Purification Or Recovery Patents (Class 568/856)
  • Patent number: 7605292
    Abstract: The present invention relates to a process for purifying 1,4-butynediol, which comprises compressing 1,4-butynediol to from 50 to 1500 bar, depressurizing it, waiting for phase separation to occur after depressurization and separating off the bottom phase, and a process for the hydrogenation of 1,4-butynediol to 1,4-butenediol and 1,4-butanediol using the purified 1,4-butynediol.
    Type: Grant
    Filed: January 9, 2009
    Date of Patent: October 20, 2009
    Assignee: BASF Aktiengesellschaft
    Inventors: Rudolf Erich Lorenz, Rolf Pinkos, Michael Steiniger, Gerd Schaefer, Thomas Danner
  • Patent number: 7572941
    Abstract: The present invention relates to processes for making 1,4-butanediol, 1,4-butenediol, or a mixture thereof by processing 1,4-butynediol in a dynamic mixing apparatus in an inert gas atmosphere at from 25 to 150° C. at a shear rate in the radial gap between rotor and stator of the mixing apparatus of more than 100 000 sec?1; phase separating the processed 1,4-butynediol at a temperature of from 25 to 150° C.; removing a bottom phase to obtain purified 1,4-butynediol; and reacting the purified 1,4-butynediol with hydrogen in the presence of a catalyst.
    Type: Grant
    Filed: January 27, 2009
    Date of Patent: August 11, 2009
    Assignee: BASF Aktiengesellschaft
    Inventors: Rudolf Erich Lorenz, Rolf Pinkos, Michael Steiniger, Gerd Schaefer
  • Patent number: 7538254
    Abstract: The present invention relates to a process for purifying 1,4-butynediol, which comprises compressing 1,4-butynediol to from 50 to 1500 bar, depressurizing it, waiting for phase separation to occur after depressurization and separating off the bottom phase, and a process for the hydrogenation of 1,4-butynediol to 1,4-butenediol and 1,4-butanediol using the purified 1,4-butynediol.
    Type: Grant
    Filed: August 23, 2006
    Date of Patent: May 26, 2009
    Assignee: BASF Aktiengesellschaft
    Inventors: Rudolf Erich Lorenz, Rolf Pinkos, Michael Steiniger, Gerd Schaefer, Thomas Danner
  • Patent number: 7524996
    Abstract: The present invention relates to a process for purifying 1,4-butynediol, which comprises processing 1,4-butynediol in a dynamic mixing apparatus in an inert gas atmosphere at from 25 to 150° C. at a shear rate in the radial gap between rotor and stator of the mixing apparatus of more than 100 000 sec?1, awaiting phase separation at temperatures of from 25 to 150° C. and separating off the bottom phase, and a process for the hydrogenation of 1,4-butynediol to 1,4-butenediol and 1,4-butanediol using the purified 1,4-butynediol.
    Type: Grant
    Filed: August 23, 2006
    Date of Patent: April 28, 2009
    Assignee: BASF Aktiengesellschaft
    Inventors: Rudolf Erich Lorenz, Rolf Pinkos, Michael Steiniger, Gerd Schaefer
  • Publication number: 20080242897
    Abstract: The present invention relates to a process for purifying 1,4-butynediol, which comprises processing 1,4-butynediol in a dynamic mixing apparatus in an inert gas atmosphere at from 25 to 150° C. at a shear rate in the radial gap between rotor and stator of the mixing apparatus of more than 100 000 sec?1, awaiting phase separation at temperatures of from 25 to 150° C. and separating off the bottom phase, and a process for the hydrogenation of 1,4-butynediol to 1,4-butenediol and 1,4-butanediol using the purified 1,4-butynediol.
    Type: Application
    Filed: August 23, 2006
    Publication date: October 2, 2008
    Applicant: BASF SE
    Inventors: Rudolf Erich Lorenz, Rolf Pinkos, Michael Steiniger, Gerd Schafer
  • Publication number: 20080221371
    Abstract: The present invention relates to a process for purifying 1,4-butynediol, which comprises compressing 1,4-butynediol to from 50 to 1500 bar, depressurizing it, waiting for phase separation to occur after depressurization and separating off the bottom phase, and a process for the hydrogenation of 1,4-butynediol to 1,4-butenediol and 1,4-butanediol using the purified 1,4-butynediol.
    Type: Application
    Filed: August 23, 2006
    Publication date: September 11, 2008
    Applicant: BASF SE
    Inventors: Rudolf Erich Lorenz, Rolf Pinkos, Michael Steiniger, Gerd Schafer, Thomas Danner
  • Patent number: 6956141
    Abstract: A process for preparing at least one unsaturated alcohol (B) comprises the steps (I) to (III) below: (I) reaction of at least one alkali metal hydroxide or alkaline earth metal hydroxide with at least one alcohol (A) in at least one organic solvent (L) to give a mixture (G-I) comprising at least the alcohol (A), the solvent (L) and an alkoxide (AL); (II) reaction of at least one carbonyl compound of the formula R—CO—R? with at least one alkyne of the formula R?—C?C—H and the mixture (G-I) obtained in step (I) to give a mixture (G-II) comprising at least the alcohol (A), the solvent (L) and an unsaturated alcohol (B); (III) distillation of the mixture (G-II) obtained in step (II) to give the alcohol or alcohols (B) and a mixture (G-III) comprising the solvent (L) and the alcohol (A), wherein the solvent (L) obtained in step (III) and the alcohol (A) obtained in step (III) are recycled as a mixture to step (I).
    Type: Grant
    Filed: February 22, 2000
    Date of Patent: October 18, 2005
    Assignee: BASF Aktiengesellschaft
    Inventors: Melanie Maas-Brunner, Jochem Henkelmann, Gerd Kaibel, Alois Kindler, Christian Knoll, Harald Rust, Christian Tragut, Manfred Stroezel, Udo Rheude, Rudolf Erich Lorenz, Juan Aiscar
  • Patent number: 5973213
    Abstract: Solids are separated from aqueous 1,4-butynediol solutions by passing a solids-containing aqueous butynediol solution in the downflow mode through a column and thus bringing it into contact with a solvent which has a lower density than the solids-containing butynediol solution and forms a second phase with the latter, with the solvent rising in countercurrent to the aqueous butynediol solution, the solid accumulating at the interface between the aqueous butynediol and the solvent and the solid being removed from the column by taking off a mixture of aqueous butynediol and solvent.
    Type: Grant
    Filed: January 27, 1998
    Date of Patent: October 26, 1999
    Assignee: BASF Aktiengesellschaft
    Inventors: Gerald Flood, Gerald Klossek, Wernfried Vondung, Edmund Klausmann
  • Patent number: 5874651
    Abstract: A process for increasing the amount of isolatable products in a by-product stream generated in the production of 1,6 hexanediol includes combining the by-product stream with water to form a combination of the water and the by-product stream; and reacting the combination at a temperature between about 250.degree. C. to about 400.degree. C. at a pressure from about 1,000 psig to about 3,000 psig to form one or more reaction products.
    Type: Grant
    Filed: December 23, 1996
    Date of Patent: February 23, 1999
    Assignee: BASF Corporation
    Inventors: Andrew J. McNabb, Rebecca E. Phillips
  • Patent number: 5444169
    Abstract: The conversion of formaldehyde and acetylene in the presence of a suspension catalyst to butynediol is usually performed in a cascade of reactors, wherein the separation of the catalyst from the product solution takes place per individual reactor. This can be performed by filters installed in the reactor or by suitable filter apparatuses outside the reactor. A part of the catalyst present in the reactors can be drawn off and replaced by regenerated and/or fresh catalyst. The catalyst drawn off from the reactors can advantageously be fed to a regeneration. The replacement of the catalyst in the reactor can take place discontinuously or continuously. In the reactors of the cascade, a catalyst amount of 50-200 g, preferably of 75-125 g, per liter of reaction solution is used.
    Type: Grant
    Filed: December 20, 1993
    Date of Patent: August 22, 1995
    Assignee: Linde Aktiengesellschaft
    Inventor: Frank Wiessner
  • Patent number: 4960959
    Abstract: A process for manufacturing an alkynediol is disclosed. In this process, a C.sub.3-12 ketone is reacted with acetylene in the presence of potassium hydroxide in an C.sub.1-4 alkyl-tert-butyl ether solvent. The potassium hydroxide is used in a molar ratio, relative to the amount of ketone used, of from 1.0:1.0 to 1.6:1.0.
    Type: Grant
    Filed: July 17, 1989
    Date of Patent: October 2, 1990
    Assignee: Huels Aktiengesellschaft
    Inventor: Gerhard Thelen
  • Patent number: 4954527
    Abstract: This invention relates to novel polyacetylene compositions, a process of producing the compositions and a method for inhibiting tumors utilizing the compositions. More particularly, the compositions are antitumor polyacetylenes which are derived form marine organisms, i.e., the marine sponge Cribrochalina dura.
    Type: Grant
    Filed: December 7, 1987
    Date of Patent: September 4, 1990
    Assignee: Harbor Branch Oceanographic Institution, Inc.
    Inventors: Amy E. Wright, Winnie C. Thompson, May S. Lui
  • Patent number: 4952292
    Abstract: A method of manufacturing 2,4-hexadiyne-1,6-diol by the oxidative coupling of propargyl alcohol, in the presence of an aliphatic C.sub.4 alcohol solvent is disclosed. The 2,4-hexadiyne-1,6-diol is completely dissolved in the butanol. Residual salts dissolved in the butanol solution at the end of the reaction are separated out by electrodialysis. The salt-containing stream which is separated out and contains the catalyst salts, water, and butanol is suitable as a reaction mixture, and can be recycled to the reactor.
    Type: Grant
    Filed: June 15, 1988
    Date of Patent: August 28, 1990
    Assignee: Huels Aktiengesellschaft
    Inventors: Srinivasan Sridhar, Helmut Westernacher
  • Patent number: 4933488
    Abstract: Described are triisobutylene alcohols and esters and halogenated intermediates for preparing same defined according to the generic structure: ##STR1## wherein one of the dashed lines represents a carbon-carbon single bond and the other of the dashed lines represents a carbon-carbon double bond; wherein R.sub.1 " and R.sub.2 " are the same or different and each represents hydrogen, chloro, bromo, hydroxyl or a C.sub.1 -C.sub.3 acyloxy with the provisos that when the dashed line in the 4--4' position is a carbon-carbon double bond then R.sub.1 " is hydrogen and R.sub.2 " is not hydrogen; and R.sub.1 " and R.sub.2 " are not both hydrogen.Also described are the uses of the triisobutylene alcohols and esters in augmenting or enhancing the aroma of perfume compositions, colognes and perfumed articles including but not limited to perfumed polymers solid or liquid anionic, cationic, nonionic or zwitterionic detergents, fabric softener compositions, fabric softener articles, cosmetic powders and hair preparations.
    Type: Grant
    Filed: December 26, 1989
    Date of Patent: June 12, 1990
    Assignee: International Flavors & Fragrances Inc.
    Inventors: Mark A. Sprecker, Robert P. Belko, Marie R. Hanna
  • Patent number: 4906795
    Abstract: Vitamin A containing practically no 2-cis or 6-cis isomer is prepared by hydrogenation of the aldehyde of vitamin A, optionally in the form of a complex with hydroquinone, in the presence of a ruthenium hydride catalyst.
    Type: Grant
    Filed: November 29, 1988
    Date of Patent: March 6, 1990
    Assignee: Rhone-Poulenc Sante
    Inventors: Jean-Michel Grosselin, Claude Mercier
  • Patent number: 4599467
    Abstract: A process is provided for production of vicinal alkylene glycols by hydrolysis of an epoxyalkane having from 6 to 24 carbon atoms in the presence of water and a basic catalyst and under carbon dioxide pressures of from 100 to 300 bars and temperatures of from about 200.degree. C. to 350.degree. C. Also disclosed are homogeneous mixtures of epoxyalkanes and/or vicinal alkylene glycols having from 6 to 24 carbon atoms, water, a basic catalyst and carbon dioxide in an amount corresponding to a carbon dioxide partial pressure of from about 100 to 300 bars, provided at temperatures from about 200.degree. C. to 350.degree. C. The process provides high yields, selectivities and reaction velocities and the resulting products are of high purity.
    Type: Grant
    Filed: April 10, 1985
    Date of Patent: July 8, 1986
    Assignee: AKZO NV
    Inventors: Hilde Kersten, Gerhard Meyer
  • Patent number: 4373999
    Abstract: A process permitting hazard free purification by distillation of compounds which are distillable per se but which present the risk of explosive decomposition under the effect of elevated temperatures. A desensitizing substance is added to the compounds to be distilled.Aliphatic alcohols for instance are suitable additives for alkinols.Examples are provided for the distillation of butinediol-1,4 together with the additive glycerin.
    Type: Grant
    Filed: March 30, 1982
    Date of Patent: February 15, 1983
    Assignee: GAF-Huls Chemie GmbH
    Inventors: Helmut Westernacher, Karl Aertken
  • Patent number: 4371723
    Abstract: In accordance with the present invention, there is provided herein a process for producing a distilled butanediol product of high quality in high yield. The process begins with a crude butynediol solution which is made by an ethynylation reaction between aqueous formaldehyde and acetylene. The crude butynediol solution contains at least a metallic ion, usually sodium, magnesium and/or calcium ion, and an anion, particularly, formate ion, and usually also acetate ion, and often silicic acids and silicic acid salts, as impurities, and unreacted formaldehyde. After substantially stripping the solution of the unreacted formaldehyde, the stripped solution is treated with ion exchange resin, including at least a cation exchange resin to remove one or more of the metallic ions present, and as an anion exchange resin to remove the formate ion, and the acetate ion and silicic acids and silicic acid salts, should they be present in the solution.
    Type: Grant
    Filed: August 6, 1981
    Date of Patent: February 1, 1983
    Assignee: GAF Corporation
    Inventor: Max E. Chiddix
  • Patent number: 4319055
    Abstract: A process for removing formaldehyde from aqueous solutions of but-2-yne-1,4-diol by treating the solutions with an alkaline agent at an elevated temperature in the presence of hydrogen peroxide.
    Type: Grant
    Filed: August 1, 1980
    Date of Patent: March 9, 1982
    Assignee: BASF Aktiengesellschaft
    Inventors: Walter Rebafka, Gerd Heilen, Werner Fliege
  • Patent number: 4180687
    Abstract: Formaldehyde in crude BYD, can be reacted to a polymeric substance in the presence of NaOH or Na.sub.2 CO.sub.3 at high temperatures.
    Type: Grant
    Filed: April 24, 1978
    Date of Patent: December 25, 1979
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: Harry O. Burrus, Donald I. Garnett
  • Patent number: RE32072
    Abstract: In accordance with the present invention, there is provided herein a process for producing a distilled butanediol product of high quality in high yield. The process begins with a crude butynediol solution which is made by an ethynylation reaction between aqueous formaldehyde and acetylene. The crude butynediol solution contains at least a metallic ion, usually sodium, magnesium and/or calcium ion, and an anion, particularly, formate ion, and usually also acetate ion, and often silicic acids and silicic acid salts, as impurities, and unreacted formaldehyde. After substantially stripping the solution of the unreacted formaldehyde, the stripped solution is treated with ion exchange resin, including at least a cation exchange resin to remove one or more of the metallic ions present, and as an anion exchange resin to remove the formate ion, and the acetate ion and silicic acids and silicic acid salts, should they be present in the solution.
    Type: Grant
    Filed: March 2, 1983
    Date of Patent: January 28, 1986
    Assignee: GAF Corporation
    Inventor: Max E. Chiddix