Purification Or Recovery Per Se Patents (Class 562/600)
  • Patent number: 7495129
    Abstract: The invention concerns a process for purification of an acidic monomer having a double bond, as well as a device for synthesis of an acidic monomer having a double bond, a process for producing an acidic monomer having a double bond, an acid monomer having a double bond and obtainable by this process, fibers, formed bodies, films, foams, superabsorbent polymers and other special polymers based on or containing this acidic monomer, the use of this acidic monomer in or for producing fibers, formed bodies, films, foams, superabsorbent polymers or other special polymers.
    Type: Grant
    Filed: January 13, 2004
    Date of Patent: February 24, 2009
    Assignee: Evonik Stockhausen GmbH
    Inventors: Torsten Balduf, Stefan Nordhoff, Dennis Thong Yu-Chiang, Axel Kobus, Martin Roos
  • Publication number: 20090018347
    Abstract: A process for purifying removal of acrylic acid, methacrylic acid, N-vinylpyrrolidone or p-xylene crystals from their suspension in mother liquor by means of a wash column with forced transport, whose shell of the process chamber is a metal wall, the wash column additionally being enveloped by a thermal insulation material having a water vapor barrier and a specific heat flow of >0.1 W/m2 and <10 W/m2 flowing into the process chamber through the metal wall of the wash column.
    Type: Application
    Filed: July 9, 2008
    Publication date: January 15, 2009
    Applicant: BASF SE
    Inventors: Jorg HEILEK, Ulrich Hammon, Klaus Joachim Muller-Engel, Dieter Baumann
  • Patent number: 7476299
    Abstract: A decomposition reaction apparatus or distillation apparatus for acrylic acid in which a column bottom liquid heated in a reboiler (5) is supplied from a supply port (1a) provided on a side wall of a column body (1) having: a top plate (12a) above the supply port (1a); and an impingement plate (12b) provided vertically to the top plate (12a), for preventing scattering of the column bottom liquid to a supply direction. The top plate (12a) is provided such that the top face of the top plate (12a) is inclined downward from a base end to a tip end. The present invention allows: suppression of formation of a polymerized product due to flowing of a liquid or gas heated in a reboiler into a column with a simple structure; and a stable continuous operation of column equipment over a long period of time.
    Type: Grant
    Filed: April 7, 2006
    Date of Patent: January 13, 2009
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Yasushi Ogawa, Yoshiro Suzuki, Kenji Takasaki
  • Patent number: 7473338
    Abstract: A distillation apparatus for subjecting a crude readily polymerizable compound to distillation under vacuum conditions to purify it, the distillation apparatus having a distillation column and a vacuum generator and an exhaust gas conduit of the vacuum generator connected to a connecting conduit therebetween through a pressure control valve. A method provides purifying of a readily polymerizable compound by subjecting a crude readily polymerizable compound to distillation under vacuum conditions to purify it, the method including using a distillation apparatus having a distillation column and a vacuum generator and an exhaust gas conduit of the vacuum generator connected to a connecting conduit therebetween through a pressure control valve and controlling the action of the pressure control valve based on a pressure of the distillation column.
    Type: Grant
    Filed: July 26, 2005
    Date of Patent: January 6, 2009
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Yasushi Ogawa, Yoshiro Suzuki, Kenji Takasaki, Kiyoshi Takahashi
  • Publication number: 20080287616
    Abstract: A process for production of (meth)acrylic acid is disclosed. The process includes synthesizing and distillatively working-up a crude (meth)acrylic acid phase to obtain a (meth)acrylic acid phase and a dimer phase including (meth)acrylic acid dimers and/or (meth)acrylic acid oligomers. At least a part of the (meth)acrylic acid dimers and/or of the (meth)acrylic acid oligomers from the dimer phase is split to obtain a (meth)acrylic acid including a low-boiling phase and a high-boiling phase including less (meth)acrylic acid than the low-boiling phase. At least a part of the (meth)acrylic acid from the low-boiling phase is separated by forming of one or more crystals to obtain a pure (meth)acrylic acid and a residue. Also disclosed is a device for production of (meth)acrylic acid, a process for production of a polymer as well as chemical products based on or including (meth)acrylic acid or a polymer as well as the use of (meth)acrylic acid or polymers in chemical products.
    Type: Application
    Filed: August 11, 2006
    Publication date: November 20, 2008
    Inventors: Torsten Balduf, Gunther Bub, Jurgen Mosler, Andreas Sabbagh, Jurgen Kohn, Arndt Selbach
  • Publication number: 20080281125
    Abstract: A process for preparing enantiopure E-(2S)-alkyl-5-halopent-4-enoic acids and their esters of the formula (I), in which R is a C1-C6-alkyl radical, R1 is H or C1-C4-alkyl and X is chlorine, bromine or iodine, in which the corresponding racemic 2-alkyl-5-halopent-4-enoic acid a) is reacted in a suitable solvent first with (S)-3-Methyl-2-phenylbutylamine, quinine or with N-methyl-D-glucamine, after which b) the corresponding (S)-3-Methyl-2-phenylbutylamine salt, quinine or glucamine salt of the (R)-pentenoic acid is precipitated and removed, and c) the remaining filtrate is mixed with a second chiral base or an inorganic salt, after which the corresponding salt of the (S)-pentenoic acid is precipitated and d) is then converted into the corresponding E-(2S)-alkyl-5-halo-4-pentenoic acid and subsequently where appropriate into the corresponding ester of the formula (I) in which R1 is C1-C4-alkyl.
    Type: Application
    Filed: February 22, 2006
    Publication date: November 13, 2008
    Inventors: Markus Rossler, Gerhard Steinbauer, Peter Pojarliev
  • Publication number: 20080281124
    Abstract: The present invention relates to a method for purifying (meth)acrylic acid obtained by catalytic or redox oxidation of a gaseous substrate constituting propane, propylene, acrolein, isobutane, isobutene, tert-butyl alcohol and/or (meth)acrolein or mixtures thereof by sending the gaseous reaction mixture to the bottom of a countercurrent absorption column (C1) which is supplied at the top with at least one type of hydrophobic heavy solvent, sending the flow (4) from the bottom of column (C1) to a separation column (C2). Column (C1) is operated at a flow rate of heavy solvent of from 3 to 5.6 times the flow rate of the (meth)acrylic acid in the gaseous reaction mixture and the rectifying column used as a separation column (C2) is operated with the feed at the top and without reflux.
    Type: Application
    Filed: October 1, 2004
    Publication date: November 13, 2008
    Inventors: Michel Fauconet, Denis Laurent
  • Publication number: 20080197086
    Abstract: The present invention relates to an arrangement (1) for treatment of a polymerizable material (12) comprising at least one gassing device (2) to feed a gas (11) into the polymerizable material (12) and a heating device (3) to heat the polymerizable material (12) provided with gas (11), characterized in that the heating device (3) is designed such that the polymerizable material (12) flows through the heating device (3) via an inlet (4) against gravity (9) and means for even distribution of the gas (11) over the inlet (4) are provided. The invention also relates to a process for heating of a polymerizable material, a device for production of (meth)acrylic acid and a process for production of high purity (meth)acrylic acid.
    Type: Application
    Filed: June 30, 2006
    Publication date: August 21, 2008
    Inventor: Jurgen Mosler
  • Patent number: 7414150
    Abstract: A method for purifying a crude (meth)acrylic acid obtained by a vapor phase catalytic oxidation method, characterized in that the crude (meth)acrylic acid having most parts of water and acetic acid removed therefrom, is fed to and distilled in a first distillation column of a purification system comprising first to third three distillation columns, the top fraction from the first distillation column is fed to and distilled in the second distillation column, the resulting top fraction is recovered as a high purity (meth)acrylic acid product, the bottoms from the first and second distillation columns are fed to and distilled in the third distillation column, and the resulting top fraction is fed to the first distillation column.
    Type: Grant
    Filed: April 29, 2004
    Date of Patent: August 19, 2008
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Yasushi Ogawa, Yoshiro Suzuki, Kenji Takasaki
  • Publication number: 20080183014
    Abstract: A process for preparing acrylic acid, in which an acrylic acid-comprising product gas mixture obtained by catalytic gas phase partial oxidation of a C3 precursor of acrylic acid is fractionally condensed in a condensation column provided with internals ascending into itself with side draw removal of crude acrylic acid and with liquid phase draw removal of acrylic acid-comprising acid water, and acrylic acid present in acid water is taken up into an extractant and then removed from the extractant and recycled into the condensation column, or taken up in aqueous metal hydroxide, or sent to further purification of the crude acrylic acid.
    Type: Application
    Filed: January 25, 2008
    Publication date: July 31, 2008
    Applicant: BASF SE
    Inventors: Armin DIEFENBACHER, Ulrich Hammon, Volker Schliephake, Georg Sieder
  • Patent number: 7396957
    Abstract: In the stopping and starting operations of a distillation column used for producing (meth)acrylic acids according to the present invention, upon stopping the operation of the distillation column, the heating of a reboiler attached thereto is interrupted and then the reboiler is rapidly cooled; and/or upon starting the operation of the distillation column for production of the (meth)acrylic acids, an inner wall surface of the distillation column is heated to a temperature higher than a condensation temperature of the (meth)acrylic acids and the operation of the distillation column is started under the heated condition. According to the present invention, it is possible to early and safely stop the operation of the distillation column while preventing the occurrence of polymerization within the distillation column, and stably perform an operation for distillation of acrylic monomers for a long period of time.
    Type: Grant
    Filed: April 6, 2004
    Date of Patent: July 8, 2008
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Yasushi Ogawa, Yoshiro Suzuki, Kimikatsu Jinno, Hirochika Hosaka, Kenji Takasaki, Masayasu Goriki
  • Patent number: 7393976
    Abstract: A method is provided herein for purifying (meth)acrylic acid to provide a purified (meth)acrylic acid product having a low aldehyde concentration and not more than 0.2 wt % water. One embodiment of the method includes distilling (meth)acrylic acid in the presence of an aldehyde treating compound. Another embodiment of the method includes also distilling crude (meth)acrylic acid in the presence of a reactive drying agent. (Meth)acrylic acid produced in this manner is especially suitable for use in specialty (meth)acrylic acid polymers, such as for example superabsorbent polymers, binders, and ethylene-(M)AA copolymers.
    Type: Grant
    Filed: November 1, 2004
    Date of Patent: July 1, 2008
    Assignee: Rohm and Haas Company
    Inventors: Abraham Benderly, Michael Stanley DeCourcy, Alan Sopchik
  • Patent number: 7393436
    Abstract: A thermal separating process for removing a stream containing enriched (meth)acrylic monomers from a mixture containing (meth)acrylic monomers, in which the liquid phases retained in the separating space at high temperature and high (meth)acrylic monomer content are minimized.
    Type: Grant
    Filed: July 12, 2004
    Date of Patent: July 1, 2008
    Assignee: BASF Aktiengesellschaft
    Inventors: Bernd Eck, Ulrich Hammon, Klaus Joachim Mueller-Engel, Juergen Schroeder, Joachim Thiel, Hans Martan
  • Patent number: 7381839
    Abstract: The objective of the present invention is to provide method for acrylic acid in which a generation of polymerized substance is prevented while acrylic acid is stored in a storage tank. A method of the present invention for producing acrylic acid, comprising storing acrylic acid in a storage tank, wherein a process liquid containing 50 mass % or more of acrylic acid is subjected to at least one filtering operation at 15 to 70° C. when the process liquid is supplied to the storage tank.
    Type: Grant
    Filed: January 19, 2007
    Date of Patent: June 3, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Koji Ueno, Yoshitake Ishii
  • Publication number: 20080119669
    Abstract: The invention relates the preparation of (meth)acrylic acid comprising the steps: i) bringing a composition Z1 comprising (meth)acrylic acid and aldehydes into contact with an aldehyde-trapping agent to give a composition Z2 comprising (meth)acrylic acid, the high-boiling reaction product of the aldehyde, and the aldehyde-trapping agent, and unreacted aldehyde-trapping agent; ii) separating off (meth)acrylic acid from the composition Z2 by means of distillation, whereby a composition Z3 comprising the high-boiling reaction product from the reaction between the aldehyde and the aldehyde-trapping agent and unreacted aldehyde-trapping agent is being obtained as the bottom product; iii) extracting the unreacted aldehyde-trapping agent from the composition Z3 by water, a first, aqueous phase P1 and a second, organic phase P2 being obtained; iv) separating off of the first, aqueous phase P1 from the second, organic phase P2.
    Type: Application
    Filed: February 7, 2006
    Publication date: May 22, 2008
    Inventors: Torsten Balduf, Andreas Sabbagh, Thomas Nehrkorn, Manfred Lucas
  • Publication number: 20080119668
    Abstract: A process for the preparation of (meth)acrylic acid is disclosed that includes: (a) contacting a product gas containing (meth)acrylic acid obtained from a gas phase oxidation with an aqueous phase in a quenching unit to obtain an aqueous quenched phase, (b) contacting the quenched phase with an organic separating agent in an extraction unit to give a first phase and at least one other phase, (c) crystallizing at least one of the first phase and the at least one other phase, such as by a suspension crystallization, in a crystallization unit to obtain a pure (meth)acrylic acid. Also disclosed are a device for the preparation of (meth)acrylic acid, a process for the preparation of a polymer from the (meth)acrylic acid, a device for the preparation of the polymer, a polymer obtainable by this process, and the use of the (meth)acrylic acid or the polymer in a chemical product, such as fibers or shaped articles.
    Type: Application
    Filed: September 13, 2005
    Publication date: May 22, 2008
    Inventors: Stefan Nordhoff, Axel Kobus, Torsten Balduf, Thomas Rathke, Dennis Thong Yu-Chiang, Jorg Leistner
  • Patent number: 7368601
    Abstract: In the stopping and starting operations of a distillation column used for producing (meth)acrylic acids according to the present invention, upon stopping the operation of the distillation column, the heating of a reboiler attached thereto is interrupted and then the reboiler is rapidly cooled; and/or upon starting the operation of the distillation column for production of the (meth)acrylic acids, an inner wall surface of the distillation column is heated to a temperature higher than a condensation temperature of the (meth)acrylic acids and the operation of the distillation column is started under the heated condition. According to the present invention, it is possible to early and safely stop the operation of the distillation column while preventing the occurrence of polymerization within the distillation column, and stably perform an operation for distillation of acrylic monomers for a long period of time.
    Type: Grant
    Filed: September 26, 2006
    Date of Patent: May 6, 2008
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Yasushi Ogawa, Yoshiro Suzuki, Kimikatsu Jinno, Hirochika Hosaka, Kenji Takasaki, Masayasu Goriki
  • Patent number: 7368602
    Abstract: There is provided a process for producing (meth)acrylic acid including an absorption step of bringing a (meth)acrylic acid-containing gas obtained by a gas phase catalytic oxidation method into an absorption tower and allowing the gas to contact with an absorbent, in which absorption step a crude (meth)acrylic acid solution is withdrawn from a withdrawal outlet positioned between a supply point for the (meth)acrylic acid-containing gas and a supply point for the absorbent on the absorption tower, and then supplied to a next step. The process for producing (meth)acrylic acid makes it possible to suppress the formation of Michael adducts, thereby obtaining a (meth)acrylic acid containing solution in high yield and in high concentration.
    Type: Grant
    Filed: January 19, 2007
    Date of Patent: May 6, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Toyofumi Sakai, Naoki Serata
  • Publication number: 20080097123
    Abstract: A process for separating acrylic acid and benzoic acid present in the product gas mixture of a partial oxidation to acrylic acid, in which the acrylic acid and the benzoic acid are first converted to a liquid phase, constituents having a lower boiling point than benzoic acid and acrylic acid are removed therefrom by thermal separating processes, and the acrylic acid is removed by crystallization from the remaining liquid phase.
    Type: Application
    Filed: October 17, 2007
    Publication date: April 24, 2008
    Applicant: BASFAktiengesellschaft
    Inventors: Jorg Heilek, Klaus Joachim Muller-Engel, Martin Dieterle, Armin Diefenbacher
  • Publication number: 20080091048
    Abstract: The present invention relates to a process for production of (meth)acrylic acid, whereby first a crude (meth)acrylic acid is produced and this crude (meth)acrylic acid is then continuously purified, whereby the continuous purification of the crude (meth)acrylic acid comprises the following process steps: a) in a composition comprising (meth)acrylic acid and impurities, precipitating the impurities in crystalline form from the composition; and b) separating the crystalline impurities precipitated from the composition. The invention also relates to the (meth)acrylic acid obtainable by this process, a device for production of (meth)acrylic acid, the use of the device or of a purification device for production of (meth)acrylic acid, (meth)acrylic acid, water-absorbing polymers, the use of water-absorbing polymers as well as fibers, sheets, foams and composites.
    Type: Application
    Filed: July 15, 2005
    Publication date: April 17, 2008
    Applicant: STOCKHAUSEN GMBH
    Inventors: Stefan Nordhoff, Torsten Balduf, Jurgen Mosler, Wilfired Uhlich, Dennis Thong Yu-Chiang, Axel Kobus, Arndt Selbach, Jurgen Kohn
  • Patent number: 7351396
    Abstract: A method for removing impurities from an aqueous mixture or purified aqueous by extracting the aqueous mixture or purified aqueous mixture with an extraction solvent in an extraction zone to form an extract stream and the raffinate stream; and optionally separating the extract stream and a solvent rich stream in a separation zone to form a high boiling point organic impurities stream and a recovered extraction solvent stream.
    Type: Grant
    Filed: June 5, 2003
    Date of Patent: April 1, 2008
    Assignee: Eastman Chemical Company
    Inventors: Robert Lin, Marcel de Vreede
  • Patent number: 7351310
    Abstract: A process for rectificatively separating fluids including (meth)acrylic monomers in a rectification column by directly cooling the vapor including (meth)acrylic monomers rising to the top of the rectification column to form top condensate including (meth)acrylic monomers, the condensation space at the top of the column being separated from the region of the rectification column containing the separating internals only by at least one chimney tray from which the top condensate formed is removed from the rectification column, which includes effecting the direct cooling of the vapor in the condensation space in at least two spray zones which are spatially successive and are flowed through by vapor by spraying supercooled top condensate including added polymerization inhibitor, and the temperature of the sprayed supercooled top condensate becoming lower from spray zone to spray zone in the flown direction of the vapor.
    Type: Grant
    Filed: September 10, 2003
    Date of Patent: April 1, 2008
    Assignee: BASF Aktiengesellschaft
    Inventors: Joachim Thiel, Albrecht Dams, Juergen Schroeder
  • Publication number: 20080071111
    Abstract: In a production method in which an acrylic acid-containing solution obtained from an acrylic acid-containing gas (or an acrylic acid-containing liquid obtained simply by subjecting the acrylic acid-containing solution to a separation process of reaction by-products) is directly subjected to a crystallization process, the crystallization process can't be carried out smoothly in an unsteady state (when the concentration of water in the acrylic acid-containing solution is high). The present invention aims to provide a method for collecting the purified acrylic acid having high purity in good yield even in an unsteady state. When the acrylic acid-containing solutions 18 and 16 have a concentration of water higher than 10 mass % (unsteady state), the purified acrylic acid 20 and 22 or the acrylic acid-containing solution 23 containing 10 mass % or less of water is mixed therewith to make the concentration of water 10 mass % or less [a] [b].
    Type: Application
    Filed: September 19, 2007
    Publication date: March 20, 2008
    Inventor: Satoshi Nakagawa
  • Patent number: 7342130
    Abstract: A method for producing acrylic acid, comprising (a) a absorption step of absorbing acrylic acid-containing gas obtained by oxidizing raw material gas in gas phase as crude acrylic acid-containing solution, (b1) a step of separating high boiling point components that separates the crude high boiling point components at a distillation column as (b) a step of purifying the acrylic acid-containing solution, and further, (c) a decomposition step of decomposing Michael adducts contained in the high boiling point components to prepare acrylic acid and (d) a collection step of collecting acrylic acid generated in the decomposition step (c), whereby the proportion of the amount of maleic acid to a sum of the sum of the maleic acid and maleic anhydride in the high boiling point components that are fed from the high boiling point component separation step (b1) to the decomposition step (c) satisfies a equation below: [ Equation ? ? 1 ] ? ` [ Maleic ? ? acid ? ? ( mass ) ] [
    Type: Grant
    Filed: December 6, 2006
    Date of Patent: March 11, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Fumio Shibusawa, Masaru Ishikawa
  • Patent number: 7332626
    Abstract: A method for producing acrylic acid by absorbing acrylic acid at a high ratio and obtaining an acrylic acid-containing solution of high concentration is provided. This method comprises a step of circulating part of a discharged gas from an absorption step of acrylic acid to the reactor and discarding the remainder to the out side of system while the gas is cooled before circulation to the reactor. By the method, the acrylic acid-containing solution of high concentration is obtained due to decrease of an acrylic acid loss.
    Type: Grant
    Filed: June 2, 2004
    Date of Patent: February 19, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Harunori Hirao, Kouji Ueno, Naoki Serata, Takeshi Yokogoshiya
  • Patent number: 7332624
    Abstract: A method for the production of acrylic acid comprises (i) a step for introducing a polymerization inhibitor to a stage other than a stage for supplying a raw material and a stage for supplying a reflux of said distilling column or (ii) a step for supplying the acrylic acid recovered by thermally decomposing said oligomer to said stage for dehydration. Thus, the present invention enjoys effective utilization of acrylic acid and exalts the efficiency of production.
    Type: Grant
    Filed: June 27, 2003
    Date of Patent: February 19, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Takeshi Nishimura, Yukihiro Matsumoto, Kenji Sanada, Harunori Hirao
  • Patent number: 7326811
    Abstract: A shell-and-tube type heat exchanger of the smallest possible length necessary for heat exchange is disclosed which is capable of obtaining uniform distribution of flow of a shell side fluid and substantially eliminating the structural restriction imposed on the shell side. This shell-and-tube type heat exchanger is provided with one annular conduit furnished with not less than two partitions concurrently serving as an expansion joint for introducing and discharging a shell side fluid and allowing the flow path for said shell side fluid to be separated into an introducing part and a discharging part and which comprises a place having no array of heat-transfer tubes in the flow path for said shell side fluid. It prevents the equipment from necessitating an unnecessary enlargement due to the structural restriction on the shell side and enables the shell side fluid to produce a uniform flow.
    Type: Grant
    Filed: October 20, 2006
    Date of Patent: February 5, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Tetsuji Mitsumoto, Takeshi Nishimura, Sei Nakahara, Osamu Dodo
  • Patent number: 7326323
    Abstract: Separations processes and apparati capable of purifying thermally sensitive materials at high capacity. An apparatus having a rectification section and a stripping section with the stripping section having a stripping tray with 5 to 50% open area, a pressure drop from 0.02 psi to 0.2 psi and a tray efficiency during operation of the column which is equal to or greater than 20%.
    Type: Grant
    Filed: August 25, 2005
    Date of Patent: February 5, 2008
    Assignee: Rohm and Haas Company
    Inventors: Robert Michael Mason, Jeffery Alan Goodwin, Ronald Drew Myers, Michael Stanley DeCourcy
  • Patent number: 7321060
    Abstract: A method for the production of acrylic acid of high concentration by absorbing acrylic acid with high absorption ratio of acrylic acid is provided. In a method for producing acrylic acid by a procedure comprising a step of catalytic gas phase oxidation reaction and a step of absorbing the acrylic acid-containing gas, while a low boiling substance-containing solution is introduced into the absorption column via a portion different from the top of the column.
    Type: Grant
    Filed: June 2, 2004
    Date of Patent: January 22, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Naoki Serata, Kouji Ueno, Harunori Hirao, Takeshi Yokogoshiya
  • Patent number: 7319166
    Abstract: The invention relates to a method for purifying a raw melt of at least one monomer by crystallization, wherein suspension crystallization is initially used and the resulting remaining melt or the suspension crystals that have been molten once again and separated are subjected to a mechanical separation operation before undergoing subsequent purification by crystallization.
    Type: Grant
    Filed: May 2, 2002
    Date of Patent: January 15, 2008
    Assignee: BASF Aktiengesellschaft
    Inventors: Ulrich Hammon, Bernd Eck, Dieter Baumann, Joerg Heilek, Klaus Joachim Mueller-Engel
  • Patent number: 7319167
    Abstract: A method for distilling (meth)acrylic acid and/or the ester thereof by withdrawing vapor generated in a distillation column by distillation from the top of the column, condensing the vapor to give a condensate, and circulating part of the condensate as reflux liquid into the distillation column from the top thereof, comprising the step of adding a polymerization inhibitor to said condensate and said reflux liquid. This method enables maintaining the purity and quality of (meth)acrylic acid and/or the ester thereof at a certain level or higher, suppressing generation of polymers in the rectification column and suppressing polymerization of the condensate obtained by distillation in the incident facilities of the column such as condenser, condensate tank, and the like. In addition, the method enables reduction in the amount of polymerization inhibitor used while suppressing polymerization in the intermediate distillation columns (except the final rectification column).
    Type: Grant
    Filed: May 7, 2004
    Date of Patent: January 15, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Sei Nakahara, Kazuhiko Sakamoto, Yukihiro Matsumoto
  • Patent number: 7319168
    Abstract: It is an object of the present invention to provide a process for producing aliphatic carboxylic acid, which can stabilize operation of a distillation column upon production of aliphatic carboxylic acid by reducing a water content in an aqueous aliphatic carboxylic acid solution by a distillation column, and can shorten a time during the non-steady state such as at starting up of distillation column operation.
    Type: Grant
    Filed: May 13, 2004
    Date of Patent: January 15, 2008
    Assignee: Nippon Shokubai Co., Ltd.
    Inventor: Kenji Sanada
  • Patent number: 7319169
    Abstract: The present invention relates to a method for producing (meth)acrylic acid comprising a process of recovering (meth)acrylic acid as an aqueous (meth)acrylic acid from a (meth) acrylic acid-containing gas mixture produced by the catalytic gas phase oxidation of at least one reactant selected from the group consisting of propane, propylene, isobutylene and (meth) acrolein, and a system usable for the method.
    Type: Grant
    Filed: February 18, 2005
    Date of Patent: January 15, 2008
    Assignee: LG Chem, Ltd.
    Inventors: Seong Pil Kang, Seok Hwan Choi, Kyoung Su Ha, Geon Yong Kim, Boo Gon Woo, Sang Youn Lee, Young Bae Kim, Koo Hyun Kang
  • Patent number: 7307132
    Abstract: This invention relates to a process for preparing a low-odor hydrogel-forming acrylic acid polymer, which comprises the steps of: a) preparing a polymeric hydrogel by free-radically polymerizing a monomer composition comprising at least 50% by weight of acrylic acid in an aqueous polymerization medium and converting said hydrogel into a particulate hydrogel or into hydrogel-forming powder; and optionally b) treating said particulate hydrogel or said hydrogel-forming powder with a crosslinking substance which, actually or latently, contain at least two functional groups capable of reacting with the carboxyl groups on the addition polymer; characterized by the acrylic acid used in step a) containing less than 400 ppm of acetic acid and propionic acid. It further relates to the hydrogel-forming addition polymers obtainable by the process and to their use.
    Type: Grant
    Filed: May 12, 2003
    Date of Patent: December 11, 2007
    Assignee: BASF Aktiengesellschaft
    Inventors: Gerhard Nestler, Klaus Joachim Mueller-Engel, Stefan Wickel
  • Patent number: 7307189
    Abstract: Crude acrylic acid is purified batchwise by crystallization by a process which comprises at least one purification stage and at least one stripping stage and in which at least the first stripping stage is carried out in a different crystallizer from the first purification stage.
    Type: Grant
    Filed: May 16, 2001
    Date of Patent: December 11, 2007
    Assignee: BASF Aktiengesellschaft
    Inventors: Bernd Eck, Dieter Baumann, Joerg Heilek, Klaus Joachim Mueller-Engel
  • Patent number: 7304176
    Abstract: It is an object of the present invention to provide a process for producing easily polymerizable substance, which can realize stable operation of a purification system, and can stably maintain a production amount by avoiding production stoppage, upon production of an easily polymerizable substance in plural reactors. The present invention is directed to a process for producing easily polymerizable substance, which comprises mixing easily polymerizable substances obtained in plural reactors in advance, and supplying the mixture to a purification apparatus.
    Type: Grant
    Filed: May 13, 2004
    Date of Patent: December 4, 2007
    Assignee: Nippon Shokubai Co., Ltd.
    Inventor: Takeshi Nishimura
  • Patent number: 7300555
    Abstract: A process for rectificatively separating liquids containing (meth)acrylic monomers in a rectification column is provided, in which a stream is withdrawn from the rectification column and recycled into the rectification column as a molecular oxygen-enriched liquid phase.
    Type: Grant
    Filed: November 17, 2003
    Date of Patent: November 27, 2007
    Assignee: BASF Aktiengesellschaft
    Inventor: Juergen Schroeder
  • Patent number: 7294240
    Abstract: Basic (meth)acrylates IV are prepared by transesterification of alkyl (meth)acrylates I in the presence of a catalyst and working-up of the reaction mixture by distillation, by a process in which a gas or gas mixture which is inert under the reaction conditions is passed through the reaction zone and/or heat exchanger.
    Type: Grant
    Filed: May 28, 2002
    Date of Patent: November 13, 2007
    Assignee: BASF Aktiengesellschaft
    Inventors: Matthias Geisendoerfer, Gerhard Nestler, Juergen Schroeder, Hugues Vandenmersch
  • Patent number: 7282118
    Abstract: This invention resides in providing a method for the prevention of possible polymerization of the easily polymerizable substance during the purification thereof by a column provided with (a) at least one tray directly fixed to a support ring with a bolt and a nut and/or (b) at least one tray fixed to a support ring with a vertical clamp or a distillation column provided in the lower part thereof with a splash collision plate.
    Type: Grant
    Filed: April 6, 2001
    Date of Patent: October 16, 2007
    Assignee: Nippon Shokubai Co., Ltd.
    Inventors: Tetsuji Mitsumoto, Takeshi Nishimura, Sei Nakahara, Hidefumi Haramaki
  • Patent number: 7279075
    Abstract: In a thermal separating process between at least one gaseous and at least one liquid stream, of which at least one comprises (meth)acrylic monomers, in a separating column containing sieve trays as separating internals, at least some of the sieve trays are operated above an entrainment fraction of 10% by weight.
    Type: Grant
    Filed: August 26, 2003
    Date of Patent: October 9, 2007
    Assignee: BASF Aktiengesellschaft
    Inventors: Joachim Thiel, Hugues Vandenmersch, Juergen Schroeder, Albrecht Dams
  • Patent number: 7279076
    Abstract: In an apparatus capable of distilling and refining an easily polymerizable substance, piping is performed so that when a strainer in action is switched to a backup strainer, the strainer can be switched after removing air in the backup strainer to replace air in the backup strainer with a discharge liquid of a pump. According to the apparatus, switching the strainers installed on an upstream side of the pump for extracting a liquid of a vacuum distillation column, which distills and refines the easily polymerizable substance, can be performed with no trouble during operation of the distillation column. When the apparatus includes a device for measuring a differential pressure between an upstream side and a downstream side of the strainer in action, two or more strainers installed in parallel can be switched at proper times and the easily polymerizable substance can be produced efficiently.
    Type: Grant
    Filed: March 1, 2006
    Date of Patent: October 9, 2007
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Yasushi Ogawa, Hirochika Hosaka, Yoshiro Suzuki, Mitsuo Nakamura
  • Patent number: 7279598
    Abstract: Disclosed is a process for separating and recovering 3-hydroxypropionic acid from an aqueous solution comprising 3-hydroxypropionic acid and acrylic acid, comprising counter current extracting the aqueous solution with ethyl acetate extractant. Further disclosed is a process for separating and recovering 3-hydroxypropionic acid and acrylic acid from an aqueous solution comprising 3-hydroxypropionic acid and acrylic acid.
    Type: Grant
    Filed: June 25, 2004
    Date of Patent: October 9, 2007
    Inventors: Xiangsheng Meng, Paraskevas Tsobanakis, Jeffrey Malsam, Timothy Abraham
  • Patent number: 7265241
    Abstract: A method for purifying a crude (meth)acrylic acid obtained by a vapor phase catalytic oxidation method, characterized in that the crude (meth)acrylic acid having most parts of water and acetic acid removed therefrom, is fed to and distilled in a first distillation column of a purification system comprising first to third three distillation columns, the top fraction from the first distillation column is fed to and distilled in the second distillation column, the resulting top fraction is recovered as a high purity (meth)acrylic acid product, the bottoms from the first and second distillation columns are fed to and distilled in the third distillation column, and the resulting top fraction is fed to the first distillation column.
    Type: Grant
    Filed: April 12, 2005
    Date of Patent: September 4, 2007
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Yasushi Ogawa, Yoshiro Suzuki, Kenji Takasaki
  • Patent number: 7258766
    Abstract: A method for collecting acrylic acid is provided, which includes the step of collecting acrylic acid using an aqueous medium from a reaction gas containing acrylic acid obtained by catalytic vapor-phase oxidation of propane, propylene, and/or acrolein, the step being conducted so as to satisfy the following formula (1) (B/A)<1.25 (1) wherein A represents a weight fraction of acrylic acid to all condensable ingredients in the reaction gas before collecting acrylic acid and B represents a weight fraction of acrylic acid in bottoms of a collection device used in the step of collecting. According to the method, acrylic acid can be efficiently collected from the reaction gas containing acrylic acid obtained by catalytic vapor-phase oxidation.
    Type: Grant
    Filed: April 21, 2004
    Date of Patent: August 21, 2007
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Kimikatsu Jinno, Yasushi Ogawa, Yoshiro Suzuki
  • Patent number: 7253313
    Abstract: The present invention relates to a method for purifying (meth)acrylic acid obtained by oxidizing propane, propylene, acrolein, isobutane, isobutene, ter-butyl alcohol, (meth)acrolein and mixtures thereof by sending the gaseous reaction mixture to the bottom of a countercurrent absorption column (C1) which is supplied at the top with at least one type of hydrophobic heavy solvent, sending the flow (2) from the bottom of column (C1) to a light component separation column (C2) and sending the flow from the base of column (C2), stream (4) to a separation device made up of three sections, exhaustion (S1), concentration (S2) and rectification (S3) respectively in order to extract pure (meth)acrylic acid.
    Type: Grant
    Filed: October 1, 2004
    Date of Patent: August 7, 2007
    Assignee: Arkema France
    Inventors: Michel Fauconet, Jean-Marie Destenay
  • Patent number: 7253314
    Abstract: A method for refining an easily polymerizable matter while preventing an easily polymerizable matter-containing substance from being polymerized and an apparatus for use in the method are disclosed. The method and apparatus for refining and separating the easily polymerizable matter-containing substance by the use of a distillation column provided with a heat exchanger set the linear velocity of a vapor in a connecting line intervening between the distillation column and the heat exchanger at a level of not less than 5 m per second and the retention time of the vapor at a level of not more than 3 seconds.
    Type: Grant
    Filed: August 15, 2003
    Date of Patent: August 7, 2007
    Assignee: Nippon Shokubai Co., Ltd
    Inventors: Takeshi Nishimura, Yukihiro Matsumoto
  • Publication number: 20070173666
    Abstract: The objective of the present invention is to provide methods of efficiently purifying and producing acrylic acid by removing solid acrylic acid polymers dissolving and existing in crude acrylic acid supplied to purifying process. The purifying method of the present invention comprises: filtrating the crude acrylic acid to obtain a filtrate at temperature from 15 to 70° C. and at liquid linear velocity of 5 m/s or less, wherein the crude acrylic acid contains an acrylic acid of 50% by mass or more; and purifying the acrylic acid from the filtrate. The producing method of the present invention comprises carrying out the purifying method.
    Type: Application
    Filed: January 19, 2007
    Publication date: July 26, 2007
    Inventors: Yoshitake Ishii, Koji Ueno
  • Publication number: 20070173665
    Abstract: The objective of the present invention is to provide method for acrylic acid in which a generation of polymerized substance is prevented while acrylic acid is stored in a storage tank. A method of the present invention for producing acrylic acid, comprising storing acrylic acid in a storage tank, wherein a process liquid containing 50 mass % or more of acrylic acid is subjected to at least one filtering operation at 15 to 70° C. when the process liquid is supplied to the storage tank.
    Type: Application
    Filed: January 19, 2007
    Publication date: July 26, 2007
    Inventors: Koji Ueno, Yoshitake Ishii
  • Publication number: 20070173667
    Abstract: There is provided a process for producing (meth)acrylic acid including an absorption step of bringing a (meth)acrylic acid-containing gas obtained by a gas phase catalytic oxidation method into an absorption tower and allowing the gas to contact with an absorbent, in which absorption step a crude (meth)acrylic acid solution is withdrawn from a withdrawal outlet positioned between a supply point for the (meth)acrylic acid-containing gas and a supply point for the absorbent on the absorption tower, and then supplied to a next step. The process for producing (meth)acrylic acid makes it possible to suppress the formation of Michael adducts, thereby obtaining a (meth)acrylic acid containing solution in high yield and in high concentration.
    Type: Application
    Filed: January 19, 2007
    Publication date: July 26, 2007
    Inventors: Toyofumi Sakai, Naoki Serata
  • Patent number: 7244863
    Abstract: The invention provides a process for producing and/or purifying acrylic acid or methacrylic acid or an ester of any of these, wherein mixtures of high-boiling heavy ingredients (high-boiling matter mixtures) discharged from individual step units are classified by the content therein of (meth)acrylic acid and/or of the dimer thereof and handled. According to the invention, even when high-boiling matters which have been discharged from distillation columns, high-boiling-matter cracking reactors, and the like in a plant for producing (meth)acrylic acid and/or an ester thereof and are alike in liquid nature are mixed with each other in the same tank, no polymer precipitation occurs. The handling and storage thereof are hence easy. Consequently, tanks can be united into one, and the process is extremely advantageous in reducing the construction cost and the area necessary for equipment.
    Type: Grant
    Filed: May 20, 2004
    Date of Patent: July 17, 2007
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Shuhei Yada, Yasushi Ogawa, Yoshiro Suzuki, Hirochika Hosaka