24, 1986Date of Patent: February 16, 1988Assignee: Mitsui Toatsu Chemicals, IncorporatedInventors: Tadashi Asanuma, Tatuo Ohoka, Minoru Hino, Nobutaka Uchikawa
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Patent number: 4722769Abstract: This invention is a process for purifying crude acetone obtained by cleavage of cumene hydroperoxide, said crude acetone containing aldehyde impurities and appreciable amounts of unreacted cumene, by fractionally distilling the acetone in a multiple plate distillation column, said process comprising: continuously feeding crude acetone; continuously feeding a dilute aqueous solution of an alkaline material at a point above the crude acetone feed point; and controlling the temperature profile of the column by adjusting the amount of liquid acetone removed in step (c) to maintain a preselected temperature on a plate in the region between the crude acetone feed point and the alkaline material feed point.Type: GrantFiled: April 24, 1986Date of Patent: February 2, 1988Assignee: Allied CorporationInventors: Chong H. Chan, Lamberto Crescentini, Everett H. Hinton, Jr.
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Patent number: 4717454Abstract: A process for removing by product acetone from reaction mixtures obtained by reacting methyl acetate and/or dimethylether with carbon monoxide at elevated temperatures to obtain acetic anhydride in the presence of a catalyst system consisting essentially of carbonyl complexes of noble metals belonging to group VIII of the Periodic System of the elements, acetic acid, an organophosphorus or organonitrogen compound, and methyl iodide whereby the acetone obtained as a by-product during the reaction is subjected to condensation at temperatures of 50.degree. to 250.degree. C., under pressures of 0.01 to 150 bars and at a molar ratio as above defined for the catalyst system constituent of 1:(25-500):(10-100):(15-150) so as to obtain predominantly higher-boiling secondary products to be distillatively separated in a successive distillation zone together with volatile constituents of the catalyst system.Type: GrantFiled: September 10, 1985Date of Patent: January 5, 1988Assignee: Hoechst AktiengesellschaftInventors: Heinz Erpenbach, Klaus Gehrmann, Peter Horstermann, Georg Kohl
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Patent number: 4716244Abstract: If the transesterification of esters of formula II ##STR1## with alcohols of formula III A--OH).sub.m is catalysed by treatment with catalytic amounts of an organic or inorganic zinc salt and the resultant melt is subsequently distilled in a short-time distillation apparatus under specific conditions, then compounds of the formula ##STR2## are obtained in virtually quantitative yield, in which formulae I, II and III n is a number from 0 to 2, m is 1 or 2, A is a radical derived from an m-valent aliphatic alcohol, which radical contains 2 to 18 carbon atoms, B is methyl or tert-butyl and R is methyl or ethyl. The products thus obtained contain no troublesome by-products and do not have to be additionally purified.Type: GrantFiled: April 21, 1986Date of Patent: December 29, 1987Assignee: Ciba-Geigy CorporationInventor: Ivan Orban
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Patent number: 4698440Abstract: A batch process for preparing n-butyl methacrylate directly from n-butanol and methacrylic acid by employing azeotropic distillation and azeotropic phase separation.Type: GrantFiled: August 5, 1985Date of Patent: October 6, 1987Assignee: E. I. Du Pont de Nemours and CompanyInventors: Leslie M. Blair, Roddy M. Conrad
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Patent number: 4683033Abstract: Hydrocarbon solutions containing iodine or iodine-containing impurities are rendered essentially color-free by distillation in the presence of small amounts of a hydrocarbon soluble organometallic compound.Type: GrantFiled: January 24, 1986Date of Patent: July 28, 1987Assignee: Phillips Petroleum CompanyInventor: Raymond L. Cobb
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Patent number: 4645576Abstract: This invention provides a process for isolating and recovering butene-1 of high purity at high yield. Firstly, a butane-butene fraction containing 0.1 to 7 wt % of isobutylene, 10 to 50 wt % of butene-1 and 5 to 20 wt % of isobutane is rectified to reduce the content of isobutane to not more than 0.1 wt %. Then, the rectified butane-butene fraction is passed through a reactor packed with an extrusion molded silica-alumina catalyst to polymerize isobutylene at a reaction velocity as high as 50 times or more of that of butene-1, thus forming oligomers of isobutylene. Finally, the hydrocarbon mixture from the reactor is rectified to remove the oligomers of isobutylene and the other C.sub.4 -hydrocarbons.Type: GrantFiled: May 10, 1984Date of Patent: February 24, 1987Assignee: Nippon Oil Co., Ltd.Inventors: Tetsuya Takezono, Takaaki Amari, Hirosuke Imai
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Patent number: 4624748Abstract: A novel catalyst system for use in a distillation column reactor is disclosed including annularly-defined spaces within the reactor comprised of vapor-permeable material with packed catalyst and alternately positioned vapor barrier means.Type: GrantFiled: June 29, 1984Date of Patent: November 25, 1986Assignee: Chevron Research CompanyInventor: Willard M. Haunschild
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Patent number: 4620024Abstract: In a continuous alkoxidation-phosphorylation process for producing tributyl phosphate having low color utilizing excess butanol in the alkoxidation reaction which is heated by an alcohol flasher wherein the excess butanol is recovered after phosphorylation by two stage flash distillation, the bottoms product from the first stage going to the second stage, the overhead product from the second stage returning to the first stage flash distillation, and the bottoms from the second stage distillation going to final product washing and drying process while the overhead from the first stage flash distillation is fed to the process alkoxidation alcohol flasher, the improvement which comprises distilling in a distillation column the overhead product from the first stage flash distillation and then feeding the overhead from the distillation column to the alkoxidation alcohol flasher.Type: GrantFiled: October 22, 1984Date of Patent: October 28, 1986Assignee: FMC CorporationInventors: Robert I. Davis, Thomas G. Seador
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Patent number: 4597947Abstract: An apparatus comprised of a mass transfer microchannel plate (MCP) struct distillation column in a columnar configuration within an air tight cylindrical housing. The apparatus may be used in separation of organic chemicals like petrochemicals, vegetable oils, inorganic chemicals like steam stripping of bromine from aqueous potassium chloride/potassium bromide solutions, corrosive as well as separation of hazardous gases.The MCP structures may have an electric field or electromagnetic field across the MCP to create synergestic mass transfer separation potential either to increase or decrease separations. Blood filtering as well as other biomedical separations are possible by this synergestic mass transfer.Catalytic depositions within the channels of the MCPs, either as wall coatings with the channels open or as solid porous catalytic material that has osmosis action thereacross further enhances chemical reactions during the separation process or during passage through the channels.Type: GrantFiled: February 21, 1985Date of Patent: July 1, 1986Assignee: The United States of America as represented by the Secretary of the ArmyInventor: Bipin C. Almaula
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Patent number: 4578501Abstract: A process for the production of a crude dimethyl terephthalate suitable for hydrolyzing into a fiber grade terephthalic acid involves separating a crude ester obtained from the production of dimethyl terephthalate by the Witten process by vacuum distillation at elevated pressure in a three-column series arranged distillation system. In the first distillation column of the system the crude is separated into a methyl p-toluate-rich fraction as head product; in a second column of the series, into a fraction rich in methyl ester of terephthalaldehydic acid as head product; and in a third distillation column, a crude dimethyl terephthalate fraction. The crude dimethyl terephthalate fraction has a methyl ester of terephthalaldehydic acid content of 0.01-0.1% by weight as a head product.Type: GrantFiled: April 18, 1980Date of Patent: March 25, 1986Assignee: Dynamit Nobel AktiengesellschaftInventors: Anton Schoengen, Georg Schreiber, Heinz Schroeder
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Patent number: 4569725Abstract: A C.sub.4 -hydrocarbon mixture which essentially contains n-butenes and butanes is separated by a process in whichthe mixture is reacted with a carboxylic acid in the presence of an acidic catalyst to form a butyl carboxylate,the reaction mixture obtained from the esterification zone is distilled to give, as the top product, a fraction containing the butanes, and, as the bottom product, a fraction containing the resulting butyl carboxylate,the butyl carboxylate is decomposed at elevated temperatures to give the carboxylic acid and n-butenes, andthe mixture of n-butenes and carboxylic acid is then distilled, the n-butenes being obtained as the top product, and the carboxylic acid as the bottom product.Type: GrantFiled: May 23, 1984Date of Patent: February 11, 1986Assignee: BASF AktiengesellschaftInventors: Alfred Lindner, Klaus Broellos, Gerhard Sandrock, Klaus Volkamer, Werner Hefner
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Patent number: 4544776Abstract: The reaction product from etherification of C.sub.4 -C.sub.7 isoolefins with methanol in the presence of an acidic catalyst is washed with water in the presence of inert hydrocarbons thereby removing methanol and a part of the tertiary alcohol. The aqueous extract solution bottoms is distilled to separate methanol as overhead. Tertiary alcohols are withdrawn as a side stream from a tray of the distillation column with a high concentration thereof and fed into the washing column.Type: GrantFiled: December 20, 1982Date of Patent: October 1, 1985Assignee: Deutsche Texaco AktiengesellschaftInventors: Gunther Osterburg, Milan Prezelj
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Patent number: 4519875Abstract: Ethylene glycol is purified, particularly for fiber-grade applications, by removal of the residual ethylene carbonate from which the glycol was derived. The effluent from a reactor in which ethylene carbonate is hydrolyzed to ethylene glycol is distilled to produce a lower-boiling fraction comprising substantially ethylene glycol and water and a higher-boiling fraction comprising substantially ethylene glycol, higher glycols, and concentrated in hydrolysis catalyst. The higher-boiling fraction is recirculated to reflux against the lower-boiling product, thereby essentially completing the hydrolysis of unreacted ethylene carbonate thereby reducing the ethylene carbonate content of the ethylene glycol to very low levels suitable for fiber-grade applications.Type: GrantFiled: May 9, 1984Date of Patent: May 28, 1985Assignee: The Halcon SD Group, Inc.Inventors: Mitchell Becker, Howard M. Sachs
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Patent number: 4504687Abstract: A method for producing tertiary ethers from C.sub.4 or C.sub.5 streams containing isobutene and isoamylene respectively in a process wherein a acidic cation exchange resin is used as the catalyst and as a distillation structure in a distillation reactor column, wherein the improvement is the operation of the catalytic distillation in two zones at different pressures, the first zone containing the catalyst packing and operated a higher pressure in the range of 100 to 200 psig in the case of C.sub.4 's and 15 to 100 psig in the case of C.sub.5 's which favors the etherification reaction and the second zone being a distillation operated at a lower pressure in the range of 0 to 100 psig in the case of C.sub.4 's and 0 to 15 psig in the case of C.sub.Type: GrantFiled: September 7, 1983Date of Patent: March 12, 1985Assignee: Chemical Research & Licensing CompanyInventor: Edward M. Jones, Jr.
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Patent number: 4504363Abstract: 2,6-Dimethylmorpholine containing a high proportion of the cis compound is prepared by cyclization of diisopropanolamine (1,1'-iminobispropan-2-ol) in the presence of sulfuric acid, with simultaneous addition of the components and full utilization of the heat of reaction.Type: GrantFiled: May 5, 1983Date of Patent: March 12, 1985Assignee: BASF AktiengesellschaftInventors: Norbert Goetz, Bjoern Girgensohn, Fritz Zanker
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Patent number: 4482733Abstract: An improved process for preparing diaryl esters of dicarboxylic acids is disclosed, in which the esterification reaction is optimized by gradually increasing the temperature at which the reaction is being conducted according to a predetermined pattern. The temperature increase should be a function of the degree of esterification. The diaryl esters so prepared are useful in making linear polyesters.Type: GrantFiled: September 24, 1982Date of Patent: November 13, 1984Assignee: Occidental Chemical CorporationInventor: Gautam R. Ranade
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Patent number: 4482732Abstract: An improved process for preparing diaryl esters of dicarboxylic acids is disclosed, in which the esterification reaction is optimized by removing water and other by-products of the reaction according to a predetermined pattern. The removal of water and other by-products of the esterification reaction is most easily carried out by a distillation means, and the rate of removal is controlled by varying the reflux ratio in the distillation means during the course of the esterification reaction. The diaryl esters so prepared are useful in making linear polyesters.Type: GrantFiled: September 24, 1982Date of Patent: November 13, 1984Assignee: Occidental Chemical CorporationInventor: Gautam R. Ranade
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Patent number: 4482775Abstract: A method for isomerizing isobutene or n-butene to produce a mixture of isobutene and normal butene, and polymerizing at least a portion thereof to produce isobutene/n-butene codimer, which comprieses feeding at least 80 weight % of either the isobutene or n-butene to a catalytic distillation reactor containing a fixed bed acidic cation exchange resin catalyst packing which provides both the catalyst sites and distillation sites for the reaction products, isomerizing a portion of the isobutene or n-butene to produce a mixture of isobutene and n-butene and reacting at least a portion of the isobutene and n-butene to form codimer of isobutene and n-butene, whereby an overhead fraction containing any unreacted isobutene and n-butene and a bottoms fraction containing codimer is produced. The result of the reaction is substantially the same regardless whether the feed is isobutene or n-butene. Other aspects of the invention, include combinations of procedures to produce high purity isobutene and n-butene.Type: GrantFiled: September 22, 1982Date of Patent: November 13, 1984Assignee: Chemical Research & Licensing CompanyInventor: Lawrence A. Smith, Jr.
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Patent number: 4481146Abstract: The invention relates to a process for the preparation of an ethyl ester from ethanol-containing mixtures of aliphatic alcohols, which comprises esterifying the alcohols with a carboxylic acid in the presence of an acid catalyst in a distilling column and separating in the same column the ethyl ester continuously from the ester mixture obtained. To this purpose, the alcohol mixture is introduced into the sump and the carboxylic acid is introduced into the column at a point located in the central part and the ethyl ester as well as the water formed during esterification are withdrawn continuously at the top of the column and the higher esters are withdrawn continuously at the sump.Type: GrantFiled: September 29, 1981Date of Patent: November 6, 1984Assignee: Hoechst AktiengesellschaftInventors: Ernst I. Leupold, Hans-Joachim Schmidt, Knut Popp
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Patent number: 4479012Abstract: Aldehydes are obtained from the gaseous product of the hydroformylation of olefinically unsaturated compounds using a rhodium catalyst by a process (cf. FIG. 2) in which(a) this gaseous product is introduced, without being cooled or depressured, into a distillation column D,(b) the top fraction from this column is cooled in a condenser K so that the greater part of the aldehydes contained therein is condensed,(c) the condensate is separated, in a separator A, into a gas phase and a liquid phase,(d) the gas phase from A, after waste gas has been separated off, is again brought to the hydroformylation pressure by means of a compressor P, and is returned to the reactor as a recycle gas,(e) the liquid phase from A is returned to D, and(f) the aldehydes are taken off from column D as liquid bottom products and/or as a vaporous side stream.Type: GrantFiled: March 30, 1982Date of Patent: October 23, 1984Assignee: BASF AktiengesellschaftInventors: Karl Fischer, Armin V. Grenacher, Manfred Herr, Max Strohmeyer
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Patent number: 4475005Abstract: A process for preparing tertiary alkyl ethers from isoolefins and aliphatic alcohols in the presence of a catalyst in the form of sulphonated styrene-divinylbenzene resins, characterized in that both the reaction leading to the formation of the tert-alkyl ether and the separation of the tert-alkyl ether from the hydrocarbons and compounds which accompany it take place in a single plate fractionating apparatus, in which some of the plates are provided with beds of catalyst in the form of spherules suitable for preparing said tert-alkyl ether, the ether obtained being withdrawn as a substantially pure bottom product.Type: GrantFiled: March 24, 1982Date of Patent: October 2, 1984Assignee: Snamprogetti S.p.A.Inventor: Giancarlo Paret
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Patent number: 4471154Abstract: A distillation-reactor for separating constituents of a feedstock having similar boiling points includes at least one stage with containing screens defining a series of containment volumes for a heterogeneous particulate catalyst. The catalyst is fluidized within the volumes defined by the containing screens by the action of vapor passing through the tray. Liquid flowing across the tray intimately contacts the fluidized catalyst and vapor without the occurrence of liquid back-up or high pressure drop.Type: GrantFiled: June 10, 1983Date of Patent: September 11, 1984Assignee: Chevron Research CompanyInventor: Frederick C. Franklin
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Patent number: 4465853Abstract: 3,4-Diacetoxybutene-1 can be easily isomerized into 1,4-diacetoxybutene-2 by contacting it with a cation exchange resin. This method is capable of providing an excellent reaction result and is free of the problem of corrosion of apparatus as well as the problem of formation of by-products. When acetic acid is present in said isomerization operation, the reaction rate is increased. Further, combination of this isomerization method with separation of 1,4-diacetoxybutene-2 from 3,4-diacetoxybutene-1 by distillation enables production of high-purity 1,4-diacetoxybutene-2 at a high efficiency.Type: GrantFiled: November 26, 1982Date of Patent: August 14, 1984Assignee: Japan Synthetic Rubber Co., Ltd.Inventors: Yoshinori Yoshida, Hironobu Shinohara
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Patent number: 4454356Abstract: Methanol is reacted with branched monoolefins such as isobutylene, or mixtures of hydrocarbons such as mixed C-4's from or in a refinery, in the presence of methanesulfonic acid. A column (10) operation is described wherein methanesulfonic acid (11) and methanol (12) are fed in countercurrent fashion to hydrocarbons (13). Crude product ether is removed as a liquid sidestream (25) above the feed of methanesulfonic acid (11), while hydrocarbons depleted of the reactive branched monoolefins (24) are removed overhead. The methanesulfonic acid suppresses the vapor pressure of methanol relative to product ether.Type: GrantFiled: October 14, 1982Date of Patent: June 12, 1984Assignee: Allied CorporationInventors: Divakaran Masilamani, Andiappan K. S. Murthy
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Patent number: 4454358Abstract: Ethanol is produced continuously via the carbonylation of methanol, by(a) carbonylating methanol, in a reactor R, in the presence of a carbonyl complex of a metal of group VIII of the periodic table and of a halogen compound,(b) separating, in a distillation column D1, the reactor discharge, into a top fraction comprising methyl acetate, methanol, dimethyl ether and an organohalogen compound, and into a bottom fraction comprising water, small quantities of acetic acid and the catalyst, if the latter is not in a fixed bed, the residence time being so adjusted that the greater part of the acetic acid reacts with the methanol present to give methyl acetate,(c) separating the top fraction from D1, in a distillation column D2, into a top fraction comprising small quantities of methyl acetate, methanol, dimethyl ether and the organo-halogen compound, and a bottom fraction comprising methyl acetate and methanol, and recycling the top fraction to reactor R,(d) distilling off, via the top of distillation column D3, thType: GrantFiled: January 7, 1982Date of Patent: June 12, 1984Assignee: BASF AktiengesellschaftInventors: Rudolf Kummer, Volker Taglieber, Heinz-Walter Schneider
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Patent number: 4448643Abstract: A process for isolating isobutene from C.sub.4 -hydrocarbon mixtures containing isobutene by reacting the mixture with a primary alcohol in the presence of an acid condensing agent, to form the tertiary ether, separating off the unconverted hydrocarbons and decomposing the tertiary ether in the presence of an acid catalyst at an elevated temperature, wherein a primary C.sub.3 - or C.sub.4 -alcohol is used and the temperature at which the reaction mixture leaves the etherification stage, in which the tertiary ether is formed, is lower than the mean temperature in the etherification stage.Type: GrantFiled: July 13, 1981Date of Patent: May 15, 1984Assignee: BASF AktiengesellschaftInventors: Alfred Lindner, Klaus Volkamer, Ulrich Wagner
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Patent number: 4443559Abstract: Catalytic distillation structure for use in reaction distillation columns, a providing reaction sites and distillation structure and consisting of a catalyst component and a resilient component intimately associated therewith. The resilient component has at least about 70 volume % open space and being present with the catalyst component in an amount such that the catalytic distillation structure consist of at least 10 volume % open space.Type: GrantFiled: September 30, 1981Date of Patent: April 17, 1984Assignee: Chemical Research & Licensing CompanyInventor: Lawrence A. Smith, Jr.
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Patent number: 4440601Abstract: A method and apparatus for high volume distillation of impure liquid, particularly of binary mixtures of relatively low boiling organic substances and water, comprises fractionally distilling the impure liquid to form a vapor of a low boiling organic substance; compressing the vapor; passing at least a portion of the compressed vapor through a vapor composition adjustment zone wherein the organic substance may catalytically or otherwise react or merely stabilize following compression; compressing the vapor exiting the adjustment zone to form a recompressed vapor; cooling the recompressed vapor in heat transfer relation with the impure liquid whereby the vapor at least partially condenses, transferring sufficient heat to the impure liquid for evaporating the liquid and to form the aforementioned low boiling organic vapor; and collecting the condensed low boiling organic vapor.Type: GrantFiled: January 15, 1981Date of Patent: April 3, 1984Inventors: Jerome Katz, Sidney J. Fogel
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Patent number: 4439350Abstract: A method for conducting catalytic chemical reactions and fractionation of the reaction mixture comprising feeding reactants into a distillation column reactor contracting said reactant in liquid phase with a fixed bed catalyst in the form of a contact catalyst structure consisting of closed porous containers containing the catatlyst for the reaction and a clip means to hold and support said containers, which are disposed above, i.e., on the distillation trays in the tower. The trays have weir means to provide a liquid level on the trays to substantially cover the containers. In other words, the trays function in their ordinary manner with the addition thereto of the catalyst. The reaction mixture is concurrently fractionated in the column.Type: GrantFiled: June 21, 1982Date of Patent: March 27, 1984Assignee: Chemical Research & Licensing CompanyInventor: Edward M. Jones, Jr.
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Patent number: 4435595Abstract: The present invention provides a process for the production of high purity methyl acetate from methanol and glacial acetic acid wherein the acetic acid functions both as a reactant and as an extractive agent. The process comprises countercurrently flowing approximately stoichiometric quantities of acetic acid and methanol through a single reactive distillation column in the presence of an acidic catalyst which is preferably sulfuric acid. The column provides intimate contact between the acetic acid and the methanol and between the acetic acid and the azeotropes (methyl acetate/water and methyl acetate/methanol) which are formed in the column. At preferred catalyst concentrations, the residence time in the column is at least about two hours. The process further comprises continuously removing high purity methyl acetate from the top of the column and continuously removing water from the bottom of the column.Type: GrantFiled: April 26, 1982Date of Patent: March 6, 1984Assignee: Eastman Kodak CompanyInventors: Victor H. Agreda, Lee R. Partin
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Patent number: 4431838Abstract: A C.sub.1 -C.sub.4 alkanol and its corresponding acetate or a C.sub.1 -C.sub.2 alkanol and its corresponding propionate are separated by extractive distillation utilizing an aromatic hydrocarbon as the extractive solvent. Transesterification of lower alkanols and lower alkyl acetates or propionates is effected by means of extractive distillation and the preparation of an intermediate ester of a higher boiling alcohol.Type: GrantFiled: February 8, 1982Date of Patent: February 14, 1984Assignee: National Distillers and Chemical CorporationInventors: Julian Feldman, John M. Hoyt
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Patent number: 4409403Abstract: This invention relates to oxyalkylations which take place in the presence of solid acid catalysts. More particularly this invention relates to increasing the selectivity of such processes employing a solid acid catalyst, preferably a polyfluorosulfonic acid catalyst, in which an hydroxylic compound reactant reacts with an alkylene oxide reactant to produce a desired mono-oxyalkylated product which tends to react with the alkylene oxide to produce an undesired second product.Type: GrantFiled: September 28, 1981Date of Patent: October 11, 1983Assignee: Varen TechnologyInventor: Ronald J. Vaughan
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Patent number: 4408063Abstract: Processes for preparing (S) or (R) epihalohydrin and an (S) substituted glycerol intermediate are disclosed.Type: GrantFiled: April 19, 1982Date of Patent: October 4, 1983Assignee: Merck & Co., Inc.Inventors: John J. Baldwin, David E. McClure
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Patent number: 4401514Abstract: A method of recovering or extracting chemicals, such as furfural, formic acid, acetic acid and other organic compounds from acidic hydrolysates of plants or vegetable matter, especially spent sulfite liquors after conversion of the pentosans into pentoses and then into furfural by heating the hydrolysate in an acidic environment. The conversion of the pentosans pentoses into furfural, preferably with acidulation, is accomplished in a counterflow or countercurrent flow heat exchanger and a reactor, preferably a tubular reactor. The hydrolysate which has additionally been heated and converted in the reactor is used as a heating medium or heat carrier for heating up the hydrolysate which is converted in the counterflow heat exchanger, whereupon there is recovered as the distillate furfural in conjunction with the formic acid, acetic acid and the like.Type: GrantFiled: March 18, 1981Date of Patent: August 30, 1983Assignee: Vereinigte Edelstahlwerke AG (VEW)Inventors: Walter Kanzler, Johannes Schedler
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Patent number: 4390398Abstract: 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: GrantFiled: May 12, 1980Date of Patent: June 28, 1983Assignee: Fiberglas Canada LimitedInventors: Robert J. Coker, Gary W. Bate, Henk J. Deuzeman
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Patent number: 4381407Abstract: A process for the continuous production of triacetin consisting essentially of continuously charging liquid glycerol into a first liquid reaction area through which acetic acid vapors and water vapors flow, said liquid reaction area being divided into a number of separate individual areas through which liquid glycerol and liquid acetin reaction products flow in one direction and gaseous acetic acid and water flow in a countercurrent direction, continuously charging acetic acid vapor to a separate individual area where said liquid mixture has an OH number of less than 600, continuously separating a liquid mixture of acetins and water having an OH number of less than 600, continuously passing said liquid mixture into a second liquid reaction area, continuously adding thereto liquid acetic acid anhydride in an amount sufficient to react with water dissolved in said liquid mixture to form acetic acid and to react with monoacetin and diacetin present to form triacetin and continuously recovering triacetin.Type: GrantFiled: January 26, 1981Date of Patent: April 26, 1983Assignee: Henkel Kommanditgesellschaft auf AktienInventors: Norbert Bremus, Gerhard Dieckelmann, Lutz Jeromin, Wolfgang Rupilius, Hartwig Schutt
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Patent number: 4370491Abstract: A process for the preparation of acetic acid esters CH.sub.3 --CO--O--R.sup.1 (I, R.sup.1 =an organic radical other than methyl and ethyl) by alkali-catalyzed trans-esterification of an acetic acid ester CH.sub.3 --CO--O--R.sup.2 (II, R.sup.2 =methyl or ethyl) with an alcohol R.sup.1 --OH (III), accompanied by elimination of the alcohol R.sup.2 --OH (IV), wherein(a) the trans-esterification reaction is carried out in the middle section K.sub.M of a distillation column K, the alcohol III being fed as liquid into the upper zone and the ester II into the lower zone of K.sub.M,(b) the alkaline catalyst is introduced into the upper part K.sub.U of K,(c) the alcohol IV, or a mixture of IV and the ester II, is taken off the top of the column,(d) the mixture obtained from (c) (unless the alcohol IV alone is obtained) is separated in the column section K.sub.U or in a stripper column K.sub.S into IV and the azeotrope of II and IV, and the latter is recycled to the lower zone of K.sub.Type: GrantFiled: May 14, 1981Date of Patent: January 25, 1983Assignee: BASF AktiengesellschaftInventors: Kaspar Bott, Gerd Kaibel, Herwig Hoffmann, Rudolf Irnich, Eberhard Schaefer
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Patent number: 4359533Abstract: An improved fermentation process for producing alcohol which includes the combination of vacuum fermentation and vacuum distillation. Preferably, the vacuum distillation is carried out in two phases, one a fermentor proper operated at atmospheric pressure and a flash phase operated at reduced pressure with recycle of fermentation brew having a reduced alcohol content to the fermentor, using vapor recompression heating of the flash-pot recycle stream to heat the flash-pot or the distillation step, and using "water load balancing" (i.e., the molar ratio of water in the fermentor feed is the same as the molar ratio of water in the distillation overhead).Type: GrantFiled: November 26, 1980Date of Patent: November 16, 1982Assignee: The United States of America as represented by the Department of EnergyInventors: Charles R. Wilke, Brian L. Maiorella, Harvey W. Blanch, Gerald R. Cysewski
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Patent number: 4352940Abstract: In the hydrolysis of methyl acetate to acetic acid, the improvement comprising a flasher or stripper to separate methyl acetate and water from the hydrolyzer product stream and the recycle of these directly to the hydrolyzer.Type: GrantFiled: April 28, 1980Date of Patent: October 5, 1982Assignee: E. I. Du Pont de Nemours and CompanyInventors: Robert L. Adelman, Roy Segars, Jr.