Purification Or Recovery Patents (Class 568/621)
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Patent number: 10836861Abstract: A polyalkylene glycol derivative with a minimal impurity content is prepared simply by the steps of reacting a compound having formula (III-I) or (III-II) with an electrophile having formula (IV) in the presence of an optional basic compound, to form a reaction solution containing a compound having formula (V), and passing the reaction solution through a column of cation and anion exchange resins to remove water-soluble impurities, for thereby purifying the desired polyalkylene glycol derivative.Type: GrantFiled: July 23, 2018Date of Patent: November 17, 2020Assignee: SHIN-ETSU CHEMICAL CO., LTD.Inventors: Shiori Nonaka, Yuki Suka, Yuji Harada
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Patent number: 10240071Abstract: Described are aqueous adhesive dispersions comprising dispersed polyurethanes and also ethoxylated fatty alcohols as emulsifiers. The polyurethanes are constructed from certain organic diisocyanates, dihydroxy compounds selected from certain polyester diols and polyether diols, and compounds having groups reactive toward isocyanate groups and having at least one ionic group. The adhesive dispersions can be used as laminating adhesives, for example for composite film lamination or for the lamination of rigid moldings with flexible decorative foils.Type: GrantFiled: December 2, 2015Date of Patent: March 26, 2019Assignee: BASF SEInventors: Karl-Heinz Schumacher, Gemma Sanders, Kimberly Simancas, Oliver Hartz
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Patent number: 10144683Abstract: Methods include contacting a fermented gas including isoprene with a porous adsorbent and desorbing isoprene adsorbed on the porous adsorbent. The fermented gas may be obtained by culturing a microorganism having an ability to produce isoprene.Type: GrantFiled: September 28, 2015Date of Patent: December 4, 2018Assignee: Ajinomoto Co., Inc.Inventors: Hiroaki Rachi, Hiromoto Watanabe, Yosuke Nishio, Keiji Takita, Satoshi Hioki
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Patent number: 10144684Abstract: Methods include contacting a fermented gas including isoprenoid compound with a porous adsorbent and desorbing isoprenoid compound adsorbed on the porous adsorbent. The fermented gas may be obtained by culturing a microorganism having an ability to produce isoprenoid compound.Type: GrantFiled: September 28, 2015Date of Patent: December 4, 2018Assignee: Ajinomoto Co., Inc.Inventors: Hiroaki Rachi, Hiromoto Watanabe, Yosuke Nishio, Keiji Takita, Satoshi Hioki
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Patent number: 9879918Abstract: Configurations and related processing schemes of specific inter-plants and hybrid, intra- and inter-plants waste heat recovery schemes for thermal energy consumption reduction in integrated refining-petrochemical facilities synthesized for grassroots medium grade crude oil semi-conversion refineries to increase energy efficiency from specific portions of low grade waste heat sources are described. Configurations and related processing schemes of specific inter-plants and hybrid, intra- and inter-plants waste heat recovery schemes for thermal energy consumption reduction in integrated refining-petrochemical facilities synthesized for integrated medium grade crude oil semi-conversion refineries and aromatics complex for increasing energy efficiency from specific portions of low grade waste sources are also described.Type: GrantFiled: August 19, 2016Date of Patent: January 30, 2018Assignee: Saudi Arabian Oil CompanyInventors: Mahmoud Bahy Mahmoud Noureldin, Hani Mohammed Al Saed
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Patent number: 9353039Abstract: A method to provide polyether polyols comprises the steps of •providing a crude polyether polyol mixture comprising polyether polyol and a base catalyst; •neutralizing said base catalyst; •removing, in a first dehydration step, at least part of the water from the neutralized polyether polyol; •redissolving at least part of the salt crystals obtained by removal of at least part of the water; •removing, in a second dehydration step, at least part of the water from the neutralized polyether polyol mixture, thereby providing salt crystals; •removing the salt crystals from the neutralized polyether polyol, thereby providing the polyether polyol mixture.Type: GrantFiled: April 25, 2013Date of Patent: May 31, 2016Assignee: HUNTSMAN INTERNATIONAL LLCInventors: Rene Den Heeten, Paul Anton Termorshuizen
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Patent number: 9132387Abstract: The invention relates to a process for working-up a reaction mixture (5) comprising polyetherol and dissolved alkali metal comprising catalyst, wherein at least alkali metal ions of the dissolved alkali metal comprising catalyst are partially or completely removed from the mixture by a membrane separation process, the process comprising following steps: (a) feeding the reaction mixture (5) comprising polyetherol and dissolved alkali metal comprising catalyst into a first chamber (1) of a separation unit (3), (b) feeding a solvent into a second chamber (7) of the separation unit (3), the first chamber (1) and the second chamber (7) being separated by a membrane (9), (c) transporting at least the alkali metal ions of the alkali metal comprising catalyst from the first chamber (1) into the second chamber by passing through the membrane (9).Type: GrantFiled: December 12, 2012Date of Patent: September 15, 2015Assignee: BASF SEInventors: Vinit Chilekar, Hartwig Voss, Jelan Kuhn, Ann De Colvenaer, Andreas Brodhagen
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Publication number: 20150133696Abstract: A method to provide polyether polyols comprises the steps of •providing a crude polyether polyol mixture comprising polyether polyol and a base catalyst; •neutralizing said base catalyst; •removing, in a first dehydration step, at least part of the water from the neutralized polyether polyol; •redissolving at least part of the salt crystals obtained by removal of at least part of the water; •removing, in a second dehydration step, at least part of the water from the neutralized polyether polyol mixture, thereby providing salt crystals; •removing the salt crystals from the neutralized polyether polyol, thereby providing the polyether polyol mixture.Type: ApplicationFiled: April 25, 2013Publication date: May 14, 2015Inventors: René Den Heeten, Paul Anton Termorshuizen
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Patent number: 9012695Abstract: A process for neutralizing an unneutralized polyether polyol prepared using a base catalyst according to the invention comprises the steps of addition of a polyprotic acid to the unneutralized polyether polyol, the highest pKa-value of the polyprotic acid being less than 3.5, wherein, per kilogram of unneutralized polyether polyol, “A” moles of said polyprotic acid are added to the unneutralized polyether polyol, such that (n?1)*A<B<n*A, wherein ? B being the moles of protons necessary to completely neutralize a kilogram of unneutralized polyether polyol; ? n being the number of protons which said polyprotic acid can donate; removing water from said neutralized polyether polyol at a temperature between 100 deg C. and 160 deg C.Type: GrantFiled: May 18, 2010Date of Patent: April 21, 2015Assignee: Huntsman International LLCInventors: Sylvie De Mars, Joris Karel Peter Bosman
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Publication number: 20140364652Abstract: The present invention relates to a method for refining polyoxymethylene dialkyl ethers by catalytic hydrogenation using a slurry bed, wherein, using a slurry bed reactor of refining by hydrogenation, an equilibrium system of products containing polyoxymethylene dialkyl ethers is refined by catalytic hydrogenation, so as to remove formaldehyde contained therein. The refining method by hydrogenation described in the present invention is able to remarkably increase the extracting rate of polyoxymethylene dialkyl ethers, and the polyoxymethylene dialkyl ethers obtained after subsequent rectification have purity greater than 99.5%, yield greater than 97% and atom utilization ratio close to 100%.Type: ApplicationFiled: April 21, 2014Publication date: December 11, 2014Applicant: Dongfang Hongsheng New Energy Application Technology Research Institute Co., Ltd.Inventors: Zhengpeng HONG, Hongyan SHANG, Xiaoting FENG
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Publication number: 20140364653Abstract: The present invention relates to a method for refining polyoxymethylene dialkyl ethers by catalytic hydrogenation using a fixed bed, wherein, using a fixed bed reactor of refining by hydrogenation, an equilibrium system of products containing polyoxymethylene dialkyl ethers is refined by catalytic hydrogenation, so as to remove formaldehyde contained therein. The refining method by hydrogenation described in the present invention is able to remarkably increase the extracting rate of polyoxymethylene dialkyl ether products with various degrees of polymerization, and the polyoxymethylene dialkyl ethers obtained after subsequent rectification have purity greater than 99.5%, yield greater than 97% and atom utilization ratio close to 100%.Type: ApplicationFiled: April 21, 2014Publication date: December 11, 2014Applicant: Dongfang Hongsheng New Energy Application Technology Research Institute Co., Ltd.Inventors: Hongyan SHANG, Zhengpeng HONG, Yu HAN
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Patent number: 8865945Abstract: The present invention provides polyols which can be obtained by a simple process. These polyols, unless explicitly specified, are to be understood to encompass both polyether polyols and polyether ester polyols. The invention further provides the simple process for the production of the polyols, and also, the production of polyurethanes comprising reacting a polyol according to the invention with a polyisocyanate.Type: GrantFiled: August 15, 2008Date of Patent: October 21, 2014Assignee: Bayer MaterialScience AGInventors: Klaus Lorenz, Arnulf Werner, Marcus Eichmann
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Patent number: 8816132Abstract: The present invention relates to a process for accelerated preparation of polyglycerol from crude glycerol using microwave irradiation as the heat element in the presence of soap as the catalyst. The process includes the steps of (a) heating the crude glycerol that contain soap to an elevated temperature for a certain reaction time by using a microwave technology, (b) acidifying the crude polyglycerol with mineral acid at a specific temperature and centrifuging acidified crude product obtained from step (b) at a specific temperature for a certain duration of time.Type: GrantFiled: May 7, 2010Date of Patent: August 26, 2014Assignee: Malaysian Palm Oil Board (MPOB)Inventors: Hoong Seng Soi, Zailan Abu Bakar, Nik Siti Mariam Nek Mat Din, Zainab Idris, Yeong Shoot Kian, Hazimah Abu Hassan, Salmiah Ahmad
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Patent number: 8816133Abstract: Accordingly, the present invention provides a process for preparing polyglycerol from crude glycerol, wherein the crude glycerol having a glycerol content from about 60 to about 90%, soap content from about 10 to about 15% and methanol content from about 5 to about 20%, the process includes the steps of (a) heating the crude glycerol that contains soap to an elevated temperature for a certain reaction time, (b) acidifying the crude polyglycerol with mineral acid at a specific temperature and (c) centrifuging the acidified crude product obtained from step (b) at specific temperature for a certain duration of time.Type: GrantFiled: June 23, 2010Date of Patent: August 26, 2014Assignee: Malaysian Palm Oil Board (MPOB)Inventors: Seng Soi Hoong, Zailan Abu Bakar, Nik Siti Mariam Nek Mat Din, Zainab Idris, Shoot Kian Yeong, Hazimah Abu Hassan, Salmiah Ahmad
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Patent number: 8501998Abstract: A method for producing a polyoxyalkylene derivative represented by the following general formula (1): Z(OA)n-OH]m??(1) wherein Z is a residue of glycerin or diglycerin, OA is an oxyalkylene group having 2 to 4 carbon atoms, n is an average number of moles of the oxyalkylene group added and is 80 to 800, and m is 3 to 4, the method comprising steps (A), (B), (C), (D), (E), and (F) defined in the present description.Type: GrantFiled: March 31, 2010Date of Patent: August 6, 2013Assignee: NOF CorporationInventors: Satoshi Matsuo, Kazuhiro Hashimoto, Ken-ichiro Nakamoto, Chika Itoh
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Patent number: 8431672Abstract: The present invention relates to a method for manufacturing an isocyanate group-terminated prepolymer, comprising the following steps (a) to (d): (a) a step of ring-opening polymerizing an alkyleneoxide-containing cyclic compound by using an initiator in the presence of a composite metal cyanide complex catalyst, thereby obtaining a polyol composition containing the catalyst; (b) a step of, without removal of the composite metal cyanide complex catalyst from the polyol composition obtained in the step (a), adding water and performing a heat treatment in a closed system; (c) a step of subjecting the hydrous polyol composition after the step (b) to a dehydration treatment; and (d) a step of adding a polyisocyanate compound to the polyol composition after the step (c) and subjecting to a reaction with the polyol in the polyol composition.Type: GrantFiled: March 30, 2012Date of Patent: April 30, 2013Assignee: Asahi Glass Company, LimitedInventors: Chitoshi Suzuki, Takeaki Arai, Yukio Matsumoto
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Patent number: 8362304Abstract: Glycol ether compositions useful for metal recovery by froth flotation and processes for making the compositions are disclosed. In one process, dipropylene glycol methyl ether (DPM) is propoxylated to give a composition comprising 4 to 15 wt. % of DPM and at least 20 wt. % of tripropylene glycol methyl ether (TPM). In another process, the glycol ether composition is made from a distillation residue which comprises DPM, TPM, and a basic catalyst. Extraction of the residue with water to remove some of the basic catalyst is followed by propoxylated to give a composition which comprises less than 15 wt. % of DPM, at least 20 wt. % of TPM, and one or more PO-based glycols. In comparative froth tests, glycol ether compositions of the invention meet or exceed the performance of commercial frothers.Type: GrantFiled: July 15, 2009Date of Patent: January 29, 2013Assignee: Lyondell Chemical Technology, L.P.Inventors: Farhad Fadakar, Adam Chan
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Patent number: 8114957Abstract: Processes for preparing relatively high molecular weight poly(trimethylene ether)glycol employing a cocatalyst system are provided.Type: GrantFiled: February 9, 2009Date of Patent: February 14, 2012Assignee: E. I. du Pont de Nemours and CompanyInventors: Yanhui Niu, Zuohong Yin
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Patent number: 8092682Abstract: The present invention relates to a separation matrix comprised of a support to the surfaces of which polymer chains have been coupled, wherein each polymer chain presents recurring proton-donating groups and at least the surface of the support is substantially hydrophilic. In the most advantageous embodiment, the support is porous cross-linked agarose, the polymers are poly(acrylic acid) and the proton-donating groups are carboxyl groups. The matrix is useful e.g. to remove PEG from pegylated and/or native compounds in a liquid. Accordingly, the invention also encompasses a method, such as a chromatographic method, wherein the separation matrix according to the invention is used, for example as a pre-treatment of a reaction mixture that comprises unreacted PEG, pegylated proteins and native proteins.Type: GrantFiled: July 21, 2009Date of Patent: January 10, 2012Assignee: GE Healthcare Bio-Sciences ABInventors: James Van Alstine, Jan Bergstrom, Henrik Ihre, Tobias Soderman
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Patent number: 8053607Abstract: A method for producing a polyether-polyol having a narrow molecular weight distribution, which comprises carrying out selective fractional extraction of the low-molecular weight component from a polyether-polyol (A) having an average molecular weight of from 500 to 4500 represented by formula (1): HO—[(CH2)4O]n—[(CR1R2)pO]q—H??(1) wherein R1 and R2, which may be the same or different, each represents a hydrogen atom or a linear or branched alkyl group having from 1 to 5 carbon atoms; n indicates a positive integer; p indicates an integer of from 1 to 8; and q indicates 0 or a positive integer, by the use of an aqueous solution (C) containing from 15 to 70 wt % sulfuric acid at a room temperature to 100° C., to thereby suitably determine the amount of the aqueous sulfuric acid solution to the overall organic layer and the sulfuric acid concentration in accordance with the molecular weight and molecular weight distribution of the intended polyether-polyol to be fractionally extracted.Type: GrantFiled: December 19, 2003Date of Patent: November 8, 2011Assignee: Hodogaya Chemical Co., Ltd.Inventors: Kazuaki Okabe, Hiroshi Nakaoka, Ikuhiko Kanehira
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Patent number: 8034980Abstract: A process for preparing polyether polyols by reaction of the following starting materials: a) one or more alkylene oxides and, if appropriate, carbon dioxide and also b) one or more H-functional starter substances, in the presence of a catalyst, in a reaction unit having a plurality of parallel layers A, B which are microstructured so that each layer has a multiplicity of channels which are arranged parallel to one another and form a continuous flow path from one side of the plate to the opposite side of this, wherein a distribution device for introduction of the starting materials and the catalyst is provided at one end of the channels of the layers A and a collection device for the reaction mixture is provided at the other end of these is proposed.Type: GrantFiled: May 22, 2007Date of Patent: October 11, 2011Assignee: BASF AktiengesellschaftInventors: Achim Loeffler, Wolfgang Loth, Ralf Boehling, Thomas Ostrowski, Michael Stoesser, Hartwig Voss, Axel Schimpf
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Patent number: 8017814Abstract: A process for the preparation of a polyether polyol containing at most about 15 ppm of sodium and potassium, comprising: (a) reacting an initiator having at least two active hydrogen atoms with at least one alkylene oxide in the presence of a catalyst having an alkali metal hydroxide to form a polyether polyol reaction product; (b) neutralizing the polyether polyol reaction product obtained in step (a) by contacting this reaction product with phosphoric acid and water; and (c) removing the salt crystals from the polyether polyol and recovering the neutralized polyether polyol containing at most about 15 ppm of sodium and potassium, wherein no adsorption agent and no hydrate of a metal salt of the acid are used before, during or after the neutralization.Type: GrantFiled: February 3, 2009Date of Patent: September 13, 2011Assignee: Shell Oil CompanyInventors: Melis Hasselaar, Parminder Singh Sangha, Andreas Wilhelmus De Winter
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Patent number: 7919575Abstract: The process of the present invention provides for the manufacture of lower molecular weight DMC-catalyzed polyols than is possible using non-acidified continuous addition of starter (CAOS) feeds, by adding excess acid to a starter feed stream over that required for mere neutralization of the basicity of the starter. The benefits of the invention also extend to starters which do not contain basicity. Polyether polyols made by the inventive process may be used to produce improved polyurethane products such as coatings, adhesives, sealants, elastomers, foams and the like.Type: GrantFiled: May 25, 2010Date of Patent: April 5, 2011Assignee: Bayer MaterialScience LLCInventor: Edward Browne
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Publication number: 20100292515Abstract: An impurity derived from a high-molecular-weight polyethylene glycol compound is removed from a high-molecular-weight polyethylene glycol compound whose total average number of moles of ethylene oxide units added in the molecule is 220 to 4500. In a state where the high-molecular-weight polyethylene glycol compound is dissolved in at least one of water and an organic solvent selected from aromatic hydrocarbon solvents having 8 or less carbon atoms in total and ester compound solvents having 5 or less carbon atoms in total, the water and the organic solvent are mixed. The resulting mixture was separated into an organic layer and an aqueous layer, and the organic layer is separated from the aqueous layer.Type: ApplicationFiled: March 31, 2010Publication date: November 18, 2010Applicant: NOF CORPORATIONInventors: Yuji Yamamoto, Hiroki Yoshioka
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Patent number: 7745668Abstract: Processes for reducing color in PO3G are provided. The processes include contacting PO3G with an activated carbon and then separating the PO3G from the activated carbon by, for example, filtration. The process provides PO3G having an APHA color less than that before contact with the absorbent. The processes are desirably used for polymers having a molecular weight of about 250 to about 5000.Type: GrantFiled: August 3, 2007Date of Patent: June 29, 2010Assignee: E. I. du Pont de Nemours and CompanyInventors: Hari Babu Sunkara, Hiep Quang Do
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Publication number: 20100105959Abstract: The invention relates to a process for removing poly(propylene oxide) from propylene oxide by membrane separation, wherein a membrane having an average pore size of from 0 to 5 nm is used. In said process, a liquid feed comprising propylene oxide and poly(propylene oxide) may be separated by the membrane into a permeate comprising propylene oxide and either no poly(propylene oxide) or poly(propylene oxide) at a concentration which is lower than the poly(propylene oxide) concentration in the feed, and a retentate comprising propylene oxide and poly(propylene oxide) at a concentration which is higher than the poly(propylene oxide) concentration in the feed.Type: ApplicationFiled: December 18, 2007Publication date: April 29, 2010Inventors: Johannes Gerhardus Joseph Beckers, Johannes Leendert Willem Cornelis Den Boestert, Nigel Wagstaff
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Patent number: 7678944Abstract: The invention aims at providing a process of subjecting a polyether polymer containing a double metal cyanide complex and/or residue compounds thereof as the metallic impurities to extraction with water to thereby remove the metallic impurities, which enables simpler and complete removal of the impurities; and polyether polymers obtained by the process. This aim is attained by a process for the purification of polyethers characterized by blending (A) a polyether containing a double metal cyanide complex and/or residue compounds thereof with ascorbic acid or a derivative thereof and water and then removing the aqueous phase from the resulting mixture to thereby remove the double metal cyanide and/or the residue compounds.Type: GrantFiled: October 28, 2005Date of Patent: March 16, 2010Assignee: Kaneka CorporationInventor: Hideharu Jono
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Publication number: 20100016536Abstract: An improved process for separating and isolating individual polar protic monomer(s) and/or oligomer(s) on the basis of degree of polymerization. A liquid sample containing polar protic monomer(s) and/or oligomer(s) is introduced into a liquid chromatography (LC) column packed with a polar bonded stationary chromatographic phase. The individual polar protic monomer(s) and/or oligomer(s) are separated via a binary mobile phase elution. One or more individual fractions containing the monomer(s) and/or oligomer(s) are eluted. The polar protic monomer(s) and/or oligomer(s) may be proanthocyanidins, hydrolyzable tannins, oligosaccharides, oligonucleotides, peptides, acrylamides, polysorbates, polyketides, poloxarners, polyethylene glycols, polyoxyethylene alcohols or polyvinyl alcohols. The binary mobile phase comprises an A phase consisting essentially of a polar aprotic solvent and a B phase consisting essentially of a polar protic solvent. A process for separating and isolating xanthine(s) (e.g.Type: ApplicationFiled: June 18, 2009Publication date: January 21, 2010Applicant: Mars, IncInventors: Mark A. Kelm, Christopher J. Johnson, Rebecca J. Robbins
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Patent number: 7553921Abstract: A polyether polyol composition, the reactivity of which with a polyisocyanate can be controlled, to thereby obtain an isocyanate group-terminated prepolymer having excellent storage stability. A polyether polyol composition comprising a polyether polyol obtained by a ring-opening polymerization of an alkylene oxide in the presence of a composite metal cyanide complex catalyst, and a phosphoric acid compound comprising a phosphoric acid selected from orthophosphoric acid, polyphosphoric acid and polymetaphosphoric acid, and/ or a partial ester of such a phosphoric acid, wherein the polyether polyol composition contains metals derived from the composite metal cyanide complex catalyst in an amount of from 1 to 30 ppm based on the polyether polyol, and the above phosphoric acid compound in an amount of from 0.5 to 100 ppm based on the polyether polyol.Type: GrantFiled: July 26, 2005Date of Patent: June 30, 2009Assignee: Asahi Glass Company, LimitedInventors: Chitoshi Suzuki, Hiroki Fukuda, Shigeru Ikai
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Patent number: 7528288Abstract: The invention provides a process for preparing polyether alcohols by adding alkylene oxides onto H-functional starter substances using DMC catalysts, which comprises, in a first step, adding propylene oxide or a mixture of propylene oxide and ethylene oxide onto H-functional starter substances and, in a second step, transferring the product thus formed into a tubular reactor in which mixtures of ethylene oxide and propylene oxide are metered in at least two metering points, the proportions of ethylene oxide and propylene oxide in the mixtures metered in in the first and in the second step being different, the proportions of ethylene oxide and propylene oxide in the mixtures metered in at least two metering points in the second step being different, and the mixture metered in in the second step, at least at the last metering point, comprising at least 40% by weight of ethylene oxide.Type: GrantFiled: August 21, 2006Date of Patent: May 5, 2009Assignee: BASF AktiengesellschaftInventors: Thomas Ostrowski, Achim Loeffler, Raimund Ruppel
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Patent number: 7414159Abstract: A liquid mixture comprising at least one readily volatile and at least one sparingly volatile component is separated in a film evaporator by a process in which (i) a continuous stream of a liquid starting material mixture is provided, (ii) a liquid film is produced from the continuous stream and is brought into contact with a heat exchange surface of the Mm evaporator, (ii) the liquid film is partly evaporated, a gas stream enriched with the at least one readily volatile component and a liquid stream enriched with the at least one sparingly volatile component being obtained, wherein (iv) the heat exchange surface is coated with a catalytically active material which (v) catalyzes, in the liquid film, a chemical reaction in which at least one readily volatile component is formed.Type: GrantFiled: March 3, 2004Date of Patent: August 19, 2008Assignee: BASF SEInventors: Eckhard Stroefer, Neven Lang, Ute Lichtfers, Ulrich Steinbrenner, Hans Hasse
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Patent number: 7342142Abstract: A process comprising contacting PO3G having color with hydrogen in the presence of a hydrogenation catalyst, wherein the PO3G, after hydrogenation, has a APHA color of less than about 50.Type: GrantFiled: August 5, 2003Date of Patent: March 11, 2008Assignee: E.I. du Pont de Nemours and CompanyInventors: Hari Babu Sunkara, Mayis Seapan, George Francis Diffendall, Francis Glenn Gallagher
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Patent number: 7294746Abstract: Processes for reducing color in PO3G are provided. The processes include contacting PO3G with an adsorbent and then separating the PO3G from the adsorbent by, for example, filtration. The process provides PO3G having an APHA color preferably less than about 50. The processes are desirably used for polymers having a molecular weight of about 250 to about 5000.Type: GrantFiled: November 10, 2005Date of Patent: November 13, 2007Assignee: E.I. du Pont de Nemours and CompanyInventors: Hari Babu Sunkara, Hiep Quang Do
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Patent number: 7288682Abstract: A process for separating bifunctional perfluoropolyethers (PFPEs) having two terminations —CH2OH from their mixtures with monofunctional PFPEs with one termination —CH2OH, of general formula X1—O—Rf—Y ??(I) wherein Rf is a perfluoropolyoxyalkylene chain having a number average molecular weight of 500-10,000; X1 and Y are end groups selected from —CFXCH2OH (wherein X is F or CF3), —CF3, —CF2Cl, —CF2CF2Cl, —C3F6Cl, —CF2Br, —CF2CF3, wherein at least one of the two end groups is —CFXCH2OH, said process comprising the steps of: a) addition of the PFPE mixture to an adsorbing solid phase, under stirring; b) filtration of the mixture obtained in a): c) addition to the solid phase filtered in b), of a PFPE mixture having an average functionality higher than that of the PFPE mixture of the liquid filtered in b); c2) filtration of the mixture obtained in c); and subsequent treatment of the solid phase separated in c2) with a polar solvent obtaining a liquid containing the PFPE having high functionality.Type: GrantFiled: July 8, 2005Date of Patent: October 30, 2007Assignee: Solvay Solexis S.p.A.Inventors: Alexandre Tchistiakov, Simonetta Fontana, Claudio Tonelli
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Patent number: 7214833Abstract: A process to obtain perfluoropolyethers comprising: a) synthesis of peroxidic perfluoropolyethers by one of the following reactions: al) TFE photooxidation, in solvents selected between perfluorocarbons and (mono)hydrofluorocarbons, of general formula: CyF(2y+2?X)Hx ??(II) ?wherein y is an integer from 2 to 4; x is an integer equal to 0 or 1; in the present of fluorine diluted with an inert gas; or a2) TFE oxidation using as radical initiator fluorine or hypofluorites of formula RfOF??(III) ?(Rf perfluoroalkyl radical from 1 to 3 carbon atoms), operating from ?40° C. to ?100° C. at a pressure comprised between 0 and 12 bar; b) thermal treatment of the product obtained in a) at a temperature from 1500° C. to 250° C.; c) treatment with elemental fluorine of the polymer obtained in step b) at temperatures from 100° C. to 250° C., or by treatment with fluorine in the presence of UV radiations, operating at temperatures from ?50° C. to 120° C.Type: GrantFiled: September 30, 2004Date of Patent: May 8, 2007Assignee: Solvay Solexis, S.p.A.Inventors: Giuseppe Marchionni, Elvira Pagano, Pier Antonio Guarda
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Patent number: 7186867Abstract: Process for preparing polyether polyols having an end block of ethylene oxide by addition of alkylene oxides onto H-functional starter substances, in which A) a polyether polyol precursor is prepared by means of double metal cyanide (DMC) catalysis in a semicontinuous mode of operation in which previously prepared polyether polyol together with the DMC catalyst are placed in a reactor and H-functional starter substance and propylene oxide are added continuously, B) the polyether polyol precursor from stage A) is reacted with propylene oxide or an ethylene oxide/propylene oxide mixture in the presence of the DMC catalyst in a continuously operating reactor to give a polyether polyol intermediate, C) the intermediate from stage B) is mixed with an alkali metal hydroxide as catalyst and D) reacted with ethylene oxide in a continuously operating reactor to give the final product, E) the catalyst is separated off from the final product obtained in stage D).Type: GrantFiled: April 21, 2004Date of Patent: March 6, 2007Assignee: BASF AktiengesellschaftInventors: Thomas Ostrowski, Raimund Ruppel, Gerd Höppner, Sascha Bergmann, Koenraad Vandewalle, Eva Baum
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Patent number: 7074969Abstract: There is disclosed a process for preparing polytrimethylene ether glycol by acid catalyzed polycondensation, neutralization and contact with filter aid. The process avoids hydrolysis and yet provides product substantially free of catalyst derived end groups.Type: GrantFiled: June 18, 2004Date of Patent: July 11, 2006Assignee: E.I. du Pont de Nemours and CompanyInventors: Hari Babu Sunkara, Paraskevi Parmpi
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Patent number: 7009082Abstract: A process is described for reducing the discoloration of PO3G. The discolored polymer is contacted with adsorbent and separated therefrom, for instance, by filtration. The treated polytrimethylene, preferably, has an APHA color of less than about 50 and a molecular weight of about 250 to about 5000.Type: GrantFiled: August 5, 2003Date of Patent: March 7, 2006Assignee: E.I. du Pont de Nemours and CompanyInventors: Hari Babu Sunkara, Hiep Quang Do
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Patent number: 7005552Abstract: The present invention relates to processes for preparing ethylene oxide (EO)-capped polyols in which removal of catalyst residues or salts formed by the neutralization of the basic catalyst is not required prior to discharging the polyol from the reactor because neutralization occurs during or after the starter charge of a subsequent batch. The inventive processes allow for the preparation of DMC-catalyzed intermediates and their base-catalyzed EO caps within the same reactor. Polyols produced by the processes of the invention have a high content of primary hydroxyl groups and may be useful for producing polyurethane foams, elastomers, sealants, coatings, adhesives and the like.Type: GrantFiled: November 3, 2003Date of Patent: February 28, 2006Assignee: Bayer Materialscience LLCInventor: Bryan D. Kaushiva
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Patent number: 6987201Abstract: The present invention provides acetic anhydride, a method of purifying crude acetic anhydride, and a method of producing polyoxytetramethylene glycol using acetic anhydride. A method of producing polyoxytetramethylene glycol by ring-opening-polymerizing tetrahydrofuran in the presence of acetic anhydride and an acid catalyst, wherein said ring-opening polymerization is conducted using acetic anhydride having a diketene concentration of 10 ppm or less to produce polyoxytetramethylene glycol.Type: GrantFiled: February 16, 2001Date of Patent: January 17, 2006Assignee: Daicel Chemical Industries, Ltd.Inventors: Seiji Nishioka, Ryosuke Maeda, Toshifumi Fukui, Mitsuru Yamashita
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Patent number: 6977045Abstract: A process for the purification or fractionation of aqueous soluble polymers using an aqueous two-phase system is described. The concentrations of the polymer to be fractionated and of an aqueous soluble salt, and the temperature of the aqueous fractionation medium are adjusted so that two phases form, the lower molecular weight polymer molecules partition into the high salt concentration phase, and the higher molecular weight polymer molecules partition into the low salt concentration phase. The resulting high molecular weight polymers are characterized by a higher average molecular weight and a narrower molecular weight distribution and decreased unsaturation than the unfractionated polymers. After being subjected to the fractionation process, polyol polymers that form hydrogels in aqueous solution exhibited higher viscosities and a liquid to gel transition over a narrower temperature range than the unfractionated polyol polymers.Type: GrantFiled: January 28, 2004Date of Patent: December 20, 2005Assignee: Pluromed, Inc.Inventors: Lorraine E. Reeve, Michael G. Hinsberg
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Patent number: 6939993Abstract: Method for separating reaction product from imide compound catalyst represented by Formula (1) or derivative thereof in reaction mixture obtained by reaction in presence of imide compound catalyst: wherein R1 and R2 are each, for example, a hydrogen atom or an alkyl group, where R1 and R2 may be combined to form a double bond, an aromatic ring, or a non-aromatic ring, and X is an oxygen atom or a hydroxyl group. The method includes an extraction process using two organic solvents separable from each other to thereby separate the reaction product into one organic solvent layer and the imide compound catalyst component into the other organic solvent layer. The disclosed method efficiently and simply separates the reaction product from the catalyst component.Type: GrantFiled: October 25, 2001Date of Patent: September 6, 2005Assignee: Daicel Chemical Industries, Ltd.Inventor: Michihiro Sugahara
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Patent number: 6930210Abstract: The invention relates to a process to produce high-purity, low-odour polyether polyols, with very low levels of catalytic residues, by means of alkene oxide polyaddition reactions to substances that contain active hydrogens in the presence double metal cyanides as catalysts. The process is characterized in that the reaction is carried out in the presence of sepiolites and/or by subsequent treatment with sepiolites of the polyether polyols produced with double metal cyanides in the absence of sepiolites.Type: GrantFiled: February 25, 2003Date of Patent: August 16, 2005Assignee: Repsol Quimica S.A.Inventors: Mariano Malaga Mellado, Dolores Blanco Gonzalez, Beatriz Montalvo Barroso
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Patent number: 6858761Abstract: The present invention provides a process and its utilization in a process comprising the step of carrying out an addition reaction of an alkylene oxide to an addition-receiving substance in the presence of a resin catalyst, thereby producing the addition reaction product, when the resin catalyst as used for the reaction is persevered so as to recycle it after it is recovered, the unreacted alkylene oxide remaining in the resin catalyst can be prevented from polymerizing and solidifying during the preservation, and the resin catalyst accordingly can be preserved stably for a long time. The resin catalyst as recovered after it is used for the reaction may be preserved under any of the following conditions: 1) at a low temperature of not higher than 40° C.Type: GrantFiled: March 18, 2002Date of Patent: February 22, 2005Assignee: Nippon Shokubai Co., Ltd.Inventors: Yukihiro Yoneda, Tokumasa Ishida, Masahiro Uemura
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Patent number: 6835686Abstract: A catalyst system comprising a primary catalyst chosen from one or more homogeneous or heterogeneous, inorganic, organic or complex metal-containing compound; and one or more phenolic activator/modifier(s). The catalyst system can be used for the preparation of allylic alcohols by rearrangement of corresponding epoxides, the subsequent Oppenauer type oxidation of allylic alcohols to alpha, beta-unsaturated carbonyl compounds, and/or the preparation of alpha, beta-unsaturated carbonyl compounds by rearrangement of epoxides to corresponding allylic alcohols followed by the subsequent Oppenauer type oxidation of allylic alcohols in a one pot process.Type: GrantFiled: July 5, 2001Date of Patent: December 28, 2004Assignee: Millennium Specialty ChemicalsInventors: Gennadiy G. Kolomeyer, Jacob S. Oyloe
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Patent number: 6818587Abstract: The invention relates to double-metal cyanide (DMC) catalysts for preparing polyether polyols by the polyaddition of alkylene oxides on to starter compounds containing active hydrogen atoms, wherein the DMC catalysts are composed of: a) at least one DMC compound; b) at least one organic complexing ligand which is not a cyclic polyol; and c) at least one cyclic polyol. The DMC catalysts of the present invention have increased activity compared to known catalyst.Type: GrantFiled: August 28, 2002Date of Patent: November 16, 2004Assignee: Bayer AktiengesellschaftInventors: Walter Schäfer, Jörg Hofmann, Pieter Ooms
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Patent number: 6812367Abstract: Polyethylene glycol for use in fields with application to a living body wherein the sum of the contents of ethylene glycol and diethylene glycol in the polyethylene glycol is less than or equal to that expressed in the following formula [I]: Sum ⁢ ⁢ of ⁢ ⁢ ethylene ⁢ ⁢ glycol ⁢ ⁢ and ⁢ ⁢ diethylene ⁢ ⁢ glycol ⁢ ⁢ contents ⁢Type: GrantFiled: June 18, 2003Date of Patent: November 2, 2004Assignee: NOF CorporationInventors: Kenji Sakanoue, Kouzoh Sanchika, Tohru Yasukohchi
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Patent number: 6780813Abstract: The invention relates to an improved method of producing double-metal cyanide (DMC) catalysts for the production of polyether polyols by polyaddition of alkylene oxides to starter compounds containing active hydrogen atoms, in which the DMC catalyst dispersion is produced using a mixing nozzle, preferably a jet disperser. The DMC catalysts produced in this way have an increased activity in polyether polyol production, reduced particle size and narrower particle size distribution.Type: GrantFiled: May 30, 2002Date of Patent: August 24, 2004Assignee: Bayer AktiengesellschaftInventors: Jörg Hofmann, Bernd Klinksiek, Stephan Ehlers, Thorsten Fechtel, Franz Föhles, Pieter Ooms
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Patent number: 6776925Abstract: The present invention relates to a process for the production of polyether polyols by polyaddition of alkylene oxides onto starter compounds containing active hydrogen atoms conducted in the presence of a double-metal cyanide catalyst wherein a reaction mixture is guided at least once through a zone which has an energy density of at least 105 J/m3 and wherein the residence time of the reaction mixture in this zone is at least 10−6 seconds per pass.Type: GrantFiled: February 19, 2002Date of Patent: August 17, 2004Assignees: Bayer Aktiengesellschaft, Bayer Polymers LLCInventors: Jörg Hofmann, Stephan Ehlers, Bernd Klinksiek, Lars Obendorf, Christian Steinlein, Bert Klesczewski, Jose F. Pazos
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Patent number: 6761824Abstract: A process for the purification or fractionation of aqueous soluble polymers using an aqueous two-phase system is described. The concentrations of the polymer to be fractionated and of an aqueous soluble salt, and the temperature of the aqueous fractionation medium are adjusted so that two phases form, the lower molecular weight polymer molecules partition into the high salt concentration phase, and the higher molecular weight polymer molecules partition into the low salt concentration phase. The resulting high molecular weight polymers are characterized by a higher average molecular weight and a narrower molecular weight distribution and decreased unsaturation than the unfractionated polymers. After being subjected to the fractionation process, polyol polymers that form hydrogels in aqueous solution exhibited higher viscosities and a liquid to gel transition over a narrower temperature range than the unfractionated polyol polymers.Type: GrantFiled: August 13, 2001Date of Patent: July 13, 2004Inventors: Lorraine E. Reeve, Michael G. Hinsberg