And Returning Distillation Product To A Previous Distillation Zone Patents (Class 203/82)
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Patent number: 5066365Abstract: The invention relates to a process for the isolation of vinyl acetate which involves not combining the bottom product of the recylced gas washings with the water-saturated vinyl acetate but rather introducing it to further multiple distillation columns from the gas mixture formed in the reaction of ethylene with acetic acid and oxygen over catalysts containing palladium or palladium compounds in the gas phase.Type: GrantFiled: October 15, 1990Date of Patent: November 19, 1991Assignee: Hoechst AktiengesellschaftInventors: Gunter Roscher, Karl-Heinz Schmidt, Klaus Eichler, Peter Horstermann, Reinhard Gradl, Horst Langner
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Patent number: 5061349Abstract: A method of isolating trioxane by distillative separation at atmospheric pressure without extraction steps from an aqueous trioxane solution having a trioxane concentration which does not exceed that concentration, which has an constant boiling azeotropic mixture obtained at a simple distillation of said aqueous trioxane solution at normal pressure, includes heating the aqueous trioxane solution, which may also contain formaldehyde and acid, in an evaporator to form a trioxane and water vapor-containing steam mixture substantially of the azeotrope boiling temperature (about 92.degree. C. for a solution containing only water and trioxane); feeding an inert gas stream into either the evaporator or a partial condenser connected directly to the evaporator; leading the steam mixture in a first stage together with the inert gas stream through the partial condensing means, wherein the steam mixture together with the inert gas stream is cooled to a temperature of 58.degree. to 64.degree. C.Type: GrantFiled: July 27, 1990Date of Patent: October 29, 1991Inventors: Herbert Kuppenbender, Helmut Reis
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Patent number: 5035776Abstract: A thermally-integrated extractive distillation process for recovering anhydrous ethanol from fermentation or synthetic feedstocks has a distillation train of four columns. Two columns are preconcentrators operated in parallel. The remaining columns are an extractive distillation dehydrating tower, and an entrainer-recovery column. The two preconcentrators and the dehydrating tower are operated at three successively increasing pressures so that the condensing vapors of the overhead product of the dehydrating tower supply the necessary heat to the reboiler of the intermediate-pressure preconcentrator. The overhead vapors of this preconcentrator are, in turn, used to supply the required heat to the reboiler of the lowest-pressure preconcentrator. The bottom product from each preconcentrator is used to preheat the dilute feed. Additional energy savings are accomplished by the appropriate heat exchange between the various feeds, overheads, and bottoms.Type: GrantFiled: March 29, 1990Date of Patent: July 30, 1991Assignee: University of MassachusettsInventor: Jeffrey P. Knapp
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Patent number: 5031754Abstract: A hydrocarbon material of the starting product is separated in an extractive distillation column in which an N-substituted morpholine whose substituents do not have more than seven carbon atoms is used as a selective solvent. The overhead product comes down as a top product of the extractive distillation and is fed through a coalescer in which the sump product comes down with a solvent content of 20 to 75% by weight at a temperature of 20.degree. to 70.degree. C. and subsequent to that is fed into a separating vessel. There it is separated into a heavier and lighter phase. After that the heavier phase is conducted into an extractive distillation column and the lighter phase into the overhead product distillation column.Type: GrantFiled: January 19, 1990Date of Patent: July 16, 1991Assignee: Krupp Koppers GmbHInventors: Gerd Emmrich, Hans-Christoph Schneider, Ulrich Rudel
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Patent number: 4963232Abstract: Provided by this invention is a process for producing a purified hydrazine hydrate having a low total organic carbon concentration and which involves:a first step which includes distilling an aqueous solution of hydrazine hydrate in the presence of at least one salt selected from the group consisting of chloride, sulfate, phosphate and carbonate of (a) the metals of Group Ia and IIa of the Periodic Table of the Elements, (b) ammonium or (c) hydrazinium to concentrate the aqueous solution of hydrazine hydrate by distilling water and the majority of the total organic carbon constituents off and separating the resultant concentrate as a bottom product, anda second step which includes distilling the resultant concentrate to recover a purified aqueous solution of hydrazine hydrate as a top product and separating an aqueous solution of the above salt as a bottom product.Type: GrantFiled: May 22, 1989Date of Patent: October 16, 1990Assignee: Mitsubishi Gas Chemical Company, Inc.Inventors: Yasuhisa Kuriyama, Shuuzabu Sakaguchi, Toshiaki Kohzaki, Syoichi Nito
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Patent number: 4961826Abstract: A method of distillation employing a heat pump (which may be driven by a compressor) using a vapor stream from within the distillation system as a heat source and a liquid stream from within the distillation system as a heat sink. The selection of heat-source vapors and heat-sink liquid is such that at least one is withdrawn from the phase-contacting region of the distillation system. The return of streams withdrawn from the phase-contacting region of the distillation system to the distillation system is such that at least one of the streams is returned at a temperature different from that of the point from which it was withdrawn, and all withdrawn streams are returned in manner such that a stream removed as vapor is returned at a point with a temperature at most that at the point it was withdrawn, and a stream removed as liquid is returned at a point with a temperature at least that at which it was withdrawn.Type: GrantFiled: August 19, 1986Date of Patent: October 9, 1990Assignee: Trustees of Dartmouth CollegeInventors: Hans E. Grethlein, Lee H. Lynd
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Patent number: 4925535Abstract: The process for production of an aromate concentrate for use as a blending component for gasification fuel includes subjecting another feed hydrocarbon mixture to an extractive distillation using N-substituted morpholines as selective solvent in a extractive distillation column. Low-boiling non-aromates with a boiling range up to about 105.degree. C. practically completely and higher-boiling non-aromates with a boiling range between about 105.degree. and 160.degree. C. to a substantial extent are discharged as a raffinate from the top of the extractive distillation column. The extract bottoms from the extractive distillation are fed to a solvent stripping column where the solvent is at least partially recovered from other hydrocarbons. To eliminate condensation and polymerization products due to components with a boiling point over 170.degree. C.Type: GrantFiled: August 8, 1988Date of Patent: May 15, 1990Assignee: Krupp Koppers GmbHInventors: Gerhard Preusser, Gerd Emmrich, Martin Schulze
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Patent number: 4919765Abstract: Tetrahydrofuran is recovered by a two stage distillation procedure from a crude hydrogenation product resulting from vapor phase hydrogenation of diethyl maleate and containing water, ethanol and a minor amount of n-butanol, and possibly also dissolved hydrogen, in addition to butane-1,4-diol, gamma-butyrolactone and "heavies" such as diethyl ethoxysuccinate. In the first distillation stage, conveniently operated substantially at atmospheric pressure, ethanol, water, and tetrahydrofuran are recovered as overhead product, are condensed to separate the condensible components from a hydrogen stream which can be vented, and then redistilled in the presence of a molar excess of a hydroxylic solvent containing at least two hydroxyl groups, such as butane-1,4-diol, in a second distillation zone.Type: GrantFiled: July 22, 1988Date of Patent: April 24, 1990Assignee: Davy McKee (London) LimitedInventors: Peter R. Wilkes, John Scarlett, George E. Harrison
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Patent number: 4900402Abstract: A pervaporation process for separating at least one component from a mixture of liquids, for example for separating ethanol from a fermentation mass, by a series of three separation steps: separating the mixture by a first pervaporation to form a first permeate vapor enriched in the component to be separated; fractionating the first permeate vapor, for example by temperature condensation, to form a high concentration fraction twice enriched in the component to be separated; and either distilling the high concentration fraction or a second pervaporation to form a distillate or retentate liquid thrice enriched in the component to be separated.Type: GrantFiled: March 25, 1987Date of Patent: February 13, 1990Assignee: Kernforschungszentrum Karlsruhe GmbHInventors: Jurgen Kaschemekat, Frank Schutt, Axel Wenzlaff
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Patent number: 4879407Abstract: A process for the preparation of ethyl trifluoroacetate, in which:in a first stage, trifluoroacetic acid is brought into contact with a slight excess of ethanol in the presence of concentrated sulfuric acid and a solvent, the solvent having a boiling point higher than that of trifluoroacetic acid and specific gravity relative to water less than 1 and which solvent does not form an azeotrope with ethyl trifluoroacetate, and then carrying out a phase separation and removing the sulfuric layer, followed, if required, by an additional stage in which concentrated sulfuric acid is added to complete the esterification;in a second stage, an additional quantity of sulfuric acid and trifluoroacetic acid is introduced and a phase separation is then carried out to remove the sulfuric layer; andin a third stage, the mixture obtained in the second stage is distilled to recover ethyl trifluoroacetate.Type: GrantFiled: October 16, 1987Date of Patent: November 7, 1989Assignee: Rhone-Poulenc ChimieInventor: Louis Amiet
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Patent number: 4857151Abstract: Crude phenol containing methyl benzofuran and other impurities is distilled in the presence of water to recover a phenol bottoms having a reduced quantity of impurities. The water-phenol overhead is cooled to separate a water phase essentially free of methyl benzofuran, which is recycled to the distillation. The organic phase may then be further distilled, in the presence of water, as previously described, to eventually recover a reduced quantity of phenol in which impurities are concentrated.Type: GrantFiled: June 28, 1982Date of Patent: August 15, 1989Assignee: The Lummus CompanyInventors: George D. Suciu, Ali M. Khonsari, Jamin Chen
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Patent number: 4820385Abstract: An improved process for separating high purity alkyl glyoxylate from complex mixtures containing alkyl glyoxylate, alkyl glycolate, water, alcohol and miscellaneous impurities by an azeotropic distillation operation using an azeotroping agent selected from the group consisting of methylene dichloride, 1,1,1--trichloroethane, and benzene.Type: GrantFiled: February 18, 1988Date of Patent: April 11, 1989Assignee: Monsanto CompanyInventors: Dario R. Cova, John M. Thorman
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Patent number: 4814021Abstract: A method for cleaning and reclassifying electrical apparatus designed for use with PCB fluid electrolytes is described which is capable of operation on the site of the equipment being cleaned and while said equipment is energized.Type: GrantFiled: July 27, 1987Date of Patent: March 21, 1989Assignee: ENSR CorporationInventors: Michael J. Massey, David R. Hopper
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Patent number: 4802956Abstract: The instant invention relates to a process for the purification of dimethylether, which contains impurities, by feeding a mixture which contains the dimethylether at specific trays to a distillation column and withdrawal of the dimethylether and of impurities at specific trays of the same column.Type: GrantFiled: November 20, 1986Date of Patent: February 7, 1989Inventors: Horst Dornhagen, Hartmut Hammer, Ewald Meisenburg
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Patent number: 4767869Abstract: A process is described for the production of substantially pure gamma-butyrolactone from a feed mixture containing a major amount of gamma-butyrolactone and a minor amount of diethyl succinate which comprises fractionally distilling the mixture in a fractionation zone in the presence of added diethyl maleate and recovering from the fractionation zone an overhead vaporous product comprising gamma-butyrolactone which is substantially free from diethyl succinate and a liquid bottom product comprising diethyl maleate and diethyl succinate in admixture one with another. This procedure can be used to separate a gamma-butyrolactone rich fraction obtained by distillation in one or more stages of a crude reaction product obtained by hydrogenation of a C.sub.Type: GrantFiled: July 31, 1987Date of Patent: August 30, 1988Assignee: Davy McKee LimitedInventors: George E. Harrison, Norman Harris
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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: 4744869Abstract: A process for purifying methanol which comprises introducing crude synthetic methanol obtained by catalytic reaction of carbon oxide and hydrogen into a rectifying column either as such or after it is first introduced into a topping column and distilled with or without the addition of water to remove low-boiling components from the top of the topping column, and distilling it in the rectifying column to withdraw purified methanol from the top of the column and mainly water from the bottom of the column; wherein an auxiliary distillation column is provided side by side with the rectifying column, and the rectifying column and the auxiliary distillation column are operated under particular conditions.Type: GrantFiled: August 18, 1986Date of Patent: May 17, 1988Assignee: Mitsubishi Gas Chemical Company, Inc.Inventors: Yoshihiko Saito, Osamu Hashimoto
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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: 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: 4695665Abstract: A process flow is presented for a hydrocarbon conversion process in which a relatively volatile hydrocarbon is separated from less volatile feed and product hydrocarbons present in a reaction zone effluent stream. The preferred usage is in the alkylation of benzene with propylene. The reaction zone effluent stream is passed into a lower portion of a rectified separation zone. Recycle aromatic hydrocarbon is passed into a contact exchanger/absorber present in the top portion of the rectified separation zone. The liquid collected at the bottom of the contact exchanger is removed as a sidecut stream and passed into the reaction zone.Type: GrantFiled: July 2, 1986Date of Patent: September 22, 1987Assignee: UOP Inc.Inventor: Richard R. De Graff
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Patent number: 4589957Abstract: Improved process for the separation of a hydrocarbon-containing feedstream comprising monomer, comonomer and diluent into separate product streams which comprises subjecting the feedstream to two-stage distillation provided with a common accumulation zone wherein the condensate from the accumulation zone serves as the source of feed for the second distillation and reflux for the first distillation. In a specific embodiment, a feed comprising ethylene, 1-hexene, and isobutane is separated into separate streams of 1-hexene, ethylene and isobutane, and isobutane for recycle to polymerization.Type: GrantFiled: August 25, 1983Date of Patent: May 20, 1986Assignee: Phillips Petroleum CompanyInventors: Fred T. Sherk, Donald O. Hanson
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Patent number: 4559109Abstract: A process for producing anhydrous ethanol from an ethanol-water mixture feedstock comprising subjecting the feedstock to distillation in a first distillation zone to produce an overhead vapor of from about 80 to about 90 weight percent ethanol, subjecting the thus produced overhead vapor to extractive distillation in an extractive distillation zone to produce anhydrous ethanol vapor overhead of about 99.5 weight percent ethanol and a solvent-rich bottom stream, and stripping the solvent-rich bottom stream and recycling the thus produced lean solvent bottom stream to the extractive distillation zone and recycling the thus produced overhead vapor stream to the first distillation zone. Also disclosed is a system for performing the process.Type: GrantFiled: March 31, 1983Date of Patent: December 17, 1985Assignee: Phillips Petroleum CompanyInventors: Fu-Ming Lee, Robert H. Pahl
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Patent number: 4543163Abstract: Disclosed is a process for recovering a virtually water-free amine from an amine acid salt thereof. The process comprises a unique combination of phase separation stages practiced under mild heating and distillation stages. An amine product containing less than 0.2% water can be achieved by the present process. The feedstock for the process suitably is an acid scrub liquor used to scrub amine from a vapor stream thereof which has been used in a cold-box molding process in the foundry industry or in the cure of vapor permeation curable coatings in the coatings industry.Type: GrantFiled: July 6, 1984Date of Patent: September 24, 1985Assignee: Ashland Oil, Inc.Inventors: David M. Stamerjohn, Richard V. Norton, Gregory P. Sturtz
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Patent number: 4522920Abstract: A flow of fermenting liquor from a fermentor is separated into a yeast concentrate flow, which is recirculated to the fermentor, and a yeast-free flow which is separated in a simple evaporator unit into a first ethanol-enriched vapor flow and a first liquid bottom flow. The first vapor flow is treated to produce the desired ethanol while a major part of the first liquid bottom flow is recirculated to the fermentor. A minor, residual part of the latter flow is fed to a stripping unit where it is separated into a second ethanol-enriched vapor flow and a second liquid bottom flow exhausted of ethanol.Type: GrantFiled: August 16, 1982Date of Patent: June 11, 1985Assignee: Alfa-Laval ABInventors: Conny R. Thorsson, Indrek J. Viira
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Patent number: 4472246Abstract: Disclosed is a process for recovering a virtually water-free amine from an amine acid salt thereof. The process comprises a unique combination of phase separation stages practiced under mild heating and distillation stages. An amine product containing less than 0.2% water can be achieved by the present process. The feedstock for the process suitably is an acid scrub liquor used to scrub amine from a vapor stream thereof which has been used in a cold-box molding process in the foundry industry or in the cure of vapor permeation curable coatings in the coatings industry.Type: GrantFiled: August 20, 1982Date of Patent: September 18, 1984Assignee: Ashland Oil, Inc.Inventors: David M. Stamerjohn, Richard V. Norton, Gregory P. Sturtz
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Patent number: 4469558Abstract: Disclosed is a process for the distillation of readily polymerizable vinyl aromatic compounds and a new polymerization inhibitor therefor. The process comprises subjecting a vinyl aromatic compound to elevated temperatures in a distillation system in the presence of a new polymerization inhibitor comprising 2,6-dinitro-p-cresol. Also disclosed is a distillation method and apparatus for use with this inhibitor.Type: GrantFiled: January 8, 1981Date of Patent: September 4, 1984Assignee: Cosden Technology, Inc.Inventor: James M. Watson
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Patent number: 4447318Abstract: In a method for separating a hydrocarbon mixture into relatively difficultly soluble hydrocarbons and relatively easily soluble hydrocarbons by extractive distillation using a polar solvent comprising feeding the starting hydrocarbon mixture to at least two evaporators, an extractive distillation column, a stripping column and a rectifying column; the improvement wherein(1) the polar solvent discharged at a high temperature from the bottom of the stripping column is recycled to the extractive distillation column after it has been cooled to a suitable temperature by giving up heat to a reboiler of the extractive distillation column, a reboiler of the rectifying column and successively to the two or more evaporators, and(2) the starting hydrocarbon mixture is divided into two or more streams and heated in two or more evaporators, one stream being evaporated in a first evaporator to a pressure necessary for introduction into the extractive distillation column and then fed to the extractive distillation column, aType: GrantFiled: March 28, 1983Date of Patent: May 8, 1984Assignee: Nippon Zeon Co., Ltd.Inventors: Shunichiro Ogura, Masafumi Miyamoto
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Patent number: 4444624Abstract: The disclosure relates to a process for separating acetone from reaction mixtures originating from the reaction of methyl acetate and/or dimethylether with carbon monoxide and optionally hydrogen in the presence of a catalyst system consisting of carbonyl complexes of noble metals of group VIII of the Periodic System of the elements, acetic acid, an organophosphorus or organonitrogen compound, methyl iodide and optionally carbonyl-yielding compounds of common metals.Type: GrantFiled: August 27, 1982Date of Patent: April 24, 1984Assignee: Hoechst AktiengesellschaftInventors: Heinz Erpenbach, Klaus Gehrmann, Winfried Lork, Peter Prinz
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Patent number: 4436902Abstract: A liquid containing a contaminant such as water or polymeric solids is purified. Purification of a liquid containing a contaminant is enhanced by the use of second fractionating column in conjunction with a first fractionating column to recover a portion of the liquid to be purified from the kettle product of the first column. Vapor from a second fractionating column is used to control the total energy input to a first fractionating column.Type: GrantFiled: February 12, 1982Date of Patent: March 13, 1984Assignee: Phillips Petroleum CompanyInventors: William E. Wood, Franklin T. Barber
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Patent number: 4434029Abstract: A process for producing an unsaturated nitrile with saved energy by which the bottom stream from a recovery column is used as the heat source for at least one distillation column in the process and thereafter used to pre-heat a recovery column feed withdrawn from the bottom of an absorption column, characterized in that the bottom stream of the absorption column is previously heated by at least one source of waste heat in the process, the source being selected from (1) the circulating water in the quenching column, (2) the overhead vapor of the absorption column, (3) the overhead vapor of a dehydration column and (4) the overhead vapor of a product column.Type: GrantFiled: December 2, 1981Date of Patent: February 28, 1984Assignee: Asahi Kasei Kogyo Kabushiki KaishaInventors: Shigeru Kurihara, Hiroyuki Ohashi
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Patent number: 4410754Abstract: An olefin isomerization process useful in recovering isobutylene from mixed butylene feed streams is disclosed. Preferably, the feed stream is passed through a first reaction zone to convert some butene-1 to butene-2 and then fed to the lower part of a two-part fractionation system. The butene-2-rich bottoms is withdrawn and the overhead vapor is passed through a second reaction zone in admixture with hydrogen before entering the second or upper part of the fractionation system. The bottoms liquid of the upper part of the fractionation system flows into the lower part of the fractionation system. Isobutylene and recycle hydrogen are recovered from the overhead vapor of the upper part of the fractionation system.Type: GrantFiled: September 29, 1982Date of Patent: October 18, 1983Assignee: UOP Inc.Inventor: Steve A. Gewartowski
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Patent number: 4401515Abstract: In a process for producing butadiene or isoprene having a high purity comprising a step of treating a C.sub.4 or C.sub.Type: GrantFiled: March 11, 1981Date of Patent: August 30, 1983Assignee: Japan Synthetic Rubber Co., Ltd.Inventors: Masatoshi Arakawa, Kazuyoshi Nakazawa
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Patent number: 4385965Abstract: In a process for recovering pure methylal from methanol-methylal mixtures, which can optionally contain still further compounds, the separation conducted in a rectification device comprising two rectifying columns. In the first rectifying column, the mixture to be separated is rectified under a pressure lower than that in the second column, into a methylal-rich, methanol-poor distillate, and into a practically methylal-free, methanol-rich sump product. The methylal-rich distillate of the first rectification is then separated in a second rectifying column, operated under a higher pressure than the first rectification column, into a compound stream containing methanol and methylal, which is then recycled to the first rectifying column, and into pure methylal as the sump product.Type: GrantFiled: January 26, 1982Date of Patent: May 31, 1983Assignee: Chemische Werke Huls A.G.Inventors: Wolfgang H. E. Muller, Manfred Kaufhold
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Patent number: 4385964Abstract: A method is disclosed for preventing the condensation of aluminum chloride (AlCl.sub.3) in a fractional distillation column which is operated to separate a fraction which does not include AlCl.sub.3 from a mixture containing AlCl.sub.3 and other metal chlorides and which is operated at temperatures which include the sublimation or melting points of AlCl.sub.3 at the operating pressure of the column. According to this method, titanium tetrachloride (TiCl.sub.4) is maintained in the column in an amount at least as great, by weight, as the amount of AlCl.sub.3 contained in the mixture.Type: GrantFiled: May 26, 1982Date of Patent: May 31, 1983Assignee: Aluminum Company of AmericaInventors: Roger C. Johnson, Donald L. Stewart, Jr., Utah Tsao, David A. Wohleber
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Patent number: 4362603Abstract: Crude acetonitrile is purifed to 99+ weight percent by a continuous distillation procedure.Type: GrantFiled: January 2, 1981Date of Patent: December 7, 1982Assignee: The Standard Oil CompanyInventors: Robert D. Presson, Hsin-Chih Wu, Edward J. Sockell
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Patent number: 4362604Abstract: A process for the isolation of hydroquinone, pyrocatechol, phenol and carboxylic acid from the reaction mixture containing the same such as one obtained by reaction of phenol with percarboxylic acid is disclosed. The reaction mixture is fed to a first rectification column and subjected to distillation whereby there is obtained a bottoms product containing pyrocatechol, hydroquinone and phenol. The top product is largely condensed and recycled, there being withdrawn from the top of the rectification column a mixture comprising phenol and carboxylic acid. The phenol and carboxylic acid mixture are continuously fed to a second rectification column where carboxylic acid is separated from phenol and substantially pure phenol is withdrawn from the stripping section and/or bottom of the second rectification column.Type: GrantFiled: August 14, 1981Date of Patent: December 7, 1982Assignee: Bayer AktiengesellschaftInventors: Christoph Jupe, Helmut Waldmann, Jurgen Baumert, Gunther Schummer
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Patent number: 4358536Abstract: A flow of fermenting liquor from a fermentor is separated into a yeast concentrate flow, which is recirculated to the fermentor, and a yeast-free flow which is separated in a simple evaporator unit into a first ethanol-enriched vapor flow and a first liquid bottom flow. The first vapor flow is treated to produce the desired ethanol while a major part of the first liquid bottom flow is recirculated to the fermentor. A minor, residual part of the latter flow is fed to a stripping unit where it is separated into a second ethanol-enriched vapor flow and a second liquid bottom flow exhausted of ethanol.Type: GrantFiled: February 22, 1980Date of Patent: November 9, 1982Assignee: Alfa-Laval ABInventors: Conny R. Thorsson, Indrek J. Viira
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Patent number: 4349420Abstract: Metal chlorides such as aluminum chloride (AlCl.sub.3) are separated from a mixture containing metal chlorides including AlCl.sub.3 and ferric chloride (FeCl.sub.3). In order to effect this separation, the mixture is subjected to a fractional distillation process utilizing an array of distillation columns. According to this process, the mixture is introduced into a first distillation column which is operated at temperatures and pressures sufficient to separate FeCl.sub.3 from the mixture while avoiding the formation of a solid solution of FeCl.sub.3 and AlCl.sub.3 within the column. At least one additional distillation column is then employed to separate metal chlorides from the remaining mixture from the first column.Type: GrantFiled: January 12, 1981Date of Patent: September 14, 1982Assignee: Aluminum Company of AmericaInventor: Donald L. Stewart, Jr.
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Patent number: 4347321Abstract: 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: GrantFiled: October 7, 1980Date of Patent: August 31, 1982Assignee: Bio-Systems Research, Inc.Inventors: Joseph E. Lionelle, Jeffrey A. Staffa, William L. McCormick
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Patent number: 4342627Abstract: The present invention relates to a continuous process for producing substantially anhydrous alcohols from aqueous solutions thereof by distilling a mixture of aqueous alcohol and an entrainer to a drying column withdrawing an azeotrope as a distillate and continuously recovering anhydrous alcohol with less than 0.1% by weight of water from the base of the drying column. The improvement resides in feeding the distillate to a condenser and introducing (a) the condensate therefrom in a substantially non-turbulent state into a decanter at a point close to the interface between the aqueous and organic phases present therein and (b) a specified amount of water, which is less than 0.25 volumes per volume of the anhydrous alcohol recovered, into the drying column at a point adjacent to that at which the organic hydrocarbon phase is returned as reflux.Type: GrantFiled: April 16, 1981Date of Patent: August 3, 1982Assignee: BP Chemicals LimitedInventors: Charles Cane, Bertram Yeomans
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Patent number: 4318782Abstract: A process for distilling ammoniacal solutions is disclosed comprising the utilization of two distillation columns operating at different pressures, the ammoniacal solution to be distilled being sent--after being mixed with the ammoniacal vapors flowing from the top of the column operating at the lower pressure--to the column operating at the higher pressure, from the bottom of which the partially distilled ammoniacal solution is sent to the column operating at the lower pressure; the liquid ammonia being recovered at the top of the column operating at the higher pressure while the residual ammoniacal solution is withdrawn from the bottom of the column operating at the lower pressure.Type: GrantFiled: January 6, 1981Date of Patent: March 9, 1982Assignee: Montedison S.p.A.Inventors: Giorgio Pagani, Fabrizio Socci
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Patent number: 4308111Abstract: A distillation device is provided which comprises a vaporization zone, a condensation zone, a vapor permeable barrier between the vaporization zone and the condensation zone comprising a membrane having a plurality of openings, and means for maintaining an air pressure gradiant across the barrier whereby air pressure on the vaporization zone side of the membrane is greater than air pressure on the condensation zone side of the membrane.Type: GrantFiled: February 19, 1980Date of Patent: December 29, 1981Inventor: Leonard F. Pampel
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Patent number: 4305790Abstract: The recovery of alcohol from fermentation liquors is accomplished by the evaporation of the liquor feed and simultaneous rectification of the volatile component. Evaporation of the liquor feed can be accomplished by a single flash evaporation or multiple effect evaporation combined with the flash evaporation in which the flash evaporator is one effect of the multiple effect evaporator. A concentrated alcohol component is recovered along with a concentrated residue useful as a fertilizer or animal feed supplement.Type: GrantFiled: January 31, 1980Date of Patent: December 15, 1981Inventor: Edward F. Kramer, Sr.
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Patent number: 4302298Abstract: Process for isolating methyl tert-butyl ether contained in the reaction product of methanol with a C.sub.4 hydrocarbon cut containing isobutene, comprising fractionating said reaction product by introducing it at an intermediate point of a distillation zone, recovering methyl tert-butyl ether at the bottom thereof and, at the top thereof, a mixture of C.sub.4 hydrocarbons with methanol which is washed with water and condensed and wherefrom is separated a condensed C.sub.4 hydrocarbon fraction, a portion of which is fed back as reflux to the top of the distillation zone and another portion discharged, and separating the remaining water-methanol mixture by distillation.Type: GrantFiled: February 22, 1980Date of Patent: November 24, 1981Assignee: Institut Francais du PetroleInventors: Paul Mikitenko, Lionel Asselineau
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Patent number: 4299667Abstract: A process for recovering pure benzene from hydrocarbon mixtures containing the same and non-aromatic compounds which are gaseous and difficultly condensible is described in which the feedstock is fed to an initial distillation column operated at atmospheric or sub-atmospheric pressure. Overhead comprising benzene and non-aromatics is obtained and a portion thereof condensed. The condensible material is in part returned to the distillation column and in part subjected to extractive distillation to recover pure benzene. Those components which did not condense, i.e. the non-condensible and difficultly condensible components and entrained aromatics are fed to a reflux vessel such as a scrubber, stripper, or the like for recovery of any benzene or other valuable components which might be soluble in a selective solvent and used for such recovery. The selective solvent can be the same solvent used for the extractive distillation.Type: GrantFiled: July 28, 1980Date of Patent: November 10, 1981Assignee: Metallgesellschaft AktiengesellschaftInventors: Helmut Klein, Kamar P. John
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Patent number: 4294666Abstract: A process for the manufacture of 4,4'-diphenylmethane diisocyanate and a mixture of diphenylmethane diisocyanate isomers containing a controllable amount of uretdione and hydrolizable chlorine which comprises feeding crude MDI to an evaporator, condensing a head fraction in two stages in the presence of an inert gas, feeding the first stage condensate to a distillation column, producing a mixture of diphenylmethane diisocyanate isomers as an overhead, producing 4,4'-diphenylmethane diisocyanate as a side draw, and condensing each of the overhead and side draw in two stages in the presence of an inert gas.Type: GrantFiled: August 15, 1980Date of Patent: October 13, 1981Assignee: BASF AktiengesellschaftInventors: Hans J. Astheimer, Horst Brandtstaedter, Rainer Ohlinger, Willy Van Pee, Jaak Van Steen, Friedrich Sauer, Rudolf Schmidt, Siegfried Krueger
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Patent number: 4292141Abstract: A process for isolating butadiene, with the aid of a selective solvent, from a C.sub.4 -hydrocarbon mixture which contains butadiene and small amounts of styrene and may contain oxygen, hydrocarbons more soluble than butadiene in the selective solvent and hydrocarbons less soluble than butadiene in the selective solvent, in which process the C.sub.4 -hydrocarbon mixture is separated by extractive distillation into a distillate which contains the less soluble hydrocarbons, a stream of butadiene and a stream containing the more soluble hydrocarbons, and in which a mixture of styrene and C.sub.4 -hydrocarbons is removed from the C.sub.4 -hydrocarbon mixture in a distillation zone upstream of the extractive distillation, the top product of the said distillation zone being fed to the extractive distillation.Type: GrantFiled: August 22, 1979Date of Patent: September 29, 1981Assignee: BASF AktiengesellschaftInventors: Alfred Lindner, Klaus Volkamer, Ulrich Wagner, Dieter Pommer, Klaus-Juergen Schneider, Harald Schwentker
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Patent number: 4285774Abstract: An apparatus for continuously producing concentrated alcohol from beer comprises a plurality of concentrator cells and a plurality of salvage cells arranged in a line in side-by-side relation. Liquid beer, supplied to the first upstream concentrator cell through a supply conduit, flows through passages between adjacent cells in response to the volume of beer reaching a predetermined level in the adjacent upstream cell. A microwave ignition bulb is positioned in each cell to heat the liquid beer and boil or vaporize the alcohol content thereof. The gaseous alcohol is serially bubbled through a fluid passage from each concentrator cell to the next adjacent upstream cell until the gaseous alcohol reaches the first concentrator cell where the gaseous alcohol is concentrated and condensed in a column to a liquid solution containing approximately 95% alcohol and approximately 5% water.Type: GrantFiled: June 30, 1980Date of Patent: August 25, 1981Assignee: Agrohol Systems, Inc.Inventor: A. H. J. Rajamannan
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Patent number: 4282389Abstract: A process for the simultaneous manufacture of pure methyl tertiary butyl ether (MTBE) and a substantially isotubene-free mixture of C.sub.4 -hydrocarbons, by reacting the isobutene contained in the mixture of C.sub.4 -hydrocarbons with excess methanol in the liquid phase at elevated temperatures on strongly acid, macroporous, organic ion exchange resins.The process has the following steps:(a) methanol and isobutene are reacted in a molar ratio of 2:1 to 5:1 at temperatures between 30.degree. and 100.degree. C.;(b) the unconverted hydrocarbons are then removed as the top product under a pressure of 2 to 10 bars from a first rectification column;(c) the bottom product from this first column is rectified in a second column under normal pressure or under a slight excess pressure of up to 2 bars at the top of the column, the bottom product of this rectification is recycled to reaction zone (a), if necessary, after separating off a portion of the tertiary butanol formed and the C.sub.Type: GrantFiled: December 4, 1979Date of Patent: August 4, 1981Assignee: Chemische Werke Huls A.G.Inventors: Wilhelm Droste, Fritz Obenaus
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Patent number: 4278505Abstract: A process of recovering an n-hexane product which is free from aromatic compounds by extractive distillation from a mixture of aromatic and non-aromatic compounds. The mixture is fed to and distilled in a first distillation column, from which a benzene-containing sump product and the overhead product consisting of non-aromatic compounds are withdrawn. The distillate is laterally withdrawn above the feeding point of the feed mixture and transferred to the upper portion of a second distillation column. The hexane cut is withdrawn as sump product from the second distillation column and fed to an extractive distillation column approximately in the middle thereof and is extracted in the extractive distillation column with a selective solvent which is fed above the feeding point of the hexane cut consisting of the sump product of the second distillation column. The sump product containing the selective solvent is withdrawn from the extractive distillation column and the overhead thereof vapors are condensed.Type: GrantFiled: October 10, 1978Date of Patent: July 14, 1981Assignee: Metallgesellschaft AktiengesellschaftInventors: Hans F. Danulat, Kamar P. John, Helmut Klein, Stephen Lukatsch