Purification Or Recovery Patents (Class 560/352)
  • Patent number: 11613518
    Abstract: A plant for preparing a purified isomeric methylene diphenyl diisocyanate monomer from a mixture of different isomeric monomers is disclosed herein. The plant can comprise a distillation apparatus, which comprises: a) a distillation column including a structured packing, b) a source for a mixture of different isomeric methylene diphenyl diisocyanate monomers, c) an evaporator, d) an overhead vapor condenser, e) optionally, an overhead vacuum system and f) a flow-controlled reflux system. The overhead vapor condenser comprises a shell and tube arrangement and is embodied so as to directly subcool the condensate to less than 47° C. The flow-controlled reflux system comprises a heater, which is embodied so as to reheat a partial stream of the condensate formed in the overhead vapor condenser up to 190° C.
    Type: Grant
    Filed: November 26, 2018
    Date of Patent: March 28, 2023
    Assignee: SULZER MANAGEMENT AG
    Inventors: Peter Faessler, Manfred Stepanski, Halbe Jansen
  • Patent number: 11358928
    Abstract: The method for producing pentamethylene diisocyanate includes a reaction step, in which carbonyl chloride is allowed to react with pentamethylenediamine to produce a reaction mixture containing pentamethylene diisocyanate and a tar component containing a chlorine-containing component; a heating step, in which the reaction mixture is heated; and a purification step, in which the reaction mixture after the heating step is purified to separate the pentamethylene diisocyanate from the tar component, wherein in the heating step, the reaction mixture is heated without removing the tar component from the reaction mixture.
    Type: Grant
    Filed: October 24, 2017
    Date of Patent: June 14, 2022
    Assignee: MITSUI CHEMICALS, INC.
    Inventors: Koji Takamatsu, Masashi Shimamoto, Tomohiro Kano
  • Patent number: 10703713
    Abstract: The industrial scale preparation of isocyanates gives rise to distillation bottom streams that are in need of further workup. These distillation bottom streams still also contain, as well as a distillation residue consisting of compounds that can be evaporated without decomposition only with great difficulty if at all (also referred to as residue for short), proportions of the desired target product (i.e. isocyanate to be prepared). The present invention relates to a process that enables recovery, in an efficient manner, of this proportion of isocyanate to be prepared in a distillation bottom stream which is obtained in the workup of the crude liquid process product which contains the isocyanate to be prepared and is formed in an isocyanate preparation process. More particularly, the present invention relates to a drying step in which the isocyanate to be prepared is recovered to form a solid material that has been largely to completely freed of this isocyanate.
    Type: Grant
    Filed: December 18, 2017
    Date of Patent: July 7, 2020
    Assignee: Covestro Deutschland AG
    Inventors: Tim Loddenkemper, Jurgen Arras, Markus Dugal
  • Patent number: 10131641
    Abstract: The invention relates to a novel method for producing polyisocyanurates comprising isocyanate groups, based on 2,4- and 2,6-toluylene diisocyanate (TDI) and to the use thereof in coating compositions.
    Type: Grant
    Filed: March 7, 2014
    Date of Patent: November 20, 2018
    Assignee: COVESTRO DEUTSCHLAND AG
    Inventors: Josef Sanders, Andreas Hecking, Reinhard Halpaap, Frank Richter, Oswald Wilmes, Jan Busch, Tim Loddenkemper, Friedhelm Steffens, Stefan Groth
  • Patent number: 9279030
    Abstract: Low-viscosity preparations of isocyanate compounds in solvents, and their use.
    Type: Grant
    Filed: January 4, 2007
    Date of Patent: March 8, 2016
    Assignee: BASF Aktiengesellschaft
    Inventors: Carl Jokisch, Horst Binder, Harald Schaefer
  • Patent number: 9090540
    Abstract: The present invention a process and apparatus for the production of methylene diphenyl diisocyanate (MDI) isomer mixtures with a low 2,2?-MDI isomer content and a high 2,4?-MDI isomer content. The resulting mixtures have an increased reactivity and are acceptable in food grade application due to the reduction in primary aromatic amines formed during the curing process. The process and apparatus also include controlling the amount of 4,4?-MDI, which is the most reactive isomer in the mixture allowing use in a wide variety of applications.
    Type: Grant
    Filed: September 20, 2011
    Date of Patent: July 28, 2015
    Assignee: Dow Global Technologies LLC
    Inventors: Andrei S. Merenov, Dennis W. Jewell, Paul A. Gillis, Gerard I. Jansma, Ashley W. Breed, John J. Anderson, Daniel J. Reed
  • Patent number: 9080005
    Abstract: The present invention includes a process and apparatus for the production of methylene diphenyl diisocyanate (MDI) isomer mixtures with a low 2,2?-MDI isomer content and a high 2,4?-MDI isomer content. The resulting mixtures have an increased reactivity and are acceptable in food grade application due to the reduction in primary aromatic amines formed during the curing process. The process and apparatus also include controlling the amount of 4,4?-MDI, which is the most reactive isomer in the mixture allowing use in a wide variety of applications.
    Type: Grant
    Filed: November 19, 2012
    Date of Patent: July 14, 2015
    Assignee: Dow Global Technologies LLC
    Inventors: Andrei S. Merenov, Gerard I. Jansma, Paul A. Gillis
  • Patent number: 9035087
    Abstract: A method for producing a polyisocyanate includes a purification step of purifying an unpurified polyisocyanate, the purification step including a tar ingredient removal step of removing tar ingredients from an unpurified polyisocyanate, and a distillation step of distilling the unpurified polyisocyanate from which tar ingredients have been removed through a dividing wall distillation column.
    Type: Grant
    Filed: November 10, 2008
    Date of Patent: May 19, 2015
    Assignee: MITSUI CHEMICALS, INC.
    Inventors: Koji Maeba, Haruhiko Noguchi, Tatsuki Kamatsuki, Masaaki Sasaki
  • Patent number: 8957245
    Abstract: The invention relates to a process for preparing an isocyanate, which involves contacting fluid streams of amine, phosgene and inert medium in at least one mixing device, such that an inert medium stream is metered at least between one amine stream and one phosgene stream within the mixing device, and then reacting an amine with phosgene in a reaction chamber to form an isocyanate. In this process the inert medium stream is metered such that a point of first contact of the amine and the phosgene occurs at a distance from a surface of the mixing device, and a turbulent flow is present in the reaction chamber.
    Type: Grant
    Filed: February 7, 2013
    Date of Patent: February 17, 2015
    Assignee: BASF SE
    Inventors: Gerhard Olbert, Torsten Mattke, Carsten Knoesche, Andreas Daiss, Jens Denecke
  • Patent number: 8901346
    Abstract: The present disclosure relates, according to some embodiments, to apparatus, systems, and/or methods for fractionating a feed mixture comprising, for example, one or more isocyanates, light components, solvents and/or heavier components. In some embodiments, fractionating an isocyanate feed mixture may comprise distilling the feed mixture in a non-adiabatic fractionating apparatus comprising a prefractionating section and/or column and a main section and/or column, which comprises a rectification section, a side section, and a stripping section. For example, isocyanates may be separated from light component(s), solvent(s) and/or heavier component(s). A fractionating apparatus may be configured and arranged, in some embodiments, as a dividing wall column. According to some embodiments of the disclosure, apparatus, systems, and/or methods may be energy efficient and/or may have a broad operating range.
    Type: Grant
    Filed: October 1, 2009
    Date of Patent: December 2, 2014
    Assignee: Dow Global Technologies LLC
    Inventors: Andrei S. Merenov, Luca Balbo, Douglas A. Stallard, John G. Pendergrast, Jr., Joerg-Peter Gehrke, Amilcar R. Collado, David D. Hibbitts
  • Patent number: 8779182
    Abstract: Process for the simultaneous and continuous production of two different mixtures of predominantly 4,4?-MDI and 2,4?-MDI in a single-step suspension melt crystallisation process whereby a mixed diisocyanate feed stream [MIx] is used to produce simultaneously two mixed diisocyanate streams [MIy] and [MIz] wherein x=80 to 92, y=97 to 99 and z=60 to 80 preferably x=82 to 88, y=97.2 to 98.5 and z=63 to 70 where x, y and z are percentages by weight of the 4,4?-MDI isomer contained in the diisocyanate isomer mixture.
    Type: Grant
    Filed: October 1, 2009
    Date of Patent: July 15, 2014
    Assignee: Huntsman International LLC
    Inventors: Johannes Lodewijk Koole, Adolf Daan Zijl, Robert Henry Carr
  • Patent number: 8759569
    Abstract: The present invention relates to a process for the production of isocyanates, preferably diisocyanates and polyisocyanates of the diphenylmethane series (MDI), by reacting an amine with phosgene in the liquid phase or in the gas phase to form the corresponding isocyanates, subsequent removal of the solvent in at least two steps to obtain at least two solvent streams, individual treatment of the at least two solvent streams, and recirculation of at least a portion of the solvent streams.
    Type: Grant
    Filed: June 16, 2010
    Date of Patent: June 24, 2014
    Assignee: BASF SE
    Inventors: Heiner Schelling, Ulrich Penzel, Eckhard Stroefer, Matthias Eiermann, Jon S. Speier, Kai Thiele, Michael Bock
  • Patent number: 8669394
    Abstract: The present invention relates to a method for decomposing and recovering an isocyanate compound, which comprises: continuously mixing and dispersing into water at high pressure and high temperature an isocyanate compound having at least one isocyanate group or group derived from an isocyanate group in a molten state or solution state, supplying a liquid mixture containing the isocyanate compound and the water at high pressure and high temperature continuously to a reactor, followed by subjecting the isocyanate compound to a decomposition reaction in the reactor, and recovering a raw material for the isocyanate compound or a derivative thereof; and an apparatus for decomposing and recovering an isocyanate compound, which comprises: a reactor which brings water at high pressure and high temperature into contact with an isocyanate compound having at least one isocyanate group or group derived from an isocyanate group to cause a decomposition reaction, a water supply line which continuously supplies the water at
    Type: Grant
    Filed: April 14, 2011
    Date of Patent: March 11, 2014
    Assignees: Kobe Steel, Ltd., Mitsui Chemicals, Inc.
    Inventors: Fumihiko Kasuya, Masahiro Yamagata, Shigetoshi Suzuki, Tadashi Yoshida
  • Patent number: 8584374
    Abstract: The invention relates to a method for removing water from a mixture containing at least one compound having at least one group reactive towards isocyanate and containing water, the mixture being applied to the surface of a rotating body A, the mixture flowing over the surface of the rotating body A to an outer region of the surface of the rotating body A and water evaporating from the mixture. In particular, this method is suitable for removing water from alcohols and amines.
    Type: Grant
    Filed: May 28, 2009
    Date of Patent: November 19, 2013
    Assignee: Construction Research & Technology GmbH
    Inventors: Simone Klapdohr, Burkhard Walther, Helmut Mack, Zhizhong Cai, Laurent Marc, Jochen Mezger, Tobias Austermann, Silke Flakus
  • Patent number: 8496834
    Abstract: Method of fractionating a mixture of polyisocyanates in the liquid phase, optionally in the presence of a suitable solvent or mixture of two or more solvents, by means of a selectively permeable membrane into a permeate stream and a retentate stream of polyisocyanate compositions different to each other and different to the original mixture.
    Type: Grant
    Filed: September 2, 2008
    Date of Patent: July 30, 2013
    Assignee: Huntsman International LLC
    Inventors: Robert Carr, Rabah Mouazer, Ivo Frans Johanna Vankelecom, Angels Cano Odena
  • Publication number: 20130157840
    Abstract: This disclosure provides a molecular sieve composition having a first and second crystalline molecular sieve, made by the method comprising: (a) providing a reaction mixture comprising at least one source of ions of tetravalent element Y, at least one source of alkali metal hydroxide, water, optionally at least one seed crystal, and optionally at least one source of ions of trivalent element X, the reaction mixture having the following molar composition: Y:X2=2 to infinity, preferably from about 2 to about 1000, OH?:Y=0.001 to 2, preferably from 0.1 to 1, M+:Y=0.001 to 2, preferably from 0.
    Type: Application
    Filed: February 18, 2013
    Publication date: June 20, 2013
    Applicant: ExxonMobil Chemical Patents Inc.
    Inventors: Wenyih Frank Lai, Robert Ellis Kay
  • Patent number: 8440856
    Abstract: This invention relates to a process for working up residues from production of isocyanates. This process involves hydrolyzing residues from production of at least one isocyanate with water to form a hydrolysis product, and processing the hydrolysis product within an extruder or a kneader having a heat transfer surface, to form a mixed product containing at least one amine and water. The amine and the water are separated from the mixed product to form an amine/water mixture, which is then separated to obtain the water and the amine. The process may also involve separating all or part of the water from the hydrolysis, or separating part of the amine from the hydrolysis, prior to the processing of the hydrolysis product.
    Type: Grant
    Filed: April 9, 2009
    Date of Patent: May 14, 2013
    Assignee: BASF SE
    Inventors: Michael Bock, Martin Sesing, Eckhard Stroefer
  • Patent number: 8273915
    Abstract: The invention provides a process for preparing polyisocyanates, comprising the steps of a) reacting amines with phosgene, b) removing hydrogen chloride, excess phosgene and, if appropriate, the solvent from the reaction mixture, c) separating the liquid mixture from step b) into a liquid phase and a gaseous phase, d) working up the gaseous phase from step c) to give the polyisocyanate.
    Type: Grant
    Filed: August 27, 2008
    Date of Patent: September 25, 2012
    Assignee: BASF SE
    Inventors: Bernd Rumpf, Michael Bock, Martin Fiene, Eckhard Stroefer
  • Patent number: 8263802
    Abstract: A process for redissociating Michael adducts which are present in a liquid F with a proportion by weight of ?10% by weight and have been formed in the preparation of acrylic acid or esters thereof in a redissociating apparatus which comprises a pump P, a separating column K with separating internals and a circulation heat exchanger UW, wherein, for the purpose of supplying the cleavage energy, the pump P sucks in bottoms liquid from the bottom space of the separating column K and, via the circulation heat exchanger UW, continually recycles it into the bottom space above the level of the bottoms liquid, and wherein the pump P is a radial circulation pump with an open impeller.
    Type: Grant
    Filed: December 9, 2009
    Date of Patent: September 11, 2012
    Assignee: BASF SE
    Inventors: Volker Schliephake, Thorsten Friese, Klaus Bott, Michael Blechschmitt, Till Blum, Klaus Joachim Mueller-Engel
  • Publication number: 20120142960
    Abstract: The invention relates to a method for purifying mixtures comprising 4,4?-methylenediphenyl diisocyanate, which comprises purifying by distillation a mixture I comprising 4,4?-methylenediphenyl diisocyanate having a hydrolyzable chlorine content as specified in ASTM D4663-10 of greater than 100 ppm by means of a column K1, wherein the gaseous stream comprising the mixture I is brought into contact in the column K1 with at least one liquid compound A which has the same or higher boiling point than 4,4?-methylenediphenyl diisocyanate and which has a hydrolyzable chlorine content as specified in ASTM D4663-10 of a maximum of 100 ppm, and wherein the gaseous stream O obtained at the top of the column comprises 4,4?-methylenediphenyl diisocyanate has a hydrolyzable chlorine content as specified in ASTM D4663-10 of a maximum of 100 ppm.
    Type: Application
    Filed: November 15, 2011
    Publication date: June 7, 2012
    Applicant: BASF SE
    Inventors: Michael BOCK, Johannes Jacobs, Kai Thiele, Anne-Kathrin Merten
  • Publication number: 20120123153
    Abstract: The invention relates to a method for purifying mixtures comprising 4,4?-methylenediphenyl diisocyanate, which comprises purifying by distillation a mixture I comprising 4,4?-methylene-diphenyl diisocyanate by means of a column K1, wherein the gaseous stream comprising the mixture I is brought into contact in the column K1 with at least one liquid compound A which has the same or higher boiling point than 4,4?-methylenediphenyl diisocyanate, and wherein the gaseous stream O obtained at the top of the column and comprising 4,4?-methylenediphenyl diisocyanate is cooled in a maximum of 5 seconds to a temperature of 20° C. to 60° C.
    Type: Application
    Filed: November 17, 2011
    Publication date: May 17, 2012
    Applicant: BASF SE
    Inventors: Michael BOCK, Kai Thiele, Gabriele Murrer
  • Patent number: 8110704
    Abstract: Stable NCO prepolymers are produced from polyisocyanates having a melting point greater than 70° C., preferably, naphthalene diisocyanate, having advantageous physical properties. An important feature of the process of the present invention is the rapid cooling of the prepolymer. The process of the present invention may be carried out on a continuous or batch basis. The prepolymers of the present invention are particularly suitable for the production of cast polyurethane elastomers.
    Type: Grant
    Filed: November 2, 2006
    Date of Patent: February 7, 2012
    Assignees: Bayer MaterialScience LLC, Bayer MaterialScince AG
    Inventors: James Michael Barnes, Hartmut Nefzger, Erika Bauer, Stefan Penninger, Thomas Schultz, Heinrich Lutz, Horst Di Mews, Charles S. Gracik
  • Patent number: 8088944
    Abstract: Isocyanates are prepared by a process in which a product stream from the isocyanate synthesis is purified.
    Type: Grant
    Filed: September 20, 2006
    Date of Patent: January 3, 2012
    Assignee: BASF SE
    Inventors: Andreas Woelfert, Hans-Juergen Pallasch, Eckhard Stroefer, Heinrich-Josef Blankertz
  • Patent number: 8063241
    Abstract: The present invention relates to a process for the preparation of toluene-diisocyanate. In this process, toluenediamine is reacted with phosgene to give crude toluene-diisocyanate, the crude toluene-diisocyanate is purified by distillation, the distillation residue formed during the distillation is hydrolysed at temperatures of less than 230° C. under absolute pressures of less than 30 bar, and the toluenediamine formed by this process is subsequently recycled into the reaction of toluenediamine and phosgene.
    Type: Grant
    Filed: September 30, 2010
    Date of Patent: November 22, 2011
    Assignee: Bayer MaterialScience AG
    Inventors: Wolfgang Lorenz, Lars Padeken, Bernd Pennemann, Friedhelm Steffens, Lothar Weismantel
  • Patent number: 8034972
    Abstract: A method for producing toluene diisocyanate is disclosed which comprises forming a dispersion comprising phosgene gas bubbles dispersed in toluene diamine liquid phase, wherein said gas bubbles have a mean diameter less than 1 micron; and subjecting the dispersion to phosgenation reaction conditions, whereby at least a portion of the toluene diamine is phosgenated to form toluene diisocyanate. A system for carrying out the phosgenation of toluene diamine is also disclosed.
    Type: Grant
    Filed: June 18, 2008
    Date of Patent: October 11, 2011
    Assignee: H R D Corporation
    Inventors: Abbas Hassan, Ebrahim Bagherzadeh, Rayford G. Anthony, Gregory Borsinger, Aziz Hassan
  • Publication number: 20110190534
    Abstract: The present invention relates to a method for decomposing and recovering an isocyanate compound, which comprises: continuously mixing and dispersing into water at high pressure and high temperature an isocyanate compound having at least one isocyanate group or group derived from an isocyanate group in a molten state or solution state, supplying a liquid mixture containing the isocyanate compound and the water at high pressure and high temperature continuously to a reactor, followed by subjecting the isocyanate compound to a decomposition reaction in the reactor, and recovering a raw material for the isocyanate compound or a derivative thereof; and an apparatus for decomposing and recovering an isocyanate compound, which comprises: a reactor which brings water at high pressure and high temperature into contact with an isocyanate compound having at least one isocyanate group or group derived from an isocyanate group to cause a decomposition reaction, a water supply line which continuously supplies the water at
    Type: Application
    Filed: April 14, 2011
    Publication date: August 4, 2011
    Applicants: Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd), Mitsui Chemicals, Inc.
    Inventors: Fumihiko Kasuya, Masahiro Yamagata, Shigetoshi Suzuki, Tadashi Yoshida
  • Patent number: 7842277
    Abstract: This disclosure relates to a crystalline MCM-22 family molecular sieve composition having, in its as-synthesized form, an X-ray diffraction pattern including a peak at d-spacing maximum of 12.33±0.23 Angstroms, a distinguishable peak at a d-spacing maximum between 12.57 to about 14.17 Angstroms and a non-discrete peak at a d-spacing maximum between 8.8 to 11. Angstroms, wherein the peak intensity of the d-spacing maximum between 12.57 to about 14.17 Angstroms is less than 90% of the peak intensity of the d-spacing maximum at 12.33±0.23 Angstroms. This disclosure also relates to methods of making the crystalline MCM-22 family molecular sieve composition.
    Type: Grant
    Filed: July 13, 2007
    Date of Patent: November 30, 2010
    Assignee: ExxonMobil Chemical Patents Inc.
    Inventors: Wieslaw J. Roth, Machteld M. Mertens, Els C. De Clerck, Ivy D. Johnson
  • Publication number: 20100249450
    Abstract: A method for producing a polyisocyanate includes a purification step of purifying an unpurified polyisocyanate, the purification step including a tar ingredient removal step of removing tar ingredients from an unpurified polyisocyanate, and a distillation step of distilling the unpurified polyisocyanate from which tar ingredients have been removed through a dividing wall distillation column.
    Type: Application
    Filed: November 10, 2008
    Publication date: September 30, 2010
    Inventors: Koji Maeba, Haruhiko Noguchi, Tatsuki Kamatsuki, Masaaki Sasaki
  • Patent number: 7649108
    Abstract: A mixture of isomeric diisocyanatodiphenylmethanes composed of at least 2,2?-diisocyanato-diphenylmethane, 2,4?-diisocyanatodiphenylmethane and 4,4?-diisocyanatodiphenyl-methane is distilled in at least one stage and a divided-wall column is used in at least one distillation stage.
    Type: Grant
    Filed: May 4, 2004
    Date of Patent: January 19, 2010
    Assignee: Bayer MaterialScience AG
    Inventors: Hans-Peter Schal, Ulrich Wolf, Bernd Thelen
  • Patent number: 7645900
    Abstract: The present invention relates to a process for the preparation of isocyanates by reacting the appropriate amines with phosgene, condensing the gas mixture thereby obtained, stripping the liquid phase thereby obtained and returning the solvent so retained in liquid form to the reaction stage. The gaseous constituents are then purified further in an absorption process.
    Type: Grant
    Filed: February 17, 2009
    Date of Patent: January 12, 2010
    Assignee: Bayer MaterialScience AG
    Inventors: Wolfgang Lorenz, Matthias Boehm, Richard Adamson, Friedhelm Steffens, Anke Hielscher
  • Patent number: 7615662
    Abstract: Isocyanates are produced by reaction of primary amines with phosgene in the gas phase. In this process, the reaction is terminated by guiding the reaction mixture from the reaction chamber through a cooling stretch into which liquids are injected. Direct cooling takes place in the cooling stretch in one stage in two or more cooling zones connected in series.
    Type: Grant
    Filed: December 11, 2007
    Date of Patent: November 10, 2009
    Assignee: Bayer MaterialScience AG
    Inventors: Fritz Pohl, Klaus Biskup, Rainer Bruns, Friedhelm Steffens, Herbert Stutz
  • Publication number: 20090275776
    Abstract: The present invention relates to a method for decomposing and recovering an isocyanate compound, which comprises: continuously mixing and dispersing into water at high pressure and high temperature an isocyanate compound having at least one isocyanate group or group derived from an isocyanate group in a molten state or solution state, supplying a liquid mixture containing the isocyanate compound and the water at high pressure and high temperature continuously to a reactor, followed by subjecting the isocyanate compound to a decomposition reaction in the reactor, and recovering a raw material for the isocyanate compound or a derivative thereof; and an apparatus for decomposing and recovering an isocyanate compound, which comprises: a reactor which brings water at high pressure and high temperature into contact with an isocyanate compound having at least one isocyanate group or group derived from an isocyanate group to cause a decomposition reaction, a water supply line which continuously supplies the water at
    Type: Application
    Filed: July 12, 2006
    Publication date: November 5, 2009
    Applicants: Kabushiki Kaisha Kobe Seiko Sho(Kobe Steel, Ltd), Mitsui chemicals Polyurethanes Inc.
    Inventors: Fumihiko Kasuya, Masahiro Yamagata, Shigetoshi Suzuki, Tadashi Yoshida
  • Patent number: 7595422
    Abstract: The invention relates to a novel process for conditioning isocyanates. The purpose of conditioning of isocyanates or of mixtures of isocyanates is to remove organophosphorus components in a suitable manner such that the organophosphorus compounds no longer interfere with processing of the isocyanates.
    Type: Grant
    Filed: December 20, 2007
    Date of Patent: September 29, 2009
    Assignee: Bayer MaterialScience AG
    Inventors: Frank Richter, Andreas Hecking, Martin Brahm
  • Patent number: 7592479
    Abstract: Isocyanates are prepared by reacting primary amines with phosgene in a reactor by a process in which a reaction discharge is present in the form of a suspension which contains the isocyanate to be prepared, as a liquid, and carbamyl chlorides as a solid, and the suspension is worked up in a film evaporator, and this process is carried out in a production plant.
    Type: Grant
    Filed: September 18, 2003
    Date of Patent: September 22, 2009
    Assignee: BASF Aktiengesellschaft
    Inventors: Eckhard Stroefer, Stephan Scholl, Martin Sohn, Andreas Woelfert, Hans-Juergen Pallasch, Jan Peter Bredehoeft
  • Publication number: 20090216042
    Abstract: A concentrating method and a concentrating system for concentrating polyisocyanate residues that that can effectively concentrate polyisocyanate residues from crude polyisocyanate comprising polyisocyanate and polyisocyanate residues in a short time and can also suppress increase in viscosity to provide stable transport of the residues and prevent blockage of the transport line, and a treating method and a treating system for decomposing the concentrated components to polyamine. The polyisocyanate residues are first heated on the boil by the distiller to be concentrated to a midterm concentrating rate, and then, the polyisocyanate residues are concentrated to the final concentrating rate by evaporation using a evaporator.
    Type: Application
    Filed: July 10, 2006
    Publication date: August 27, 2009
    Applicant: MITSUI CHEMICALS POLYURETHANES , INC.
    Inventors: Masaaki Sasaki, Tadashi Yoshida, Shigetoshi Suzuki
  • Patent number: 7544832
    Abstract: An arrangement for carrying out chemical reactions comprises at least one distillation column and/or at least one container and at least one circulation evaporator, which are connected to one another via connecting elements, liquid being taken off completely or partly from a tray or from a stacked packing bed or from a dumped packing bed or from a liquid collector of the distillation column or being fed as an external feed stream below the lower tube sheet of the circulation evaporator to said evaporator.
    Type: Grant
    Filed: February 15, 2002
    Date of Patent: June 9, 2009
    Assignee: BASF Aktiengesellschaft
    Inventors: Jan Peter Bredehöft, Hans-Jürgen Pallasch, Ludwig E. Heck, Eckhard Ströfer
  • Patent number: 7524405
    Abstract: The invention relates to a process for preparing isocyanates by reaction of amines with phosgene in the presence of inert organic solvents in a reactor and subsequent work-up of the reaction mixture leaving the reactor, wherein the solvent is separated off in a two-stage or multistage, preferably two-stage, distillation process in which the solvent is separated off at a pressure of 0.1-15 bar in a first apparatus and at 1-900 mbar in a second apparatus or further apparatuses, with the heat of condensation of the solvent vapor from the first apparatus being used for partial or complete vaporization of solvent in the second apparatus.
    Type: Grant
    Filed: December 13, 2003
    Date of Patent: April 28, 2009
    Assignee: BASF Aktiengesellschaft
    Inventors: Martin Sohn, Eckhard Stroefer, Filip Nevejans, Ulrich Penzel, Hans-Juergen Pallasch, Peter Van Den Abeel, Filip Deberdt, Jan D. Jacobs, Wolfgang Mackenroth
  • Patent number: 7504533
    Abstract: Isocyanates are produced by a) reacting at least one amine with phosgene, optionally in the presence of a solvent to produce the corresponding isocyanate and a stream containing hydrogen chloride, phosgene and optionally solvent, low-boiling compounds and inert substances is obtained, b) separating the stream containing hydrogen chloride, phosgene and optionally solvent, low-boiling compounds and inert substances in an at least two-stage sequence of absorption steps that includes (1) at least one isothermal absorption step and (2) at least one adiabatic absorption step, to obtain (i) a hydrogen chloride stream containing phosgene in concentrations of at most 0.5 wt. % (based on the weight of the hydrogen chloride stream) and (ii) a liquid phosgene stream, and c) recycling the liquid phosgene stream (ii) to the reaction of amine with phosgene.
    Type: Grant
    Filed: April 24, 2006
    Date of Patent: March 17, 2009
    Assignees: Bayer MaterialScience LLC, Bayer MaterialScience AG
    Inventors: Matthias Böhm, Wolfgang Lorenz, Bill L. Brady, Jr., Donald L. Pferdehirt
  • Patent number: 7495124
    Abstract: The present invention relates to a process for the production of MDI fractions containing 2,4?-MDI, and in which the 2,2?-MDI component from the MDA production is largely removed from the isomer mixture. Highly reactive monomeric MDI products can be produced in this way. These MDI products are characterised in their processing by significantly reduced emissions of MDI monomers.
    Type: Grant
    Filed: February 1, 2005
    Date of Patent: February 24, 2009
    Assignee: Bayer MaterialScience AG
    Inventors: Hans-Georg Pirkl, Jeffrey Bolton, Walter Meckel, Ulrich Wolf, Matthias Wintermantel, Jochen Mahrenholtz
  • Publication number: 20080262263
    Abstract: The present invention comprises a process for purifying isocyanate-comprising residues.
    Type: Application
    Filed: September 21, 2006
    Publication date: October 23, 2008
    Applicant: BASF SE
    Inventors: Andreas Wolfert, Carsten Knosche, Matthias Klotzer, Hermann Ascherl, Eckhard Stroefer, Heinrich-Josef Blankertz, Michael Schonherr, Martin Karches, Christian Benz
  • Patent number: 7358388
    Abstract: Isocyanates are prepared by a process in which a product stream from the isocyanate synthesis is purified.
    Type: Grant
    Filed: December 16, 2003
    Date of Patent: April 15, 2008
    Assignee: BASF Aktiengesellschaft
    Inventors: Andreas Woelfert, Hans-Juergen Pallasch, Eckhard Stroefer, Heinrich-Josef Blankertz
  • Patent number: 7205430
    Abstract: The invention relates to a process for the production of di- and polyisocyanates of the diphenylmethane series and mixtures thereof, in which aniline and formaldehyde are reacted in the presence of an acid catalyst to form di- and polyamines of the diphenylmethane series; the di- and polyamines of the diphenylmethane series are phosgenated, optionally in the presence of a solvent, to obtain a crude di- and polyisocyanate; from the crude di- and polyisocyanate, at least one fraction containing at least 5 wt. % 3-ring and multi-ring MDI and at least one fraction containing at least 95 wt. % 2-ring MDI are separated by distillation, and the acidities of the fraction containing at least 5 wt. % 3-ring MDI and multi-ring MDI, and/or the fraction containing at least 95 wt. % 2-ring MDI are determined analytically; and an acidic compound is added to the fraction containing at least 5 wt. % 3-ring MDI and multi-ring MDI, and/or the fraction containing at least 95 wt.
    Type: Grant
    Filed: February 1, 2005
    Date of Patent: April 17, 2007
    Assignee: Bayer MaterialScience Aktiengesellschaft
    Inventors: Ulrich Liman, Heinz-Herbert Müller, Robert Vieler, Ralf Echterhoff
  • Patent number: 7118653
    Abstract: Process for the purification of toluenediisocyanate from a crude distillation feed which includes toluenediisocyanate, an organic solvent and less than 2% by weight phosgene by separating the crude distillation feed in a dividing-wall distillation column into at least four product fractions P1–P4. P1 is a phosgene enriched low-boiler product, P2 is a solvent-enriched product, P3 is a high boiler enriched bottoms and P4 is a toluenediisocyanate product stream.
    Type: Grant
    Filed: June 9, 2003
    Date of Patent: October 10, 2006
    Assignee: Bayer Aktiengesellschaft
    Inventors: Bill Brady, Friedhelm Steffens, Berthold Keggenhoff, Kai Verkerk, Gerhard Ruffert
  • Patent number: 7108770
    Abstract: Toluene diisocyanate is recovered from a crude distillation feed containing less than 2% by weight of phosgene by (a) fractionating the crude distillation feed containing less than 2% by weight of phosgene to remove the solvent and optionally the reaction residues to produce a crude toluene diisocyanate feed containing less than 20% by weight of solvent and (b) separating the crude toluene diisocyanate feed containing less than 20% by weight of solvent in a divided-wall distillation column into four product fractions P1–P4. P1 is a vapor phase low-boiler and solvent-enriched gas stream, P2 is a low-boiler and solvent-enriched product, P3 is a high boiler-enriched bottoms product containing toluene diisocyanate and P4 is a toluene diisocyanate product stream lean in low-boilers, high-boilers and reaction residues.
    Type: Grant
    Filed: October 16, 2003
    Date of Patent: September 19, 2006
    Assignee: Bayer Aktiengesellschaft
    Inventors: Marcus Paul Grün, Bill Brady, Jr., Berthold Keggenhoff, Kai Verkerk, Hans-Peter Schal
  • Patent number: 6982026
    Abstract: Disclosed herein are methods for the recovery of at least one of an organic acid or an organic acid amide, such as a heat stable lactic acid or lactamide, from a feed stream which contains the organic acid and/or organic acid amide. The feed stream is mixed with at least one azeotroping agent. The azeotroping agent is a hydrocarbon capable of forming at least one heteroazeotrope with the organic acid or the organic acid amide in the feed stream. The mixture of the feed stream and the azeotroping agent is heated to produce a vapor stream. The heteroazeotrope is a component of that vapor stream. The vapor stream can be heated further to separate components or it can be condensed into a liquid stream. The liquid stream is capable of being separated into a first phase and a second phase. The first phase contains the highest concentration of the organic acid and/or the organic acid amide and the azeotroping agent is part of the second phase.
    Type: Grant
    Filed: March 15, 2001
    Date of Patent: January 3, 2006
    Assignee: Tate & Lyle Ingredients Americas, Inc.
    Inventors: Michael Charles Milner Cockrem, Istvan Kovacs
  • Patent number: 6966992
    Abstract: The current invention provides methods for molecule purification by RP-LC and RP-HPLC that uses unbranched terminal alkyldiols as eluting solvents. In particular, the present invention purifies molecules, particularly proteins and peptides, on reverse phase liquid chromatography columns using a buffer containing either 1,5 pentanediol, 1,6 hexanediol or 1,7 heptanediol.
    Type: Grant
    Filed: March 19, 2001
    Date of Patent: November 22, 2005
    Assignee: Akzo Nobel NV
    Inventors: Terry Allen Hauser, Kirk James Hayenga
  • Patent number: 6803483
    Abstract: A process for the purification of toluenediisocyanate by fractionating a crude distillation feed containing toluenediisocyante, an organic solvent and less than 2% by weight of phosgene in a heat integrated system having an upstream distillation column, an interchanger and a downstream distillation column which are connected in series. The vapor which is recovered from the upstream distillation column is used to reboil the bottoms product of the downstream distillation column or the feed to the downstream distillation column in the interchanger. The crude distillation feed comprising less than 2% by weight of phosgene is fractionated into three product fractions P1-P3 and optionally a fourth fraction P4. P1 is a noncondensible gas stream enriched with phosgene and/or low-boilers. P2 is a solvent-enriched product. P3 is a high boiler enriched bottoms product comprising toluenediisocyanate, and P4 is a toluenediisocyanate enriched stream lean in highboilers and reaction residues.
    Type: Grant
    Filed: June 9, 2003
    Date of Patent: October 12, 2004
    Assignee: Bayer Aktiengesellschaft
    Inventors: Heinrich Lokum, Ove Nommensen, Hermann Dallmeyer, Wilhelm Hagen
  • Patent number: 6800781
    Abstract: The present invention provides a process for quenching a gaseous reaction mixture during the phosgenation of diamines in the gas phase to produce diisocyanates. The gaseous reaction mixture contains at least a diisocyanate, phosgene and hydrogen chloride. The quenching liquid is injected into the gas mixture continuously flowing out of a cylindrical reaction zone into the downstream cylindrical quenching zone with the aid of at least two spray nozzles which are arranged at the entrance to the quenching zone at equal distances along the circumference of the quenching zone.
    Type: Grant
    Filed: September 25, 2003
    Date of Patent: October 5, 2004
    Assignee: Bayer Aktiengesellschaft
    Inventors: Heiko Herold, Herbert Stutz, Hans-Joachim Brockhaus, Volker Michele
  • Patent number: 6673960
    Abstract: A process for working up distillation residues from the synthesis of tolylene diisocyanate by reaction of the distillation residues with water comprises reacting the TDI distillation residues with water in a continuous or semicontinuous process in a backmixed reactor in the presence of hydrolysate.
    Type: Grant
    Filed: December 14, 2000
    Date of Patent: January 6, 2004
    Assignee: BASF Aktiengesellschaft
    Inventors: Hans Volkmar Schwarz, Markus Maurer, Michael Sander, Eckhard Ströfer, Rene Leuthold, Burghard Hantel, Siegfried Richter, Jörg Therre
  • Publication number: 20030233013
    Abstract: A process for the purification of toluenediisocyanate by fractionating a crude distillation feed containing toluenediisocyante, an organic solvent and less than 2% by weight of phosgene in a heat integrated system having an upstream distillation column, an interchanger and a downstream distillation column which are connected in series. The vapor which is recovered from the upstream distillation column is used to reboil the bottoms product of the downstream distillation column or the feed to the downstream distillation column in the interchanger. The crude distillation feed comprising less than 2% by weight of phosgene is fractionated into three product fractions P1-P3 and optionally a fourth fraction P4. P1 is a noncondensible gas stream enriched with phosgene and/or low-boilers. P2 is a solvent -enriched product. P3 is a high boiler enriched bottoms product comprising toluenediisocyanate, and P4 is a toluenediisocyanate enriched stream lean in highboilers and reaction residues.
    Type: Application
    Filed: June 9, 2003
    Publication date: December 18, 2003
    Inventors: Heinrich Lokum, Ove Nommensen, Hermann Dallmeyer, Wilhelm Hagen