Purification Or Recovery Patents (Class 562/124)
  • Patent number: 11254756
    Abstract: Disclosed are catalyst compositions having an internal electron donor which includes a 3,6-di-substituted-1,2-phenylene aromatic diester. Ziegler-Natta catalyst compositions containing the present catalyst compositions exhibit very high hydrogen response, high activity, high selectivity and produce propylene-based olefins with high melt flow rate.
    Type: Grant
    Filed: June 19, 2019
    Date of Patent: February 22, 2022
    Assignee: W.R. GRACE & CO.-CONN.
    Inventors: Linfeng Chen, Tak W. Leung, Tao Tao, Kuanqiang Gao
  • Patent number: 10981863
    Abstract: A method and a production system for recovering and treating taurine mother liquor, which is used for the process of ethylene oxide taurine production process. As for the treatment of the last mother liquor of taurine, add alkali firstly to the last mother liquor of taurine and then acid to form salt, or add salt directly; then concentrate and crystallize and filter, to remove lots of impurities in taurine mother liquor. This solves the problem of separating impurities, greatly shortening the time of removing impurities. The last mother liquor can also be decolorizes and additional impurities removes by activated carbon, and the removal of salt by mixing ammonia into the mother liquor to obtain the pure taurine mother liquor, thereby recovering the mother liquor and increasing the product yield.
    Type: Grant
    Filed: June 26, 2020
    Date of Patent: April 20, 2021
    Assignee: QIANJIANG YONGAN PHARMACEUTICAL CO LTD
    Inventors: Yong Chen, Xiquan Fang, Shaobo Li, Feng Liu, Xiaojun Jiang, Wei Zhou
  • Patent number: 10577312
    Abstract: A process comprising: (a) distilling a melt comprising crude alkanesulfonic acid to completely or partly remove low boilers, wherein the low boilers are drawn off at the top of a distillation column or of a one-stage evaporation apparatus and a material stream comprising alkanesulfonic acid, high boilers and residual low boilers is withdrawn at the bottom of the distillation column or of the one-stage evaporation apparatus, (b) sending the stream comprising alkanesulfonic acid, high boilers and residual low boilers into a melt crystallization as the starting melt to obtain crystals formed from the alkanesulfonic acid, hydrates of the alkanesulfonic acid or a mixture of both suspended in mother liquor, (c) performing a solid-liquid separation to remove the crystals from the mother liquor, and (d) optionally washing the crystals to remove mother liquor adhering to the crystals.
    Type: Grant
    Filed: November 8, 2016
    Date of Patent: March 3, 2020
    Assignee: BASF SE
    Inventors: Jan Spielmann, Michael Koch, Juergen Wortmann, Feelly Ruether, Sabine Weiguny, Frieder Borgmeier
  • Patent number: 9902689
    Abstract: A process for preparing alkanesulfonic acids from sulfur trioxide and an alkane, wherein sulfur trioxide, the alkane and dialkylsulfonoyi peroxide (DASP) react as components, characterized in that the following steps are performed: a) sulfur trioxide is charged in a high-pressure reactor in a condensed phase; b) a temperature of at least 25° C. is set; c) the gaseous alkane is introduced to the high-pressure reactor until a pressure of at least 10 bar is reached; d) dialkylsulfonoyi peroxide (DASP) is added; and e) after a duration of at least 5 hours, the produced alkanesulfonic acid is withdrawn.
    Type: Grant
    Filed: November 13, 2014
    Date of Patent: February 27, 2018
    Assignee: Grillo Chemie GMBH
    Inventors: Timo Ott, Ingo Biertümpel, Klaus Bunthoff, Alan Richards
  • Publication number: 20140367096
    Abstract: The invention relates to a hydrocarbon recovery composition comprising an anionic surfactant, wherein said composition is in the solid state, and to a shaped article comprising said composition. Preferably, said composition is in the form of a powder. Further, the invention relates to a process for treating a hydrocarbon containing formation comprising the steps of a) transporting said composition or shaped article to the location of the hydrocarbon containing formation; b) dissolving said composition or shaped article in water thereby forming an aqueous fluid containing the hydrocarbon recovery composition; c) providing the aqueous fluid containing the hydrocarbon recovery composition to at least a portion of the hydrocarbon containing formation; and d) allowing the hydrocarbon recovery composition to interact with the hydrocarbons in the hydrocarbon containing formation.
    Type: Application
    Filed: May 25, 2012
    Publication date: December 18, 2014
    Inventors: Julian Richard Barnes, Hendrik Dirkzwager, Robert Moene, Reinaldo Conrado Navarrete, Kirk Herbert Raney
  • Patent number: 8536372
    Abstract: Disclosed are procatalyst compositions having an internal electron donor which include a substituted phenylene aromatic diester and optionally an electron donor component. Ziegler-Natta catalyst compositions containing the present procatalyst compositions exhibit high activity and produce propylene-based olefins with broad molecular weight distribution.
    Type: Grant
    Filed: October 9, 2012
    Date of Patent: September 17, 2013
    Assignee: Dow Global Technologies LLC
    Inventors: Linfeng Chen, Tak W. Leung, Tao Tao
  • Patent number: 8426635
    Abstract: A process for preparing solid alkaline earth metal salts of secondary paraffinsulphonic acids is claimed. This process comprises converting an aqueous solution of a secondary paraffinsulphonic acid and an alkaline earth metal hydroxide into solid form by spray drying.
    Type: Grant
    Filed: March 4, 2009
    Date of Patent: April 23, 2013
    Assignee: Clariant Finance (BVI) Limited
    Inventors: Gerd Reinhardt, Peter Naumann, Georg Borchers, Mathias Groeschen
  • Patent number: 8299294
    Abstract: The subject invention provides: a method for producing vinyl sulfonic acid, comprising conducting demetallation of vinyl sulfonate salt, wherein the demetallation rate is not less than 95% according to the following formula: Demetallation rate(%)={(acid value after demetallation)/(acid value before demetallation)}×100; a method for producing vinyl sulfonic acid, comprising conducting demetallation of vinyl sulfonate salt, wherein demetallation is carried out using a strongly acidic ion exchange resin; and said method further comprising the step of purifying a product of the demetallation using a thin film evaporator.
    Type: Grant
    Filed: December 26, 2007
    Date of Patent: October 30, 2012
    Assignee: Asahi Kasei Finechem Co., Ltd.
    Inventors: Hiroshi Akikaze, Takehiko Miyai
  • Patent number: 8288585
    Abstract: Disclosed are procatalyst compositions having an internal electron donor which include a substituted phenylene aromatic diester and optionally an electron donor component. Ziegler-Natta catalyst compositions containing the present procatalyst compositions exhibit high activity and produce propylene-based olefins with broad molecular weight distribution.
    Type: Grant
    Filed: December 31, 2009
    Date of Patent: October 16, 2012
    Assignee: Dow Global Technologies LLC
    Inventors: Linfeng Chen, Tak W. Leung, Tao Tao
  • Publication number: 20110198227
    Abstract: Disclosed is a solution for an electrochemical process, the solution containing a sulfonic acid and having a low concentration of sulfur compounds, either low or high valence, that are susceptible to reduction and which is intended for use in electrodeposition, batteries, conductive polymers and descaling processes.
    Type: Application
    Filed: March 23, 2011
    Publication date: August 18, 2011
    Applicant: Arkema Inc.
    Inventors: Nicholas M. Martyak, Martin Nosowitz, Gary S. Smith, Patrick Kendall Janney, Jean-Marie Ollivier
  • Publication number: 20110017954
    Abstract: (1) A vinyl sulfonic acid, having a double bond content of 95 wt. % or more, and (i) a sodium (Na) content of 1 ppm or less, and (ii) a content of at least one metal selected from the group consisting of alkali earth metal and first row transition metal of 1 ppm or less. Alternatively, (2) a vinyl sulfonic acid, having a double bond content of 95 wt. % or more, and (i) a sodium (Na) content of 100 ppb or less, and (ii) a content of at least one metal selected from the group consisting of alkali earth metal and first row transition metal of 100 ppb or less. Further, a homopolymer or copolymer thereof, a production method thereof, or a thin-film distillation apparatus suited for the production thereof.
    Type: Application
    Filed: March 27, 2009
    Publication date: January 27, 2011
    Inventors: Hiroshi Akikaze, Takehiko Miyai, Kazuhiko Isshiki
  • Publication number: 20100197852
    Abstract: The invention provides a compound which is useful in production of a fluoropolymer and easy to be removed from the produced fluoropolymer, a method of producing the compound, and a method of producing a fluoropolymer using the compound. The invention provides a compound which is represented by Rf1—CH2O—CF2—CHF—Rf2—X, wherein Rf1 represents a fluoroalkyl group containing 1 to 5 carbon atoms, Rf2 represents a fluoroalkylene group containing 1 to 3 carbon atoms, X represents —COOM or —SO3M, and M represents one of H, K, Na, and NH4.
    Type: Application
    Filed: July 24, 2008
    Publication date: August 5, 2010
    Applicant: DAIKIN INDUSTRIES, LTD.
    Inventors: Nobuhiko Tsuda, Akinari Sugiyama
  • Publication number: 20100087674
    Abstract: The invention relates to a method for isolating concentrated paraffin sulfonic acids from reaction mixtures that are produced during the sulfoxidation of n-paraffins, from which a major part of the sulfuric acid and the paraffin was removed by phase separation and which contain, in addition to the free paraffin sulfonic acids, n-paraffins, water and optionally minor amounts of sulfuric acids. The method according to the invention is characterized by removing paraffin and optionally residual water by vacuum distillation. The paraffin sulfonic acids obtained by distillation have a content of more than 85% by weight of the active substance. The material is pale, odorless and low in sulfuric acid and paraffin.
    Type: Application
    Filed: April 29, 2008
    Publication date: April 8, 2010
    Applicant: Clariant Finance (BVI) Limited
    Inventors: Gerd Reinhardt, Peter Newmann, Lars Cuypers
  • Publication number: 20100081840
    Abstract: The subject invention provides: a method for producing vinyl sulfonic acid, comprising conducting demetallation of vinyl sulfonate salt, wherein the demetallation rate is not less than 95% according to the following formula: Demetallation rate(%)={(acid value after demetallation)/(acid value before demetallation)}×100; a method for producing vinyl sulfonic acid, comprising conducting demetallation of vinyl sulfonate salt, wherein demetallation is carried out using a strongly acidic ion exchange resin; and said method further comprising the step of purifying a product of the demetallation using a thin film evaporator.
    Type: Application
    Filed: December 26, 2007
    Publication date: April 1, 2010
    Applicant: ASAHI KASEI FINECHEM CO., LTD.
    Inventors: Hiroshi Akikaze, Takehiko Miyai
  • Patent number: 7297813
    Abstract: Methods of removing alkyl alkanesulfonate esters from aqueous or anhydrous compositions are provided. The invention provides methods for the conversion of alkyl alkanesulfonate esters of the formula RSO3R? to the corresponding acids of the formula RSO3H. The alkyl alkanesulfonate esters are present in an organic medium, which may contain significant amounts of water or which may be anhydrous or substantially anhydrous. In some embodiments, the invention provides methods for purifying aqueous or anhydrous alkanesulfonic acids by removing alkyl alkanesulfonate esters.
    Type: Grant
    Filed: August 5, 2004
    Date of Patent: November 20, 2007
    Assignee: Arkema Inc.
    Inventors: Gary Smith, Robert Cordova, Johnson C. H. Chen, Mabel Chen
  • Patent number: 6887442
    Abstract: The invention concerns a process for the continuous drying of a hydrocarbon stream and comprises contacting the hydrocarbon stream with an ionic, liquid drying agent of a salt of a fluorinated sulphonic acid.
    Type: Grant
    Filed: October 24, 2002
    Date of Patent: May 3, 2005
    Assignee: Haldor Topsoe A/S
    Inventor: Sven Ivar Hommeltoft
  • Patent number: 6864388
    Abstract: A process for preparing salts of methallylsulfonic acid in which the reaction mixture produced from the sulfonation is diluted with water and neutralized with a base.
    Type: Grant
    Filed: July 24, 2002
    Date of Patent: March 8, 2005
    Assignee: OXENO Olefinchemie GmbH
    Inventors: Claus York Werninger, Lothar Kerker, Hartmut Steinbeisser, Wilfried Bueschken, Franz-Felix Kuppinger, Peter Ernst Esser
  • Patent number: 6337421
    Abstract: In order to reduce the content of sulphuric acid in an alkanesulphonic acid, an aqueous solution of the latter is brought into contact with a basic anion-exchange resin. The invention relates more particularly to the purification of 70% methanesulphonic acid.
    Type: Grant
    Filed: July 27, 2000
    Date of Patent: January 8, 2002
    Assignee: Atofina
    Inventor: Christian Gancet
  • Publication number: 20020002301
    Abstract: Disclosed is a process for the preparation of trifluoromethanesulfonic acid anhydride by the steps of (1) forming a mixed anhydride comprising a trifluoromethanesulfonyl acyl residue and a carboxyl residue by contacting trifluoromethanesulfonic acid or a derivative thereof with a carboxyl compound selected from ketene, dialkyl ketenes, carboxylic acids, and derivatives of carboxylic acids and (2) subjecting the mixed anhydride to reactive distillation wherein the mixed anhydride undergoes disproportionation to produce triflic anhydride and a higher boiling carboxylic acid anhydride.
    Type: Application
    Filed: February 26, 2001
    Publication date: January 3, 2002
    Inventors: Robert Thomas Hembre, Robert Lin
  • Patent number: 6187169
    Abstract: A procedure for the generation of organosulfonic acids from solutions of corresponding metal organosulfonate compounds by electrowinning, electrolytically driven hydrolysis or chemically driven hydrolysis is described. Appropriate organosulfonate compounds include the water soluble salts of alkanesulfonic and aromatic sulfonic acids which incorporate metals from Group VIB, VIIB, VIIIB, IB, IIB or VA of the periodic table. The electrowinning and electrolytic techniques described can be applied in divided or undivided cells and can be operated in continuous fashion to provide the greatest efficiency. Hydrolysis based methods can employ either anodic oxidation or oxidation both of which function to oxidize the metal cation(s) present to hydrolytically unstable higher oxidation states.
    Type: Grant
    Filed: April 8, 1999
    Date of Patent: February 13, 2001
    Assignee: ATOFINA Chemicals, Inc.
    Inventors: Michael D. Gernon, Nicholas M. Martyak, Martin Nosowitz, Gary S. Smith
  • Patent number: 6156207
    Abstract: Process for the selective removal of metallic ion and/or ion ammonium impurities from water soluble acid compound comprising the steps of preparing an aqueous solution of the acid compound containing the impurities;contacting the aqueous solution with a cation exchange resin and removing selectively the metal-ion and/or ammonium ion impurities from the solution at condition being effective in the exchange of cations; andwithdrawing an aqueous solution of the acid compound being substantially free of the impurities.
    Type: Grant
    Filed: May 13, 1999
    Date of Patent: December 5, 2000
    Assignee: Haldor Topsoe A/S
    Inventors: Sven Ivar Hommeltoft, Susanna Lyng R.o slashed.en
  • Patent number: 6121486
    Abstract: A method for hydrolysis of a sulphonic acid ester in a hydrocarbon substrate by aqueous extraction of the hydrocarbon substrate, comprising steps of contacting the hydrocarbon substrate with an aqueous phase containing an ammonia salt, thereby hydrolyzing the sulphonic acid ester to the corresponding sulphonic acid; and recovering the sulphonic acid by separating the aqueous phase from the hydrocarbon substrate.
    Type: Grant
    Filed: February 24, 1999
    Date of Patent: September 19, 2000
    Assignee: Haldor Topsoe A/S
    Inventors: Sven Ivar Hommeltoft, Gitte Kobber.o slashed. Mikkelsen, John Zavilla
  • Patent number: 5873981
    Abstract: A is a process for removing water from an alkanesulfonic acid such as methanesulfonic acid or ethanesulfonic acid by mixing an azeotropic excess of a phenolic compound with water and the alkanesulfonic acid, then boiling off substantially all of the water, and leaving as a remnant substantially all the alkanesulfonic acid and some of the phenol. This process is particularly useful for recycling an alkanesulfonic acid for a reaction which requires the phenolic compound as one of the reagents. One such reaction is the alkanesulfonic acid catalyzed condensation reaction of a phenolic compound with an .alpha.haloketone to form a chlorinated intermediate of a dihydroxy-.alpha.-alkylstilbene such as 4,4'-dihydroxy-.alpha.-alkylstilbene (DHAMS).
    Type: Grant
    Filed: December 26, 1996
    Date of Patent: February 23, 1999
    Assignee: The Dow Chemical Company
    Inventors: Son T. Nguyen, Louis L. Walker, Katherine S. Clement
  • Patent number: 5731459
    Abstract: The invention relates to a process for removing amino acids and/or aminosulphonic acids from preferably aqueous solutions which contain these as impurities by adsorbing the amino acids on zeolites. Solutions to which the process according to the invention can be applied are produced, for example, from the industrial synthesis of oligopeptides in which the amino acids serving as starting materials are always present in solution, sometimes to a not inconsiderable residual concentration, together with the desired end product.
    Type: Grant
    Filed: August 28, 1996
    Date of Patent: March 24, 1998
    Assignee: Degussa Aktiengesellschaft
    Inventors: Stefan Stockhammer, Wiltrud Schafer-Treffenfeldt, Gunter Knaup, Karlheinz Drauz, Elfriede Sextl
  • Patent number: 5583253
    Abstract: A process of preparing purified alkanesulfonic acid from crude aqueous alkanesulfonic acid containing oxidizable impurities wherein the crude material is treated with a sufficient amount of chlorine to convert the oxidizable impurities to alkanesulfonyl chloride and then hydrolyzing said alkanesulfonyl chloride to alkanesulfonic acid by heating.
    Type: Grant
    Filed: March 27, 1991
    Date of Patent: December 10, 1996
    Inventors: Phyllis A. Henderson, Steven G. Schon, Carl Postuma
  • Patent number: 5525726
    Abstract: Racemic Feist's acid is treated with (R)-(+) -.alpha.-methylbenzylamine to yield (1R-trans)-3-methylene -cyclopropane-1,2-dicarboxylic acid, (R)-.alpha.-methylbenzyl-amine (1:1) salt. This salt can then be converted to (1R-trans)-3-methylene-1,2-cyclopropanedicarboxylic acid, dimethyl ester which is an intermediate in the preparation of the antiviral agent [1R-(1.alpha.,2.beta.,3.alpha.)]-2-amino-9-[2,3-bis(hydroxymethyl)cyclobut yl]-1,9-dihydro-6H-purin-6-one. The improved process also enables the recovery of racemic Feist's acid from the resolution.
    Type: Grant
    Filed: November 12, 1993
    Date of Patent: June 11, 1996
    Assignee: E. R. Squibb & Sons, Inc.
    Inventors: Jollie D. Godfrey, Jr., Richard H. Mueller, Thomas P. Kissick, Janak Singh
  • Patent number: 5498754
    Abstract: A process for refining a crude fluoroalkylsulfonic acid represented by the general formula RfSO.sub.3 H wherein Rf is a fluoroalkyl group having 1 to 4 carbon atoms into a highly refined one substantially free of impurities, said process comprising the steps of: (a) providing said crude fluoroalkylsulfonic acid, (b) mixing said crude fluoroalkylsulfonic acid with water or said water and an active silica to obtain a mixture, (c) stirring said mixture while maintaining said mixture at a higher temperature than room temperature, and (d) subjecting the mixture treated in said step (c) to distillation.
    Type: Grant
    Filed: April 18, 1994
    Date of Patent: March 12, 1996
    Assignee: Central Glass Co., Ltd.
    Inventors: Tamio Nakamura, Takashi Yokoyama, Yoshiyuki Kobayashi
  • Patent number: 5449819
    Abstract: Disclosed is a process for removing by-product phosphorus-containing (PO.sub.x) materials, alendronate and alendronate byproducts from crude mother liquors in an omega amino-1-hydroxy-C.sub.2 -C.sub.6 alkylidene-1,1-bisphosphonic acid synthesis process, e.g. alendronate sodium. Calcium chloride is added first to the crude mother liquors, then calcium oxide to precipitate the PO.sub.x materials, then neutralized to about pH 7 to complete precipitation. Substantially all of the alendronate sodium active ingredient is removed from the precipitate. Following filtration, the PO.sub.x filtercake can then be disposed of by incineration, landfilling or reclamation of usable phosphorus as fertilizer. The remaining filtrate can then be further treated in an environmentally acceptable manner by wastewater treatment or recycling to the process.
    Type: Grant
    Filed: June 6, 1994
    Date of Patent: September 12, 1995
    Assignee: Merck & Co., Inc.
    Inventors: Edamanal S. Venkataramani, Andrew L. Forman, Ralph J. Magliette, Jr., Donald McKinney
  • Patent number: 5395486
    Abstract: Dehydrated compositions are obtained by: combining a hydrous composition, e.g., a hydrous electrolyte salt, with inert fluorochemical liquid; heating the resulting mixture in a vessel to volatilize water and inert fluorochemical liquid therein until the water content of the mixture is reduced to a desired level; optionally treating the resulting dehydrated mixture with another chemical material, e.g., a polar organic solvent; and optionally subjecting the dehydrated mixture or the treated dehydrated mixture to further treatment, e.g., separation of the mixture. Liquid electrolytes suitable for use in battery applications can be prepared by this method.
    Type: Grant
    Filed: October 19, 1993
    Date of Patent: March 7, 1995
    Assignee: Minnesota Mining and Manufacturing Company
    Inventors: Michael E. Killian, John C. Stone
  • Patent number: 5312974
    Abstract: The description is of a process for the production of light-colored lower alkane sulfonic acids, especially methane sulphonic acid, by reacting the corresponding alkyl halide with alkaline halides and obtaining the free alkane sulphonic acid. In the process of the invention, the reaction is performed as a liquid/liquid reaction at temperature not exceeding 120 degrees C., and at such high pressures that even the lower alkyl halide is in the liquid phase at the reaction temperature, the aqueous reaction mixture is reduced by water content of some 50% wt. at the most, the alkaline sulphonic acid is liberated from its alkaline salt by the addition of HCl, the solid salt phase still remaining in the reaction mixture is separated out and the free alkaline sulphonic acid is obtained from the liquid phase.
    Type: Grant
    Filed: December 19, 1991
    Date of Patent: May 17, 1994
    Assignee: Henkel Kommanditgesellschaft auf Aktien
    Inventors: Willi Wuest, Rainer Eskuchen, Christoph Lohr
  • Patent number: 5248812
    Abstract: When 2-naphthylamine-1,5-disulphonic acid is precipitated from the as-sulphonated reaction mixtures by dilution, a purer product is obtained, with a low level of adherent sulphuric acid, if the precipitation by dilution of the reaction mixture is carried out under precisely defined conditions.
    Type: Grant
    Filed: September 2, 1992
    Date of Patent: September 28, 1993
    Assignee: Bayer Aktiengesellschaft
    Inventors: Horst Behre, Heinz-Ulrich Blank, Holger Heidenreich, Fritz Pohl, Paul Uhrhan
  • Patent number: 5171448
    Abstract: A process for separating and recovering paraffin sulphonic acids from mixtures with water and sulphuric acid is described, consisting of: bringing such a mixture into contact under extraction conditions with a saturated aliphatic or cycloaliphatic liquid hydrocarbon; separating an aqueous liquid phase containing sulphuric acid from an organic liquid phase consisting of the extraction solvent containing the paraffin sulphonic acids; and recovering the paraffin sulphonic acids from said organic liquid phase. The process is particularly applicable to products obtained from processes involving the sulphoxidation of paraffins with sulphur dioxide and oxygen, catalyzed by U.V. radiation.
    Type: Grant
    Filed: November 28, 1990
    Date of Patent: December 15, 1992
    Assignees: Eniricerche S.p.A., Enimont Augusta S.p.A.
    Inventors: Calogero Genova, Irena Blute, Edoardo Platone
  • Patent number: 5107019
    Abstract: The invention is concerned with an improved process for preparing paraffin-sulfonic acids containing from 10 to 20 carbon atoms, as well as their salts. The process comprises the initial reaction of sulfo-oxidation of the concerned mixture of n-paraffins, the removal of unreacted n-paraffins from the reaction mixture, the removal of the excess of SO.sub.2 from said mixture, and the removal from the reaction mixture of the therein formed sulfuric acid, with the simultaneous recovery of the end product.After the removal of SO.sub.2, to the reaction mixture hydrogen peroxide is added and the so obtained solution is submitted to one treatment selected from among the following treatments:(a) addition of an alcohol with a number of carbon atoms comprised within the range of from 4 to 8;(b) heating up to a temperature comprised within the range of from 50.degree. to 150.degree. C. and vacuum distillation under a residual pressure comprised within the range of from 5 to 500 mm.sub.
    Type: Grant
    Filed: June 7, 1990
    Date of Patent: April 21, 1992
    Assignee: Enichem Augusta S.p.A.
    Inventors: Onorio Gallistru, Artemio Gellera, Camilla Maraschin, Cosimo Franco, Giuseppe La Torre, Luciano Cavalli
  • Patent number: 5095132
    Abstract: A process for dehydrating phenol sulfonate salts by azeotropic distillation of water wherein a surfactant such as sodium dodecylbenzene sulfonate is used to prevent the salts from agglomerating and plating out on the walls of the reaction vessel.
    Type: Grant
    Filed: November 26, 1990
    Date of Patent: March 10, 1992
    Assignee: E. I. du Pont de Nemours and Company
    Inventor: Robert B. Pinkerton
  • Patent number: 5055610
    Abstract: The mixture from which sulphuric acid must be separated according to the present invention are those which derive from the sulphoxidation of (C.sub.12 -C.sub.8)-n-paraffins with SO.sub.2 and O.sub.2 in the presence of water and of U.V. light at a temperature comprised within the range of from 25 to 50.degree. C., after the removal of n-paraffins, which separate spontaneously, and of SO.sub.2 excess. In order to remove said sulphuric acid, the refined mixture, possibly diluted with water, is mixed with one or more halogenated solvents, the separation being obtained of water and sulphuric acid from the refined mixture, to the total mixture (with the two phases) a cosolvent is added, which is constituted by alcohols or ethers, with the separation being obtained of a phase constituted by H.sub.2 O and H.sub.2 SO.sub.4, which is removed. The residual organic phase, practically free from sulphuric acid, is submitted to the removal of solvents and cosolvents by means of conventional techniques.
    Type: Grant
    Filed: June 28, 1990
    Date of Patent: October 8, 1991
    Assignees: Eniricerche S.p.A., Enichem Augusta S.p.A.
    Inventors: Enrico Borgarello, Lucio Faggian, Edoardo Platone, Cosimo Franco
  • Patent number: 5047580
    Abstract: The purpose of the process of the present invention is to remove excess sulfuric acid from a mixture of paraffin-sulfonic acids free or substantially free, from paraffins.In order to remove said sulfuric acid, according to the process of the present invention, the paraffin-sulfonic acid mixture is mixed with one or more halogenated solvent(s), possibly in mixture with sulfuric acid to form a two phase mixture consisting of an organic phase containing paraffin-sulfonic acids dissolved therein and an aqueous phase substantially containing sulfuric acid. The organic phase is then treated with sulfuric acid and the organic phase and aqueous phase are then separated and the organic phase is submitted to evaporation, for the removal of the halogenated solvent(s), and with the concentrated paraffin-sulfonic acids being obtained.
    Type: Grant
    Filed: March 22, 1990
    Date of Patent: September 10, 1991
    Assignees: Eniricerche S.p.A., Enichem Augusta S.p.A.
    Inventors: Lucio Faggian, Enrico Borgarello, Cosimo Franco, Gerardo Carrillo
  • Patent number: 5028736
    Abstract: The invention relates to a process for the separation and recovery of naphthalenesulfonic acids from aqueous solutions. In this, the naphthalenesulfonic acids are adsorbed on basic ion exchangers and subsequently desorbed again, preferably with the aid of an alkaline liquor, from which the alkali metal sulfonates are then precipitated by cooling.
    Type: Grant
    Filed: May 24, 1990
    Date of Patent: July 2, 1991
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Ulrich Girrbach, Siegbert Rittner, Siegfried Bildstein, Klaus Schmiedel
  • Patent number: 4938846
    Abstract: A process for the removal of water from a lower alkanesulfonic acid-water mixture by causing the mixture to run down the internal walls of two vertical evaporator columns operated in series, is disclosed herein.
    Type: Grant
    Filed: December 8, 1986
    Date of Patent: July 3, 1990
    Assignee: Atochem, North America, Inc.
    Inventors: Perry D. Comstock, Karen M. Keys
  • Patent number: 4927962
    Abstract: A fluorocarbon carboxylic acid Rf(COOH).sub.m (Rf is C.sub.1 -C.sub.10 perfluoroalkyl group, m is 1 or 2) is prepared by the steps of hydrolyzing Rf(COF).sub.m with water to obtain an acidic solution, neutralizing the acidic solution with aqueous solution of KOH to form Rf(COOK).sub.m, precipitating and separating Rf(COOK).sub.m from the solution and converting Rf(COOK).sub.m into Rf(COOH).sub.m by acid decomposition. The content of free fluorine can extremely be reduced by treating Rf(COOK).sub.m with sulfuric acid and silica. The mother liquor is recycled after removing KF by treatment with a metal hydroxide and replenishing with KOH. In preparing a fluorocarbon sulfonic acid RfSO.sub.3 H (Rf is C.sub.1 -C.sub.3 perfluoroalkyl group) in substantially the same way, RfSO.sub.3 K is formed in aqueous solution of KOH by bringing gaseous RfSO.sub.2 F into contact with the KOH solution under normal pressure, while controlling the feed rate of RfSO.sub.
    Type: Grant
    Filed: August 29, 1988
    Date of Patent: May 22, 1990
    Assignee: Central Glass Company, Limited
    Inventors: Minoru Aramaki, Hiroaki Sakaguchi, Tamio Nakamura
  • Patent number: 4925975
    Abstract: In preparing a fluoroalkylsulfonate RfSO.sub.3 M, where Rf is a perfluoroalkyl gruop having not more than 6 carbon atoms and M is an alkali metal, by neutralization reaction between a fluoroalkylsulfonic acid RfSO.sub.3 H and an alkali metal carbonate or hydroxide, the reaction is carried out under acidic conditions such that at the end of the reaction pH of the reaction liquid is lower than 6, and preferably not higher than 3. By so maintaining the reaction liquid acidic, the obtained RfSO.sub.3 M becomes very low in the concentrations of anionic impurities such as free fluorine, free chlorine and carbonate radical and, besides becomes low in moisture absorbency.
    Type: Grant
    Filed: April 21, 1989
    Date of Patent: May 15, 1990
    Assignee: Central Glass Company, Limited
    Inventors: Minoru Aramaki, Kimitaka Okamoto, Hiroaki Sakaguchi, Tamio Nakamura
  • Patent number: 4910335
    Abstract: A method for decolorizing color contaminated alkanesulfonic or arenesulfonic acids represented by Formula I:RSO.sub.3 H Icomprises mixing the color contaminated acid with an effective amount of a dialkanesulfonyl or diarenesulfonyl peroxide represented by Formula II:R.sup.1 SO.sub.2 --O--O--O.sub.2 SR.sup.1 IIand allowing the mixture to stand at a temperature and for a period of time sufficient to allow the color of the acid to decrease to the desired level, wherein R in Formula I and R.sup.1 in Formula II may each represent an alkyl radical or an aryl radical, with the proviso that R in Formula I may be the same as or different from R.sup.1 in Formula II.
    Type: Grant
    Filed: August 1, 1989
    Date of Patent: March 20, 1990
    Assignee: Pennwalt Corporation
    Inventor: Gregory A. Wheaton
  • Patent number: 4895977
    Abstract: The removal of oxidizable organic impurities which include alkylthiolsulfonate from alkanesulfonic acids by treatment with an ozone containing gas is disclosed. The treated products have improved color and odor and exhibit improved long-term color stability.
    Type: Grant
    Filed: December 12, 1988
    Date of Patent: January 23, 1990
    Assignee: Pennwalt Corporation
    Inventor: Martin Nosowitz