Initial Distillation Under Positive Pressure Or Vacuum Patents (Class 203/80)
  • Patent number: 5449440
    Abstract: From a mixture containing methanol, ethanol, n-propanol, isobutanol water and other high-boiling and low-boiling compounds, the claimed process enables three separate streams to be obtained, one an anhydrous stream of methanol or methanol and ethanol (I), one containing most of the n-propanol present in the feed mixture (II), and one containing most of the isobutanol present in the feed mixture (III), by using three fractionating columns.
    Type: Grant
    Filed: November 15, 1993
    Date of Patent: September 12, 1995
    Assignee: Snamprogetti S.p.A.
    Inventors: Carlo Rescalli, Flavio Cianci
  • Patent number: 5435436
    Abstract: A thermomechanically integrated distillation column and method for the separation of ethylene from ethane and other close-boiling light hydrocarbons. The column has a plurality of sections operated at successively lower pressures from a high pressure subcritical section to a superatmosphere bottoms product zone. Bottoms liquid from the high pressure and intermediate sections are flashed in respective cooling loops to about the pressure of the section of next lower pressure, vaporized in heat exchange with an overhead condensing zone and introduced to the top stage of next lower pressure section. Vapor from the intermediate sections and the bottoms product zone are compressed in respective compression loops and fed to the bottom stage of the section of the next higher pressure. External refrigerant can be supplied to the overhead condensing zone for trim as needed for control purposes.
    Type: Grant
    Filed: January 21, 1994
    Date of Patent: July 25, 1995
    Inventors: David B. Manley, Dominic G. Greene
  • Patent number: 5429721
    Abstract: A process for preparing diacetoxybutene, including:reacting butadiene, acetic acid and oxygen in the presence of a palladium-based catalyst;feeding continuously the resulting reaction product into a first distillation tower;feeding continuously a withdrawn bottoms withdrawn from the first distillation tower into a second distillation tower;withdrawing bottoms containing high boiling point materials from the bottom of the second distillation tower, so that the content of the high boiling point materials in the bottoms of the second distillation tower is not more than 20 wt %;feeding continuously the withdrawn bottoms into a thin-film evaporator whose internal pressure is kept lower than the bottom pressure of the second distillation tower to carry out evaporation treatment; andrecycling the evaporated materials mainly containing diacetoxybutene into the second distillation tower.
    Type: Grant
    Filed: May 18, 1994
    Date of Patent: July 4, 1995
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Hiroaki Kandori, Nobuyuki Murai
  • Patent number: 5413681
    Abstract: A process useful for the recovery of terephthalic acid and ethylene glycol from poly(ethylene terephthalate) or its copolymers. The process is economical, beneficial to the environment and provides polymer grade terephthalic acid and ethylene glycol from post-consumer resin. The process is a six-step process including: (1) contacting a resin containing poly(ethylene terephthalate) with water at elevated temperature and pressure, (2) cooling the resulting mixture to provide a solid portion containing terephthalic acid and a liquid portion containing ethylene glycol, (3) recovery of the ethylene glycol from the liquid portion by distillation, (4) recovery of the terephthalic acid by heating the solid portion in the presence of water vapor at elevated temperature to produce a vapor containing terephthalic acid and water, (5) cooling terephthalic acid water vapor mixture to a temperature below the dew point of terephthalic acid and (6) collecting the polymer grade terephthalic acid.
    Type: Grant
    Filed: November 15, 1993
    Date of Patent: May 9, 1995
    Assignee: Eastman Chemical Company
    Inventors: Gerald C. Tustin, Thomas M. Pell, Jr., David A. Jenkins, Mary T. Jernigan
  • Patent number: 5370774
    Abstract: The invention relates to a process for isolating pure diketene with recovery of materials of value by continuous, two-stage distillation of crude diketene at reduced pressure and with continuous reaction of the resulting distillation residue with acetic acid, pure diketene and acetic anhydride being separated off by means of the two-stage distillation. In the stabilization of the distillation residue with acetic acid, reutilizable acetic acid, which contains acetone with or without acetic anhydride, is recovered.
    Type: Grant
    Filed: November 3, 1993
    Date of Patent: December 6, 1994
    Assignee: Wacker-Chemie GmbH
    Inventors: Gerhard Kuenstle, Alois Maier
  • Patent number: 5354430
    Abstract: Contaminants are removed from impure propylene oxide by fractionating in a first column to remove overhead essentially all of the pentenes and pentanes and most of the oxygen-containing impurities to provide a partially purified first propylene oxide bottoms fraction, extractively distilling the first bottoms fraction in a second extractive column using a C.sub.2 to C.sub.6 alkylene glycol extractive distillation agent to form a second overhead fraction comprising propylene oxide, hexenes, hexanes, water, residual quantities of pentenes and pentanes and oxygen-containing impurities, extractively distilling the second overhead fraction in a third column using a C.sub.6 to C.sub.10 alkane hydrocarbon extractive distillation agent to form a third bottoms fraction comprising the extractive distillation agent, propylene oxide, hexenes, hexanes, residual quantities of pentenes and pentanes and water, and extractively distilling said third bottoms fraction in a fourth column using a C.sub.6 to C.sub.
    Type: Grant
    Filed: October 26, 1993
    Date of Patent: October 11, 1994
    Assignee: Texaco Chemical Company
    Inventors: William K. Culbreth, III, Yu-Hwa E. Sheu, David G. Pottratz
  • Patent number: 5348624
    Abstract: For separating ETBE and ethanol the following principal stages are employed:(1) Extraction of ethanol by water, the raffinate being ETBE saturated in water and the extract an ethanol/water mixture containing a small proportion of ETBE;(2) Concentration of the above mixture, the distillate being a mixture close to the ethanol/water azeotrope in composition and containing a very small proportion of ETBE;(3) Heteroazeotropic distillation of this distillate in two coupled columns with an overhead decanter, this distillation using ETBE as azeotroping agent; the residue of the first column being ethanol which is ca. 99% by mole and the residue of the second column being practically pure water, this water and the water recovered during the concentration stage being used as extraction solvent in stage (1).Stage (3) may be an ethanol dehydration unit using ETBE as dehydrating agent.
    Type: Grant
    Filed: November 12, 1992
    Date of Patent: September 20, 1994
    Assignee: Institut Francais du Petrole
    Inventors: Annick Pucci, Paul Mikitenko, Massimo Zuliani
  • Patent number: 5342509
    Abstract: A process flow sequence for the reduction of polymer fouling while maintaining efficient production levels wherein a dual pressure, dual column configuration is used to effect the reduction in polymer fouling. The dual pressure, dual column configuration of the invention uses a high pressure and a separate low pressure to isolate the desired fractions while effecting a reduction in the production of fouling polymers.
    Type: Grant
    Filed: September 24, 1992
    Date of Patent: August 30, 1994
    Assignee: Exxon Chemical Patents Inc.
    Inventors: Sheri R. Snider, David A. Bamford, Rimas V. Vebeliunas, Roy T. Halle, Robert D. Strack
  • Patent number: 5342488
    Abstract: A process for the separation of 1,4-butanediol from mixtures obtained by the catalytic hydrogenation of maleates, fumarates, and/or succinates, which also contain tetrahydrofuran, water, C.sub.1 -C.sub.4 alcohols, succinic diesters, hydroxybutyrates, alkylhydroxyalkyl succinates, gamma-butyrolactone and butyrates, in addition to 1,4-butanediol, comprising the following steps:a) separating, in a first column having an actual number of plates of from 20 to 70 and operated at a top pressure of from 50 to 1100 mbar and preferably from 50 to 500 mbar and a top temperature of from 40.degree. to 120.degree. C., alcohol, water and tetrahydrofuran, as overhead product,b) feeding the bottom product of the first column into a second column having an actual number of plates of from 30 to 90 and withdrawing the overhead product consisting of alcohol and butyrate and obtained at a top pressure of from 45 to 250 mbar and a top temperature of from 45.degree. to 120.degree. C.
    Type: Grant
    Filed: February 17, 1993
    Date of Patent: August 30, 1994
    Assignee: BASF Aktiengesellschaft
    Inventors: Hans-Juergen Gosch, Harald Rust, Rolf Fischer, Claus Hechler, Rolf Pinkos
  • Patent number: 5328670
    Abstract: A method of regenerating an etching waste fluid, includes the steps of dissolving HCl gas in an etching waste fluid at a temperature falling within a range of 20.degree. C. to 50.degree. C. and crystallizing NiCl.sub.2 and FeCl.sub.2 crystals, the etching waste fluid containing NiCl.sub.2, FeCl.sub.3, and FeCl.sub.2 and being obtained by etching Ni or an Ni alloy with an etching solution consisting of an aqueous solution containing FeCl.sub.3, distilling a mother liquor at the atmospheric pressure after crystallization and separation thereof to reduce the HCl concentration in the mother liquor, and distilling, at a reduced pressure, a concentrate obtained upon distillation at the atmospheric pressure to further reduce the HCl concentration, thereby obtaining an aqueous solution containing FeCl.sub.
    Type: Grant
    Filed: March 20, 1992
    Date of Patent: July 12, 1994
    Assignees: Nittetu Chemical Engineering, Ltd., Kabushiki Kaisha Toshiba
    Inventors: Teruhiko Hirabayashi, Yoshiyuki Imagire, Toshiaki Kurihara, Eiichi Akiyoshi, Ryoichi Maekawa
  • Patent number: 5302255
    Abstract: Polyether glycols, especially poly(tetramethylene ether) glycol (PTMEG) having a narrow molecular weight distribution of about 1.25 to 1.80, or dispersity of 1.05 to 1.90, are made by a process involving distilling the low molecular weight fraction in unit operations including at least one short-path distillation evaporator. Two short-path distillation evaporators, in series, are desirable if significant narrowing of the PTMEG is required. In these units, PTMEG is subjected to temperatures in the range of 270.degree.-400.degree. C. with the hold-up time varying between 10-200 seconds. The required vacuum to force the separation of the low molecular weight PTMEG varies between 0.001 mm and 1.0 mbar. PTMEG residue from the distillation unit is also characterized by its low water content and low concentration of oligomeric cyclic ethers.
    Type: Grant
    Filed: September 15, 1992
    Date of Patent: April 12, 1994
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: Suriyanarayan Dorai, Frank L. Rawling, Jr., James A. Schultz
  • Patent number: 5294304
    Abstract: This invention relates to a process for the production of absolute alcohol from aqueous alcohol, whereby saving of energy to a greater extent is rendered possible in a more simple process, as compared with the prior art azeotropic distillation method using benzene or cyclohexane. That is, aqueous alcohol is subjected to extractive distillation in a first distillation column under such a condition that a liquid and gas of a solvent simultaneously coexist using low pressure propane, propylene and butane as the solvent, absolute alcohol substantially free from water is recovered from the bottom of the distillation column and subjected to stripping of hydrocarbons in a second distillation column, during which the gaseous phases of the first and second distillation columns are mixed and compressed, utilized through recompression as a heat source of a reboiler of the first distillation column, subjected to separation of water content and recycled to the upper parts of the first and second distillation columns.
    Type: Grant
    Filed: March 9, 1993
    Date of Patent: March 15, 1994
    Assignee: Ministry of International Trade and Industry
    Inventors: Yoshikazu Kano, Hirotoshi Horizoe, Tetsuya Tanimoto, Itsuo Yamamoto
  • Patent number: 5288370
    Abstract: For the separation of butenes and butanes by extractive distillation, a charge mainly containing butenes and butanes is contacted in an extractive distillation column under pressure with a first selective polar solvent, S1 (e.g., dimethyl formamide), the butanes being collected at the top. The solvent S1 containing the butenes and passing out at the bottom is mixed with a second solvent, S2, having a boiling point intermediate between that of butenes and that of the solvent S1, the mixture passing into a desorption column under pressure, where the butenes are collected at the top. The mixture of solvent S1 and S2 is separated in a purification column under atmospheric pressure, the solvent S2 passing out at the top is recycled to the desorption column, and the solvent S1 passing out at the bottom is recycled to the extractive distillation column.
    Type: Grant
    Filed: March 20, 1992
    Date of Patent: February 22, 1994
    Assignee: Institut Francais Du Petrole
    Inventors: Lionel Asselineau, Alexandre Rojey
  • Patent number: 5264087
    Abstract: Disclosed is a continuous method for refining acetic anhydride produced by the reaction of ketene and acetic acid by means of a vacuum distillation system to provide a refined material comprised of at least 99.5 weight percent acetic anhydride, not more than 0.5 weight percent acetic acid and not more than about 90 parts per million (ppm) diketene.
    Type: Grant
    Filed: October 13, 1992
    Date of Patent: November 23, 1993
    Assignee: Eastman Kodak Company
    Inventors: H. Ford Lowery, Steven L. Cook, Vicky K. Pinto
  • Patent number: 5262016
    Abstract: A stream of raw phenol, coming from the acidic cracking of cumene hydroperoxide, is purified by a process of extractive distillation carried out in the presence of acetophenone.
    Type: Grant
    Filed: May 24, 1991
    Date of Patent: November 16, 1993
    Assignee: Enimont Anic S.r.l.
    Inventors: Loreno Lorenzoni, Salvatore Simula, Giuseppe Messina, Vittorio Bruzzi
  • Patent number: 5242550
    Abstract: For the separation of butanes and butenes by extractive distillation, a charge mainly containing butanes and butenes is contacted in an extractive distillation column under pressure with a polar solvent (e.g., dimethyl formamide), the butanes being collected at the head. The solvent containing the butenes passes into a second column under pressure, where the butenes are partly desorbed and collected at the head. The solvent still containing butenes is purified in a third column under atmospheric pressure and the solvent-containing vapor distillate thereof is returned, after compression, to the lower part of the second column.
    Type: Grant
    Filed: February 26, 1992
    Date of Patent: September 7, 1993
    Assignee: Institut Francais du Petrole
    Inventors: Lionel Asselineau, Paul Mikitenlo
  • Patent number: 5240566
    Abstract: A process for separating acetone, dichloromethane and trifluoroacetic acid from a mixture of acetone, dichloromethane, and a trifluoroacetic acid/acetone azeotropeby (1) fractionally distilling the mixture of acetone, dichloromethane, and the trifluoroacetic acid/acetone azeotrope;(2) fractionally distilling the mixture of the trifluoroacetic acid/acetone azeotrope and free acetone;(3) adding at least about 16 parts of water to the trifluoroacetic acid/acetone azeotrope per 100 parts by volume of the trifluoroacetic acid/acetone azeotrope;(4) fractionally distilling the mixture of free acetone and the water/trifluoroacetic acid azeotrope;(5) adding at least about 10 parts of sulfuric acid to the water/trifluoroacetic acid azeotrope per 100 parts by volume of the water/trifluoroacetic acid azeotrope;(6) fractionally distilling the mixture of trifluoroacetic acid and the water/sulfuric acid complex.
    Type: Grant
    Filed: December 7, 1992
    Date of Patent: August 31, 1993
    Assignee: The Goodyear Tire & Rubber Company
    Inventors: Bruce R. Hahn, Thomas R. Maier, Surendra K. Chawla
  • Patent number: 5223101
    Abstract: Purification of crude sulfolane to remove color imparting and turbidity imparting impurities therefrom is achieved by a two-pass distillation process wherein purified sulfolane is withdrawn from the bottom of a column in the second distillation pass.
    Type: Grant
    Filed: February 22, 1991
    Date of Patent: June 29, 1993
    Assignee: Phillips Petroleum Company
    Inventor: David L. Yeary
  • Patent number: 5217582
    Abstract: A process is provided for separating high purity alkyl glycolate from a gaseous reaction mixture resulting from the catalyzed gas phase oxidation of alkyl glycolate. A hot solvent which is immiscible with water but selectively dissolves alkyl glycolate and alkyl glyoxylate is brought in contact with the gaseous reaction mixture, and water and alcohol vapors are removed from the hot solvent. The alkyl glyoxylate is removed from the solution by a first distillation and the alkyl glycolate and solvent are then separated in a second distillation.
    Type: Grant
    Filed: February 7, 1992
    Date of Patent: June 8, 1993
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: George E. Heinsohn, John F. Kook, John R. Kosak, Rudolf E. Svadlenak
  • Patent number: 5209826
    Abstract: A steam stripping fraction of sesame seed oil with increased concentration of sesamin and episesamin is used in a molecular distillation process to obtain a fraction containing more than 70 weight % of sesamin and episesamin. The steam stripping fraction is preferably obtained by a steam stripping process wherein the temperature (t.degree. C.) of the sesame seed oil and the pressure (P mmHg) for the process are such that {(4.24.times.10.sup.3)/(9.41-log P)}-273 .ltoreq.t.ltoreq.280 and 0.5.ltoreq.P.ltoreq.20.
    Type: Grant
    Filed: July 28, 1992
    Date of Patent: May 11, 1993
    Assignee: Takemoto Yushi Kabushiki Kaisha
    Inventors: Tatsuhiko Ozaki, Yasunari Hoshii, Hirokazu Matsueda
  • Patent number: 5209825
    Abstract: A distillation process for the preparation of purified concentrated BDO.High boiling impurities, including color formers, precursors of color formers and tar formers are removed from the BDO early in the process and under mild conditions.
    Type: Grant
    Filed: April 24, 1991
    Date of Patent: May 11, 1993
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: Hashim M. Badat, Peter G. Gelblum, Robert E. Trotter
  • Patent number: 5207874
    Abstract: The purification by distillation of glycidyl (meth)acrylate containing light products containing epichlorohydrin and light impurities, and heavy impurities comprises: in a first stage, a distillation of the glycidyl (meth)acrylate to be purified is conducted in the presence of a first solvent, e.g., water, capable of forming a low boiling point heteroazeotrope with the light impurities and epichlorohydrin, so as to obtain a head fraction which consists essentially of a solvent-light products heteroazeotrope; and, in a second stage, the glycidyl (meth)acrylate thus freed from the light products is subjected to a distillation in the presence of a second solvent, e.g.
    Type: Grant
    Filed: June 20, 1991
    Date of Patent: May 4, 1993
    Assignee: Atochem
    Inventors: Raymond Hess, Christian Lacroix
  • Patent number: 5190618
    Abstract: A process for the production of tocopherols (T) and tocotrienols (T3) from palm fatty acid distillates (PFAD). The process includes converting free fatty acids and glycerides in PFAD into alkyl esters, then separating T and T3 from the alkyl esters and other impurities. The T and T3 are concentrated by ion-exchange and further concentrated by distilling the resulting product. Specific catalysts and optimum temperatures for the process are included. The resulting purified tocopherols and tocotrienols are useful substances, exhibiting antioxidant and physiological activities.
    Type: Grant
    Filed: March 31, 1989
    Date of Patent: March 2, 1993
    Assignees: Bioindustry Development Centre (BIDEC), Palm Oil Research & Development Board
    Inventors: Abdul G. Md. Top, Leong W. Leong, Augustine S. H. Ong, Tsukasa Kawada, Hisashi Watanabe, Nozomu Tsuchiya
  • Patent number: 5183538
    Abstract: A method for recovering a liquid diluent having a low salt content from an organic/aqueous mixture which contains significant quantities of the diluent, an alkali metal salt, and water comprises an integrated process which joins extraction and ion exchange steps and a reaction for the conversion of an alkali metal hydroxide. In the initial step the diluent is extracted from the original mixture employing a suitable extractant material. The extract from the initial step containing diluent, extractant material, along with reduced quantities of water and salt, is passed to an ion exchange column for conversion of the alkali metal salt to its hydroxide. In a following fractional distillation dewatering column the diluent begins to react with the alkali metal hydroxide to form an alkali-metal salt of aminocarboxylic acid which can pass harmlessly through the dewatering column for removal in further following fractional distillation step.
    Type: Grant
    Filed: December 24, 1990
    Date of Patent: February 2, 1993
    Assignee: Phillips Petroleum Company
    Inventors: Lacey E. Scoggins, Fu M. Lee, Allen T. Chang, Wiley D. Perkins
  • Patent number: 5176800
    Abstract: A process to modernize existing urea plants which use a stripping with carbon dioxide, and to increase urea yields and flexibility under overload conditions while at the same time reducing energy consumption, corrosion phenomena and possible risks of explosive mixtures. The plant includes: a passivation stage with the introduction of an oxidizing agent and reduction of the air fed to the system; a medium pressure distillation stage of the products leaving the stripping section, and a condensation of the products of the distillation, effected in a pre-evaporation phase to concentrate at low pressure the urea solution.The modernized plant, includes at the start at least a reactor, a scrubber, a condenser, a stripper and the evaporators, includes also a passivation section, a medium pressure distillation section, and a distillation section with double-effect technique.
    Type: Grant
    Filed: December 27, 1990
    Date of Patent: January 5, 1993
    Assignees: Ammonia Casale S.A., Umberto Zardi
    Inventors: Umberto Zardi, Giorgio Pagani
  • Patent number: 5174865
    Abstract: Aqueous hydrochloric acid of very high purity can be obtained in a process for purifying crude aqueous 5 to 20 wt. % hydrochloric acid. In the purification, process water or a water/HCl mixture is evaporated from the crude aqueous hydrochloric acid at a pressure of from 0.01 to 1.0 bar and a temperature of from 10.degree. to 100.degree. C. until a crude, azeotropic mixture of water and HCl is obtained. The crude, azeotropic mixture of water and HCl is distilled in a distillation apparatus at a pressure of from 0.1 to 1.5 bar and a temperature of from 50.degree. to 110.degree. C. A purified gaseous, azeotropic mixture of water and HCl is recovered from the head of the distillation apparatus and a liquid mixture is left at the bottom of the distillation apparatus. The liquid mixture which is left at the bottom of the distillation apparatus is distilled at a pressure of from 0.5 to 2.5 bar and a temperature of from 80.degree. to 130.degree. C.
    Type: Grant
    Filed: January 25, 1991
    Date of Patent: December 29, 1992
    Assignees: Dow Deutschland Inc., The Dow Chemical Company
    Inventors: Jeff H. Stultz, Heinz Rorup, Siegfried Unger, Edmund R. Nettersheim, Bernd Wottawa
  • Patent number: 5168983
    Abstract: A process for separating cyclohexanol and other impurities from a mixture containing cyclohexanone and cyclohexanol is disclosed.
    Type: Grant
    Filed: March 22, 1991
    Date of Patent: December 8, 1992
    Assignee: Mitsubishi Kasei Corporation
    Inventors: Kazuo Tan, Kazuhiro Fujii, Michio Nakamura, Kazunao Hanada
  • Patent number: 5167775
    Abstract: The present invention provides a method for the recover of a solvent used in the production of a polyarylene sulfide according to which the deterioration of the solvent is low and the recovery rate is high, wherein a mixed liquid, mainly composed of the solvent used in the production of the polyarylene sulfide, and generated from the process of producing the polyarylene sulfide, is subjected to a flash evaporating operation to separate the mixed liquid into a flashed vapor (A) and a flashed residue (B), and then the flashed vapor is rectified (A).
    Type: Grant
    Filed: October 16, 1989
    Date of Patent: December 1, 1992
    Assignee: Idemitsu Petrochemical Co., Ltd.
    Inventors: Masao Omori, Yoshinari Koyama, Daigo Shirota
  • Patent number: 5160414
    Abstract: An extractive distillation process for separation ethers (in particular methyl t-butyl ether or ethyl t-butyl ether), aliphatic hydrocarbons (in particular isobutane and/or isobutene) and alcohols (in particular methanol or ethanol) employs as solvent sulfolane(s) and/or dialkyl sulfone(s), or N-(.beta.-mercaptoalkyl)-2-pyrrolidone(s), or a mixture of N-alkyl-2-pyrrolidone(s) and either sulfolane(s) or glycol compound(s).
    Type: Grant
    Filed: July 19, 1991
    Date of Patent: November 3, 1992
    Assignee: Phillips Petroleum Company
    Inventors: Fu-Ming Lee, Robert L. Hair, Ronald E. Brown
  • Patent number: 5158652
    Abstract: For the separation of tert. butyl ethyl ether from mixtures with ethanol, there are provided two distillation stages, the first being carried out at a pressure p.sub.1 equal to or higher than 1 bar, the second at a pressure p.sub.2 below p.sub.1 by a value .DELTA.p or 0.5 to 12 bars, p.sub.2 then being 0.5 to 10 bars. The second column distillate is partly supplied as reflux to the head of the second column and is in part recycled to the head of the first column. The purified TBEE is collected at the bottom of the first column and the purified ethanol at the bottom of the second column.This separation process can be integrated into a TBEE production unit comprising etherification by ethanol of the isobutylene contained in a C.sub.4 fraction from a catalytic cracking or steam cracking stage. The ethanol separated from the TBEE is then recycled to the etherification zone.
    Type: Grant
    Filed: April 9, 1991
    Date of Patent: October 27, 1992
    Assignee: Institut Francais du Petrole
    Inventors: Annick Pucci, Paul Mikitenko, Massimo Zuliani
  • Patent number: 5154801
    Abstract: In the diisopropyl ether production process, the distallation step for the separation of aqueous IPA recovered from the DIPE extraction operations is modified to avoid carrying out the distillation under conditions that yield IPA-water azeotrope providing lower overall process cost. The determination has been made that the overhead and bottom streams form an aqueous IPA fractionation process operated under off-azeotrope conditions in DIPE production can be recycled, respectively, to the DIPE reactor and extractor operations. Recycling the water and IPA overhead mixture eliminates the requirement for adding fresh water to the DIPE reactor. Returning the water and IPA bottom stream to the extractor reduces the requirement for distilled water addition to the extraction step. As a consequence, a less complex and costly aqueous IPA separation process is implemented.
    Type: Grant
    Filed: May 24, 1990
    Date of Patent: October 13, 1992
    Assignee: Mobil Oil Corporation
    Inventors: Mohsen N. Harandi, Hartley Owen, Frank P. Ragonese, James A. Stoos
  • Patent number: 5139620
    Abstract: Evaporation of saline water in a desalinization process, or evaporation of other types of liquid such as black liquor from paper pulp processing, is accomplished utilizing a multiple effect evaporator. Each effect includes one or more (e.g. first and second) sets of horizontally elongated dimpled plate evaporator elements. Horizontally flowing heating fluid, such as steam, is introduced to the internal passage of at least the second set in all the effects, and a head of circulation liquid is provided to cause liquid being evaporated to flow downwardly from the head over the external surfaces of the sets of dimpled plates in a thin film. The vapor evaporated is drawn through a demistor and is used as the heating fluid for the next effect. Recirculating liquid that has not evaporated and liquid separated by the demisting process are recirculated to the head associated with each effect. Clean condensate--such as distilled water--is withdrawn from the last effect.
    Type: Grant
    Filed: August 13, 1990
    Date of Patent: August 18, 1992
    Assignee: Kamyr, Inc.
    Inventors: Carl E. Elmore, Kyle Infante
  • Patent number: 5133839
    Abstract: The present invention provides an improved process for the separation of impurities from a lower alkylene oxide, such as propylene oxide, by a process wherein the impure propylene oxide is first fractionally distilled to separate higher and lower boiling impurities, then the partially purified alkylene oxide is subjected to extractive distillation to separate additional impurities, the purified propylene oxide being separated as an overhead fraction.
    Type: Grant
    Filed: July 25, 1991
    Date of Patent: July 28, 1992
    Assignee: Arco Chemical Technology, L.P.
    Inventor: T. Thomas Shih
  • Patent number: 5112441
    Abstract: A process for the recovery of heat and chemicals from spent liquor by evaporating water out from it in order to concentrate the liquor and be feeding the concentrated liquor thereby obtained and air into the soda-ash furnace. In order to increase the dry-matter content of the liquor to a level higher than usual, without at the same time increasing the viscositty of the liquor immoderately, at least the final concentrating (5, 9) of the liquor and its feeding (16) into the soda-ash furnace (4) are carried out under pressure at a temperature higher than the atmospheric boiling point of the liquor.
    Type: Grant
    Filed: August 7, 1990
    Date of Patent: May 12, 1992
    Assignee: Oy Tampella AB
    Inventors: Tuomo Ruohola, Erik Saiha, Kari Kuukkanen, Paavo Hyoty
  • Patent number: 5098525
    Abstract: The disposal of chlorinated pitches is carried out by a process which employs two treatments with an alcohol, which are carried out in cascade.Such treatments cause the precipitation of the suspended matter to take place. This is then caused to settle, and is separated and pyrolized, while the supernatant is distilled in order to separate the alcohol, which is recycled back to the process, from other organic components, which are sent to further uses.
    Type: Grant
    Filed: June 6, 1990
    Date of Patent: March 24, 1992
    Assignee: Enichem Anic, S.p.A.
    Inventors: Loreno Lorenzoni, Giuseppe Messina, Vittorio Bruzzi, Salvatore Simula
  • Patent number: 5092964
    Abstract: Butter oil is heated under high vacuum and sparged for up to about 6 hours to remove cholesterol. Walls surrounding a vapor space above the sparged mass preferably are heated to remove cholesterol with reduced loss of desirable low molecular weight components. Alternatively, the temperature of the butter oil is lowered, and the butter oil is sparged with steam for an additional period of up to about 3 hours to partially hydrolyze triglycerides to mono- and di-glycerides and free fatty acids. The low cholesterol butter oil then is cooled before being exposed to air, thus avoiding oxidation which produces off-flavors. The resulting low-cholesterol butter fat and products made therefrom have composition and organoleptic characteristics substantially similar to those of natural butter oil and butter.
    Type: Grant
    Filed: February 3, 1989
    Date of Patent: March 3, 1992
    Assignee: Campbell Soup Company
    Inventors: Joseph A. Conte, Jr., Bobby R. Johnson
  • Patent number: 5074967
    Abstract: A process for the recovery of methoxyisopropylamine from the reaction of methoxyisopropanol and ammonia under amination conditions. Water is produced as a byproduct and in the distillation separation an azeotrope is formed which includes about 14% water and 86% methoxyisopropylamine. The improvement for enhancing separation of the azeotrope includes initially distilling the mixture of methoxyisopropylamine, methoxyisopropanol and water under sufficient elevated pressure wherein an azeotrope of water and methoxyisopropylamine overhead and an essentially water free bottoms of methoxyisopropylamine and methoxyisopropanol are formed. The overhead from this initial distillation column is charged to a second distillation column operated at reduced pressure wherein an organic free bottoms containing primarily water is obtained.
    Type: Grant
    Filed: April 8, 1991
    Date of Patent: December 24, 1991
    Assignee: Air Products and Chemicals, Inc.
    Inventor: Robert L. Fowlkes
  • Patent number: 5061348
    Abstract: An apparatus and method for reprocessing waste piranha containing contaminated H.sub.2 SO.sub.4 from, for example, a semiconductor processing operation is described. The apparatus and method include a first distillation flask which is maintained under a substantial vacuum. The first distillation flask includes a first column packed with a column packing material and an input pipe for refluxing to retard loss of H.sub.2 SO.sub.4 in the first distillation. The second distillation flask boils off substantially pure H.sub.2 SO.sub.4 and provides for a continuous automatic purge of the contaminants from the second distillation flask thus improving the purity of the H.sub.2 SO.sub.4. The substantially pure H.sub.2 SO.sub.4 flows through a column which is coupled to a condenser which condenses substantially pure H.sub.2 SO.sub.4.
    Type: Grant
    Filed: February 15, 1990
    Date of Patent: October 29, 1991
    Assignee: Alameda Instruments
    Inventors: Marshall W. McCormick, Jesse C. Dobson
  • Patent number: 5035776
    Abstract: 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: Grant
    Filed: March 29, 1990
    Date of Patent: July 30, 1991
    Assignee: University of Massachusetts
    Inventor: Jeffrey P. Knapp
  • Patent number: 5031754
    Abstract: 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: Grant
    Filed: January 19, 1990
    Date of Patent: July 16, 1991
    Assignee: Krupp Koppers GmbH
    Inventors: Gerd Emmrich, Hans-Christoph Schneider, Ulrich Rudel
  • Patent number: 5030328
    Abstract: A method of separating .gamma.-butyrolactone from a mixture containing ethanol, tetrahydrofuran, water, n-butanol, 1,4-butanediol, diethyl succinate and .gamma.-butyrolactone, by distillation in vacuum columns.
    Type: Grant
    Filed: November 5, 1990
    Date of Patent: July 9, 1991
    Assignee: BASF Aktiengesellschaft
    Inventors: Rolf Fischer, Peter Stops, Erwin Brunner, Rudolf Weigand
  • Patent number: 5004829
    Abstract: (CF.sub.3 SO.sub.2).sub.2 O is formed by reaction of CF.sub.3 SO.sub.3 H with P.sub.2 O.sub.5 and taken out of the reaction system by distillation, but the residue of the distillation contains a considerable amount of unreacted CF.sub.3 SO.sub.3 H. From the residue unreacted by adding water or a phosphoric acid solution, preferably the latter, to the residue to obtain a fluidic mixture containing an adequate amount of water and subjecting the mixture to distillation, preferably under reduced pressure at temperatures ranging from 180.degree. to 280.degree. C. It is possible to form additional CF.sub.3 SO.sub.3 H during the recovery process by adding a metal salt of CF.sub.3 SO.sub.3 H to the aformentioned mixture since the metal salt is decomposed by phosphoric acid contained in the mixture.
    Type: Grant
    Filed: April 9, 1990
    Date of Patent: April 2, 1991
    Assignee: Central Glass Company, Limited
    Inventors: Minoru Aramaki, Takashi Suenaga, Hiroaki Sakaguchi, Takanori Hamana
  • Patent number: 5002639
    Abstract: A process for the separation of ortho-, meta- and para-tolunitrile from ternary mixtures of isomers entails removing ortho-tolunitrile from these mixtures by distillation under pressures of from 10.sup.2 and 10.sup.5 Pa and with a reflux ratio of from 1:1 to 200:1, and distilling the remaining binary mixture of meta- and para-tolunitrile to concentrate to more than 75 mol-% para-tolunitrile, and freezing out the paratolunitrile at below 26.degree. C., and a process for the preparation of suitable ternary mixtures of isomers entails isomerization of pure ortho-, meta- or para-tolunitrile or mixtures thereof at from 380.degree. to 580.degree. C. on zeolite catalysts.
    Type: Grant
    Filed: August 13, 1990
    Date of Patent: March 26, 1991
    Assignee: BASF Aktiengesellschaft
    Inventors: Werner Steck, Harald Rust, Helmut Lermer, Fritz Naeumann
  • Patent number: 4994152
    Abstract: Small amounts of a medium-boiling fraction are removed from a liquid mixture by distillation using a distillation column (main column) having a rectifying part and a stripping part, the liquid mixture containing relatively large amounts of lower-boiling and higher-boiling components, and the rectifying part being connected to the upper end of a second distillation column (side column) and the stripping part to the lower end of the said column, and the medium-boiling fraction being removed in vapor or liquid form from its middle section, by a process in which the concentration of the medium-boiling fraction in the liquid mixture is less than 2%, preferably less than 0.1%, and the amount of vapor passed into the lower end of the side column from the main column is 1-20%, preferably 3-10%, based on the amount of vapor in the main column at the relevant point.
    Type: Grant
    Filed: December 27, 1989
    Date of Patent: February 19, 1991
    Assignee: BASF Aktiengesellschaft
    Inventors: Gerd Kaibel, Karl Schloemer, Hans-Horst Mayer
  • Patent number: 4982034
    Abstract: A process to purify t-butylstyrene from product containing substantial amounts of t-butylethylbenzene and small amounts of alkenyl-substituted styrene impurities by a combination of vacuum fractionation and vacuum evaporation in the presence a polymerization inhibitor, and treatment with a carbonaceous adsorbent. Such a product to be purified can be prepared by catalytically, oxidatively dehydrogenating over an alkaline pyrophosphate in the vapor phase t-butylethylbenzene containing about 95 wt. % or more of the p-isomer which can be made by alkylating ethylbenzene with isobutylene in a controlled manner in the presence of cooled concentrated sulfuric acid.
    Type: Grant
    Filed: December 19, 1989
    Date of Patent: January 1, 1991
    Assignee: Amoco Corporation
    Inventors: Eric J. Moore, Marc L. Kullberg, Lori B. Lane
  • Patent number: 4980032
    Abstract: An apparatus and method for reprocessing waste piranha containing contaminated H.sub.2 SO.sub.4 from, for example, a semiconductor processing operation is described. The apparatus and method include a first distillation flask which are maintained under a substantial vacuum. The first distillation flask includes a first column with a column packing means and a reflux means to retard loss of H.sub.2 SO.sub.4 in the first distillation. The second distillation flask boils off substantially pure H.sub.2 SO.sub.4 through a column which is coupled to a condenser which condenses substantially pure H.sub.2 SO.sub.4.
    Type: Grant
    Filed: August 12, 1988
    Date of Patent: December 25, 1990
    Assignee: Alameda Instruments, Inc.
    Inventors: Jesse C. Dobson, Marshall McCormick
  • Patent number: 4978547
    Abstract: A process for producing low alcoholic wine includes the following steps: evaporating alcohol-containing wine in a vacuum evaporator so that a first mixture comprising water, alcohol and flavoring substance is separated from a second mixture having a low-alcoholic content, separating water from said first mixture in a multistage flavor substance apparatus and drawing off a third mixture comprising alcohol and flavoring substance, distilling alcohol from the third mixture, adding the water from the multistage flavor substance apparatus to a mixing vessel in an amount, which together with the low-alcohol second mixture and the flavoring substances produces a quantity of low-alcoholic wine having an alcoholic content below legally determined values for low-alcoholic wine, the process allowing only outputs of low-alcoholic wine, distilled alcohol and flavoring substances and inputs of essentially only the alcohol-containing wine.
    Type: Grant
    Filed: June 3, 1987
    Date of Patent: December 18, 1990
    Inventor: Horst Petershans
  • Patent number: 4971660
    Abstract: A method and apparatus for distilling, especially vacuum refining and deodorizing edible oils and fats utilizing sheets of oil driven downwardly in a distiller with a vacuum source at its top. A nozzle includes pressure equalization chambers, cantilever adjustment screws, and a central drag sheet to produce longer lasting and more uniform thin oil sheets to be driven in the distiller. A continuous process deaerates, dehydrates, degums, bleaches, refines, removes tocopherol, deodorizes, and strips peroxides and hydroperoxides from raw oil in a series of isothermal stages utilizing driven sheet distillers. No stripping steam is used except in the stage which strips peroxides and hydro peroxides. The method produces valuable, pure products such as tocopherol and fractionated fatty acids. It is especially efficient in heat exchange and low in waste and pollution producing products.
    Type: Grant
    Filed: October 11, 1988
    Date of Patent: November 20, 1990
    Inventor: Jacob B. Rivers, Jr.
  • Patent number: 4971661
    Abstract: An impure propylene oxide feedstock contaminated with from about 50 to about 1000 ppm of methanol and from about 0 to about 1 wt. % of acetone is charged to the lower half of an extractive distillation column containing at least about 25 theoretical plates and an extractive distillation agent consisting essentially of a blend of acetone and water (acetone/water blend) containing about 20 to about 30 wt. % of acetone and, correspondingly, about 80 to about 70 wt. % of water is charged to the tower at a point 4 to 7 theoretical stages above the impure propylene oxide feed point; the extractive distillation agent being introduced into the extractive distillation column in the ratio of said feedstock to said extractive distillation agent of from about 5:1 to about 20:1, whereby an overhead distillate fraction is obtained consisting essentially of propylene oxide contaminated with not more than about 60 ppm of methanol, not more than about 0.02 wt. % of acetone and not more than about 0.3 wt. % of water.
    Type: Grant
    Filed: October 20, 1989
    Date of Patent: November 20, 1990
    Assignee: Texaco Chemical Company
    Inventors: Robert A. Meyer, Kenneth P. Keating, William A. Smith, Robert M. Steinberg
  • Patent number: 4966276
    Abstract: An integrated continuous processes for concentrating "weak" nitric acid and concurrently reconcentrating the spent dehydrating agent used to break the nitric acid azeotrope to obtain "strong" nitric acid, the processes involving direct coupling of the nitric acid concentration with the reconcentration of the spent dehydrating agent so that less energy input is required. The major proportion of the feed "weak" nitric acid is vaporized before being fed countercurrently into a column to contact a large volume of the dehydrating agent, this vaporization being one of the two major sources of energy input, the second being through the reboiler at the bottom of the column. Energy input is balanced by energy rejection through condensation of strong nitric acid vapor and water vapor.
    Type: Grant
    Filed: April 17, 1989
    Date of Patent: October 30, 1990
    Inventor: Alfred A. Guenkel