Purification Or Recovery Patents (Class 568/724)
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High purity 9,9-bis-(hydroxyphenyl)-fluorene and method for the preparation and purification thereof
Patent number: 6620979Abstract: A 9,9-bis (4-hydroxyphenyl) fluorene compound showing a melting curve maximum of at least 226.00° C. and a melting curve width at 5% equal to or lower than 1.30° C. A purification process for the preparation of 9,9-bis (4-hydroxyphenyl) fluorene compounds comprising a first purification step employing acetonitrile and a second purification step employing a solvent selected from the group consisting of aliphatic alcools, a mixture of aromatic hydrocarbons and aliphatic alco-hols and a mixture of aromatic hydrocarbons and nitrites.Type: GrantFiled: April 8, 2002Date of Patent: September 16, 2003Assignee: Ferrania, S.p.A.Inventors: Simone Angiolini, Mauro Avidano -
Patent number: 6600004Abstract: A method of preparing polyestercarbonates is presented in which a mixture of at least one activated diaryl carbonate is reacted under melt polymerization conditions with at least one aromatic dihydroxy compound together with at least one dicarboxylic acid. Polyestercarbonates possessing up to about percent 10 mole dicarboxylic acid residues based on the total amount of structural units derived from aromatic dihydroxy compounds are obtained. The method provides both for high levels of incorporation of the dicarboxylic acid into the polyestercarbonate backbone and a high level of polymer endcapping.Type: GrantFiled: April 10, 2002Date of Patent: July 29, 2003Assignee: General Electric CompanyInventors: Patrick Joseph McCloskey, Paul Michael Smigelski
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Patent number: 6576801Abstract: The present invention relates to a method of neutralizing residual acid species in crude dihydric phenol comprising the step of introducing a thermally stable organic base selected from the group consisting of tetraalkyl phosphonium hydroxides, tetraorganophosphonium carboxylic acid salts, or a mixture thereof into the crude dihydric phenol.Type: GrantFiled: February 25, 2002Date of Patent: June 10, 2003Assignee: General Electric CompanyInventors: Paul Michael Smigelski, Jr., Timothy Brydon Burnell, Patrick Joseph McCloskey
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Publication number: 20030096939Abstract: The invention relates to substance mixtures, containing bisphenol A, two methods for production thereof and use thereof for production of polymeric materials.Type: ApplicationFiled: September 26, 2002Publication date: May 22, 2003Inventors: Michael Bodiger, Rainer Neumann, Frieder Heydenreich, Michael Prein
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Patent number: 6545187Abstract: Low-particulate dihydric aromatic compounds such as bisphenol-A that can be used in the synthesis of low-particulate polycarbonates are prepared by introducing into a desorber column containing a non-aggregate packing material an adduct of bisphenol and phenol and optionally a stripping gas. The column is maintained at an operating temperature that is sufficiently high and an operating pressure that is sufficiently low such that the adduct is distilled. The stream of phenol and the stripping gas is recovered from the top of the column. A second stream containing bisphenol that is substantially free of added particulate matter is recovered from the bottom of the column. This purified stream of bisphenol-A can further be used in a method of producing optical-grade polycarbonate.Type: GrantFiled: September 19, 2001Date of Patent: April 8, 2003Assignee: General Electric CompanyInventors: Gaylord Michael Kissinger, Fang Christine Chen, James Cristopher Blubaugh, Darlene Hope Nance, Edward Brittain Stokes, Juan Rodriguez Ordonez, Jose M. Quintana
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Patent number: 6512148Abstract: A process for the production of bisphenol A, including providing a melt of a crystalline adduct of bisphenol A and phenol, contacting the melt with a cation donating solid to neutralize the strong acid therewith, and then heating the melt to vaporize and remove phenol from the melt.Type: GrantFiled: September 26, 2001Date of Patent: January 28, 2003Assignee: Mitsubishi Chemical CorporationInventors: Susumu Yamamoto, Atsumi Kukidome, Makoto Nomura, Keiji Maehara, Kenji Nagahama
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Publication number: 20020183562Abstract: The present application relates to a process for producing high-purity bis(4-hydroxyaryl)alkanes from adducts of bis(4-hydroxyaryl)alkanes and aromatic hydroxy compounds, which are obtained by acid-catalysed reaction of the aromatic hydroxy compounds with ketones.Type: ApplicationFiled: June 17, 2002Publication date: December 5, 2002Inventors: Rainer Neumann, Rolf Lanze, Frieder Heydenreich, Michael Bodiger, Michael Prein
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Patent number: 6464838Abstract: A process for the recovery of compounds present in a mixture containing residues of heavy products is provided. The process includes conducting a reaction and distillation to obtain the compounds and residues and macerating the residues before they can set to mass. The residues can then be destroyed. The process is particularly suitable for the treatment of the residues obtained in the preparation of phenol from cumene.Type: GrantFiled: July 12, 1999Date of Patent: October 15, 2002Assignee: Rhodia ChimieInventors: Jean-Jacques Charrin, Francoise Igersheim, Antonio Queiroz
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Patent number: 6414106Abstract: The present invention relates to a method of neutralizing residual acid species in crude dihydric phenol comprising the step of introducing a thermally stable organic base selected from the group consisting of tetraalkyl phosphonium hydroxides, tetraorganophosphonium carboxylic acid salts, or a mixture thereof into the crude dihydric phenol.Type: GrantFiled: March 2, 2001Date of Patent: July 2, 2002Assignee: General Electric CompanyInventors: Paul Michael Smigelski, Jr., Timothy Brydon Burnell, Patrick Joseph McCloskey
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Patent number: 6414198Abstract: A process of preparing bisphenol A having low residual contents of oxygen and phenol is described. The process involves: (a) melting mixed crystals of bisphenol A and phenol under a nitrogen atmosphere at a temperature of 100° C. to 120° C.; (b) feeding continuously the melt formed in step (a) into the top of a distillation unit under conditions of 120° C. to <160° C. and a pressure of >80 mbar to 200 mbar; (c) feeding contemporaneously with step (b) nitrogen into the bottom of the distillation unit; (d) allowing the melted feed material and the nitrogen feed to contact each other within the distillation unit, thereby forming a concentrated melt material having (i) a phenol content reduced to 10 to 25 wt. %, and (ii) a reduced oxygen content (e.g., an oxygen content of <1 ppm); and (e) optionally passing a stream of nitrogen through the concentrated melt material under conditions of at least atmospheric pressure, 180° C. to 220° C. and a nitrogen partial pressure of 1 to 1.Type: GrantFiled: June 21, 2001Date of Patent: July 2, 2002Assignee: Bayer AktiengesellschaftInventors: Rolf Lanze, Rainer Neumann, Steffen Kühling, Frieder Heydenreich, Tony Van Osselaer
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Publication number: 20020055661Abstract: A process for producing bis(4-hydroxyaryl)alkane is disclosed. The process comprise in sequence the steps of (a) passing inert gas through a melt at 150 to 230° C. that contains bis(4-hydroxyaryl)alkane and other aromatic hydroxy compounds, under conditions designed to remove said other aromatic hydroxy compounds from said melt and to obtain a stream of inert gas that contains said other aromatic hydroxy compounds (b) condensing the stream obtained in (a) to remove said other aromatic hydroxy compound, and to obtain a stream of inert gas, and (c) purifying and compressing the stream of inert gas obtained in (b), and recycling to step (a).Type: ApplicationFiled: January 3, 2002Publication date: May 9, 2002Inventors: Steffen Kiihling, Rolf Lanze, Rainer Neumann, Frieder Heydenreich, Tony van Osselaer
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Patent number: 6384288Abstract: A process for producing bis(4-hydroxyaryl)alkane is disclosed. The process comprise in sequence the steps of (a) passing inert gas through a melt at 150 to 230° C. that contains bis(4-hydroxyaryl)alkane and other aromatic hydroxy compounds, under conditions designed to remove said other aromatic hydroxy compounds from said melt and to obtain a stream of inert gas that contains said other aromatic hydroxy compounds (b) condensing the stream obtained in (a) to remove said other aromatic hydroxy compound, and to obtain a stream of inert gas, and (c) purifying and compressing the stream of inert gas obtained in (b), and recycling to step (a).Type: GrantFiled: April 16, 2001Date of Patent: May 7, 2002Assignee: Bayer AktiengesellschaftInventors: Steffen Kühling, Rolf Lanze, Rainer Neumann, Frieder Heydenreich, Tony van Osselaer
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Publication number: 20020045726Abstract: The present invention relates to a method for avoiding undesirable discoloration in polycarbonate production by catalytic removal of dissolved oxygen from phenol byType: ApplicationFiled: February 5, 2001Publication date: April 18, 2002Inventors: Frieder Heydenreich, Rudolf Wagner, Michael Bodiger
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Patent number: 6316678Abstract: The present invention relates to a process for producing bis(4-hydroxy-aryl)alkanes of high purity from addition products of bis(4-hydroxy-aryl)alkanes and aromatic hydroxy compounds which are obtained by the acid-catalysed reaction of the aromatic hydroxy compounds with ketones.Type: GrantFiled: February 28, 2001Date of Patent: November 13, 2001Assignee: Bayer AktiengesellschaftInventors: Steffen Kühling, Rolf Lanze, Rainer Neumann, Frieder Heydenreich, Tony van Osselaer, Gerhard Fennhoff
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Patent number: 6313355Abstract: Tetrabromobisphenol-A is produced in a bromination process where no bromine or only a very small proportion of bromine is fed to the reactor. In the process aqueous hydrobromic acid, is the sole source or a major source of the bromine. In the process there are at least three concurrent continuous feeds to the reactor. One is composed of bisphenol-A and/or underbrominated bisphenol-A and a water-miscible organic solvent. The second is gaseous hydrogen bromide or preferably, aqueous hydrobromic acid, and the third is aqueous hydrogen peroxide. Optionally a small additional continuous feed of bromine can be employed. The feeds are proportioned to maintain a liquid phase containing (i) from above about 15 to about 85 wt % water, based upon the amount of water and water-miscible organic solvent in such liquid phase, and (ii) an amount of unreacted bromine that is in excess over the stoichiometric amount theoretically required to convert the bisphenol-A and/or underbrominated bisphenol-A to tetrabromobisphenol-A.Type: GrantFiled: July 12, 2000Date of Patent: November 6, 2001Inventors: Thanikavelu Manimaran, Richard A. Holub, Randall S. Barton
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Patent number: 6307111Abstract: The present invention relates to a process for the continuous production of dihydroxydiarylalkanes (bisphenols) by the reaction of fresh phenol, phenol and isoalkenylphenol from the decomposition of by-products, and ketone. In this process the bulk of the bisphenol is recovered from the reaction mixture by crystallization and the mother liquor obtained is freed from phenol by distillation. The phenol is returned to the reaction and the bottoms obtained during the distillation are decomposed in a reactive rectification after addition of a basic catalyst. The phenol and isoalkenylphenol leaving at the top are led back into the reaction; the bottoms from the first reactive column are acidified and in a second reactive rectification, in the presence of an acid catalyst, are further decomposed into phenol, which distils off and is reused in the reaction, and bottoms, which are disposed of.Type: GrantFiled: November 12, 1999Date of Patent: October 23, 2001Assignee: Bayer AktiengesellschaftInventors: Gerhard Fennhoff, Hans-Josef Buysch, Gerd Fengler
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Patent number: 6300527Abstract: This invention relates, inter alia, to a process for the production of tetrabromobisphenol-A by the bromination of bisphenol-A and/or underbrominated bisphenol-A, which process features: a water and water-miscible organic solvent reaction medium; a relatively high reaction temperature; and the presence, in the reaction medium, of both (i) excess unreacted Br2 during the feed of bisphenol-A to the reactor, and (ii) sufficient HBr to protect the tetrabromobisphenol-A produced against undesirable color formation. Tetrabromobisphenol-A precipitates from the reaction mass and is easily recovered. Product of high purity (97% or more) and very low color (APHA of 50 or less) can be produced, even when using large excesses of bromine in the reaction.Type: GrantFiled: July 12, 2000Date of Patent: October 9, 2001Assignee: Albemarle CorporationInventors: Thanikavelu Manimaran, Hassan Y. Elnagar, Richard A. Holub, Alvin E. Harkins, Jr., Bonnie G. McKinnie
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Patent number: 6235946Abstract: Tetrabromobisphenol-A is produced in a bromination process where no bromine or only a very small proportion of bromine is fed to the reactor. In the process aqueous hydrobromic acid, is the sole source or a major source of the bromine. In the process there are at least three concurrent continuous feeds to the reactor. One is composed of bisphenol-A and/or underbrominated bisphenol-A and a water-miscible organic solvent. The second is gaseous hydrogen bromide or preferably, aqueous hydrobromic acid, and the third is aqueous hydrogen peroxide. Optionally a small additional continuous feed of bromine can be employed. The feeds are proportioned to maintain a liquid phase containing (i) from above about 15 to about 85 wt % water, based upon the amount of water and water-miscible organic solvent in such liquid phase, and (ii) an amount of unreacted bromine that is in excess over the stoichiometric amount theoretically required to convert the bisphenol-A and/or underbrominated bisphenol-A to tetrabromobisphenol-A.Type: GrantFiled: October 12, 1999Date of Patent: May 22, 2001Assignee: Albemarle CorporationInventors: Thanikavelu Manimaran, Richard A. Holub, Randall S. Barton
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Patent number: 6218584Abstract: This invention relates, inter alia, to a process for the production of tetrabromobisphenol-A by the bromination of bisphenol-A and/or underbrominated bisphenol-A, which process features: a water and water-miscible organic solvent reaction medium; a relatively high reaction temperature; and the presence, in the reaction medium, of both (i) excess unreacted Br2 during the feed of bis-phenol-A to the reactor, and (ii) sufficient HBr to protect the tetrabromobisphenol-A produced against undesirable color formation. Tetrabromobisphenol-A precipitates from the reaction mass and is easily recovered. Product of high purity (97% or more) and very low color (APHA of 50 or less) can be produced, even when using large excesses of bromine in the reaction.Type: GrantFiled: June 10, 1999Date of Patent: April 17, 2001Assignee: Albemarle CorporationInventors: Thanikavelu Manimaran, Hassan Y. Elnagar, Richard A. Holub, Alvin E. Harkins, Jr., Bonnie G. McKinnie
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Patent number: 6203612Abstract: An alternative and improved method for cleaning cooling and/or crystallization surfaces of a crystallizer fouled with a crystallized bisphenol as a result of processing a slurry derived from the production of bisphenol is provided. The method includes the steps of: (a) draining from 20 to 80%, and preferably about 50% of the slurry from the crystallizer; (b) replacing the drained slurry with a solvent comprising phenol, thereby forming a diluted slurry; (c) increasing the temperature in the crystallizer to a temperature at which the crystallized bisphenol is dissolved in the diluted slurry, and then rapidly cooling the diluted slurry to a temperature of 45 to 55° C.; and (d) adding a seed slurry containing solid bisphenol at a concentration of 5 to 30%. The seed slurry has a temperature of 45 to 55° C. and is added until conditions are established at which bisphenol crystals added to the crystallizer do not redissolve.Type: GrantFiled: March 30, 2000Date of Patent: March 20, 2001Assignee: General Electric CompanyInventors: Rudy Peemans, Jan Huibert Weijland, Mourice Van Sintemaartensdijk
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Patent number: 6197916Abstract: A method for preparing bisphenol A is disclosed, with a selectivity for the p,p′-isomer of greater than about 97%. The method involves reacting phenol with p-isopropenylphenol or 2-(4-hydroxyphenyl)-2-propanol in the presence of a catalyst, at a reaction temperature of no greater than about 65° C. The bisphenol A product is preferably purified by a technique which omits the use of adduct crystallization.Type: GrantFiled: August 30, 1999Date of Patent: March 6, 2001Assignee: General Electric CompanyInventors: Eric James Pressman, Joseph Richard Wetzel
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Patent number: 6162953Abstract: This invention relates to a process for the production of tetrabromobisphenol-A by the bromination of bisphenol-A, which process features the addition of bisphenol-A to a reaction mass containing unreacted Br.sub.2 and 30 to 85 wt % water and an alcohol solvent, the reaction mass being at a relatively high temperature.Type: GrantFiled: September 28, 1999Date of Patent: December 19, 2000Assignee: Albemarle CorporationInventors: Bonnie G. McKinnie, Richard A. Holub, Hassan Y. Elnagar
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Patent number: 6130359Abstract: An improved process for producing Bisphenol-A which is essentially free of sodium impurity using rotary vacuum filter pumps which utilize a liquid ring seal to effect drawing a vacuum on a Bisphenol-A/phenol slurry, the improvement is in using phenol as the liquid ring seal medium.Type: GrantFiled: September 16, 1998Date of Patent: October 10, 2000Assignee: General Electric CompanyInventor: Gaylord M. Kissinger
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Patent number: 6084137Abstract: This invention relates to a process for the production of tetrabromobisphenol-A by the bromination of bisphenol-A, which process features the addition of bisphenol-A to a reaction mass containing unreacted Br.sub.2 and 30 to 85 wt. % water and an alcohol solvent, the reaction mass being at a relatively high temperature.Type: GrantFiled: October 21, 1997Date of Patent: July 4, 2000Assignee: Albemarle CorporationInventors: Bonnie G. McKinnie, Richard A. Holub, Hassan Y. Elnagar
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Patent number: 6011184Abstract: An integrated process for the preparation and recovery of BPA in pure form utilizes a series of steps to crystallize the 1:1 adduct of phenol and bisphenol-A, with periodic descaling of the crystallizer surfaces with a modified reactor/crystallizer containing 1 to 40 percent water.Type: GrantFiled: April 6, 1998Date of Patent: January 4, 2000Assignee: General Electric CompanyInventors: Johan Adrianus Aarssen, Gerrit Op Den Dries, Ad Nieuwlaat, Marcel Vieveen, Rudy Francois Alain Joseph Peemans
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Patent number: 6002051Abstract: Novel compounds of the general formula ##STR1## wherein each R.sub.1 is independently a tertiary alkyl group containing from 4 to about 8 carbon atoms and each of X, Y and Z is independently hydrogen or a hydrocarbon-based group, provided at least one of X, Y and Z is an aliphatic hydrocarbon group containing at least 7 carbon atoms, and wherein R.sub.1 is different from the at least one of X, Y and Z that is an aliphatic hydrocarbon group containing at least 7 carbon atoms, R.sub.2 is an alkylene or alkylidene group, and n is a number ranging from zero to about 4. Also disclosed are methods for preparing novel phenolic compounds, organic compositions, including lubricants based on oils of lubricating viscosity and fuels based on normally liquid fuels and additive concentrates containing the novel phenolic compounds of this invention.Type: GrantFiled: October 16, 1992Date of Patent: December 14, 1999Assignee: The Lubrizol CorporationInventors: Louis Burjes, Calvin W. Schroeck
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Patent number: 5990362Abstract: A method for preparing bisphenol A is disclosed, with a selectivity for the p,p'-isomer of greater than about 97%. The method involves reacting phenol with p-isopropenylphenol or 2-(4-hydroxyphenyl)-2-propanol in the presence of a catalyst, at a reaction temperature of no greater than about 65.degree. C. The bisphenol A product is preferably purified by a technique which omits the use of adduct crystallization.Type: GrantFiled: August 31, 1998Date of Patent: November 23, 1999Assignee: General Electric CompanyInventors: Eric James Pressman, Joseph Richard Wetzel
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Patent number: 5986149Abstract: The present invention provides processes for recovering alkanols from fluids comprising the alkanol and aqueous hydrobromic acid without forming excessive amounts of alkyl bromide. In certain aspects of the invention, there are provided distillation systems wherein a fluid comprising an alkanol and aqueous hydrobromic acid is introduced into a distillation column at a point between the bottom and the top of the column to thereby separate the alkanol and the hydrobromic acid without causing the production of a significant amount of alkyl bromide.Type: GrantFiled: April 3, 1998Date of Patent: November 16, 1999Assignee: Great Lakes Chemical CorporationInventors: Richard J. DeGroot, James T. Ayers, Karl E. Reineke
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Patent number: 5959160Abstract: The invention relates to a process for the purification of p,p-bisphenolate solutions such as are obtained in the production of bisphenolates from soda lye and bisphenols by extraction.Type: GrantFiled: March 17, 1997Date of Patent: September 28, 1999Assignee: Bayer AGInventors: Claus Wulff, Kurt-Peter Meurer, Tony van Osselaer, Roelof Boyens, Jurgen Hinz
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Patent number: 5919990Abstract: The disclosure is of a process for recovering valuable by-products of the condensation of phenol and a ketone from a mother liquor obtained for example upon crystallization of a 1:1 adduct of phenol and bisphenol, said mother liquor containing phenol, bisphenol, isomers, contaminant by-products of the condensation reaction of phenol with the ketone and acidic impurities. The mother liquor is distilled/evaporated leaving a tarry residue, which is the feedstock for the process of the invention. The recovery comprises heating the feedstock with proportions of an arylamine salt, to extract the bisphenol-A values as aminophenylhydroxylphenyl-alkanes.Type: GrantFiled: October 20, 1997Date of Patent: July 6, 1999Assignee: General Electric CompanyInventor: Parfait J.M. Likibi
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Patent number: 5886198Abstract: Cyclic formal is manufactured by cyclic reaction of an alkylene glycol and an aldehyde in a reactor, producing formal mixed with unreacted aldehyde as an impurity, which impurity is reduced in amount by connecting the reactor to a distillation tower and continuously supplying alkylene glycol to the distillation tower from which unreacted formaldehyde and a cyclic formal are being distilled, and continuously reacting them with supplied raw formaldehyde by countercurrent flow during distillation; water content in azeotropic admixture with cyclic formal can be removed by azeotropic distillation with a hydrocarbon azeotropic mixture with water, distilling water from the cyclic formal.Type: GrantFiled: January 27, 1998Date of Patent: March 23, 1999Assignee: Toray Industries, Inc.Inventors: Daisuke Ogawa, Masahiro Koike, Yoshiyuki Yamamoto
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Patent number: 5874644Abstract: Methods/systems for making a relatively high-purity bisphenol A product from phenol and acetone. Controlled turbulence is used to form bisphenol A adduct solids having improved physical properties. Phenol is separated from the bisphenol A product while inhibiting decomposition of bisphenol A.Type: GrantFiled: April 12, 1996Date of Patent: February 23, 1999Inventor: Ben Gammill
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Patent number: 5874647Abstract: A zeolite catalyst for hydroxylating benzene to phenol is treated hydrothermally with a gas comprising approximately 1-100 mole percent water at a temperature between approximately 350.degree.-950.degree. C., and subsequently is treated with an acid. This treatment selectively removes aluminum species from the zeolite catalyst in a manner that increases catalyst stability in phenol production without reducing the activity of the catalyst.Type: GrantFiled: August 20, 1996Date of Patent: February 23, 1999Assignee: Solutia Inc.Inventors: William D. McGhee, Patrick P. B. Notte
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Patent number: 5851837Abstract: A method for making bisphenol salt as the result of the reaction between bisphenol and an alkali metal hydroxide. The method comprising steps to obtain the anhydrous alkali metal bisphenoxide salt within about a 0.2 mol % stoichiometry relationship between bisphenol and alkali metal hydroxide. A method for determining stoichiometry error of a sample comprises determining variables and applying the variables to an equation to determine stoichiometry.Type: GrantFiled: February 6, 1997Date of Patent: December 22, 1998Assignee: General Electric CompanyInventors: Edward Brittain Stokes, Thomas Link Guggenheim, James Marshall Finan
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Patent number: 5785823Abstract: A process for preparing bisphenol A which has a purity of at least 99.95 wt. % of p,p-bisphenol A (BPA). Thermally stable and colour-stable BPA purified in accordance with the invention produces improved thermal and colour stability and improved optical transparency in polymers such as e.g. polycarbonates prepared therefrom.Type: GrantFiled: August 2, 1996Date of Patent: July 28, 1998Assignee: Bayer AG Konzernverwaltung RPInventors: Kurt-Peter Meurer, Tony Van Osselaer, Werner Verhoeven, Johan Vaes, Ignace Hooftman, Willy Van Herck, Claus Wulff, Jurgen Hinz, Alfred Eitel, Kaspar Hallenberger
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Patent number: 5786522Abstract: An integrated process for the preparation and recovery of BPA in pure form utilizes a series of steps to crystallize pure BPA of improved color stability and recycle separated impurities to improve overall yields. The principal impurity recycled to the process is o,p-BPA which functions as a color stabilizer in the product and in polycarbonate resins prepared from the BPA.Type: GrantFiled: September 13, 1996Date of Patent: July 28, 1998Assignee: General Electric CompanyInventor: Michael J. Cipullo
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Patent number: 5783733Abstract: An integrated process for the preparation and recovery of a bisphenol based on the condensation reaction of a ketone and a phenol in the presence of an ion-exchange resin.Type: GrantFiled: June 13, 1996Date of Patent: July 21, 1998Assignee: General Electric CompanyInventor: Gaylord Michael Kissinger
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Patent number: 5756860Abstract: The invention relates to the preparation of a transparent crystalline adduct consisting of bisphenol A (75 parts) and bisphenol TMC (25 parts), which has a melting point of 144.degree. C. which is below the melting points of the pure starting compounds bisphenol A (157.degree. C.) and bisphenol TMC (208.degree. C.).Type: GrantFiled: August 2, 1996Date of Patent: May 26, 1998Assignee: Bayer AktiengesellschaftInventors: Kurt-Peter Meurer, Tony Van Osselaer, Claus Wulff, Jurgen Hinz
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Patent number: 5723693Abstract: A process for preparing a 4,4'-dihydroxy-alpha-alkylstilbene or 4,4'-dihydroxy-alpha,alpha'-dialkylstilbene which includes the steps of (A) reacting at a temperature of from -20.degree. C. to 20.degree. C. a mixture of: (1) at least one alpha-haloketone; (2) at least one compound containing one phenolic hydroxyl group or aromatic alkoxy group per molecule such that the mole ratio of phenolic hydroxyl group-containing or aromatic alkoxy group-containing compound(s):alpha-haloketone(s) is at least 0.Type: GrantFiled: September 13, 1996Date of Patent: March 3, 1998Assignee: The Dow Chemical CompanyInventors: Robert E. Hefner, Jr., David A. Carr
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Patent number: 5723688Abstract: A process for preparing an adduct of a bisphenol with a phenolic compound comprising the following steps:a) reacting a carbonyl compound with a stoichiometric excess of a phenolic compound in the presence of an acidic cation exchange resin as a catalyst, to produce a product mixture containing a bisphenol, unreacted phenolic compound, unreacted carbonyl compound and water, andb) crystallizing an adduct of the bisphenol with the phenolic compound from the product mixture in a crystallization device in the presence of water and acetone.The product mixture obtained in step a) is not subjected to a distillation step before the product mixture enters the crystallization device and prior to the crystallization step b) the content of the carbonyl compound in the product mixture is controlled and, if necessary, carbonyl compound is added such that the total concentration of the carbonyl compound is from about 0.1 to about 8 percent, based on the total weight of the product mixture.Type: GrantFiled: November 15, 1995Date of Patent: March 3, 1998Assignee: The Dow Chemical CompanyInventors: Emil Patrascu, Johann Wilhelm Frey, Hartwig Sendner
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Patent number: 5723689Abstract: A method for recovering substantially pure p,p-bisarylols from a mixture comprising the same by subjecting the mixture to vacuum distillation and melt crystallization in the absence of an adduct crystallization and the generation of a reaction recycle stream.Type: GrantFiled: January 16, 1996Date of Patent: March 3, 1998Assignee: General Electric CompanyInventors: Eric James Pressman, Sheldon Jay Shafer, Joseph Richard Wetzel, Martin Herke Oyevaar
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Patent number: 5723690Abstract: This invention relates to a process for the production of tetrabromobisphenol-A by the bromination of bisphenol-A, which process features: a water and water miscible solvent reaction medium; a relatively high reaction temperature; the presence, in the reaction medium, of unreacted Br.sub.2 during the feed of bisphenol-A to the reactor; and the oxidation of co-produced HBr to yield Br.sub.2.Type: GrantFiled: October 30, 1995Date of Patent: March 3, 1998Assignee: Albemarle CorporationInventor: Bonnie G. McKinnie
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Patent number: 5710347Abstract: This invention relates to a method of producing a high-melting powder of 2,2-bis?4'-(2",3"-dibromopropoxy)-3',5'-dibromophenyl!propane characterized by comprising a step of adding water to a solution of 2,2-bis?4'-(2",3"-dibromopropoxy)-3',5'-dibromophenyl!-propane in an organic solvent in the presence of a surfactant to give a water-in-oil emulsion and a step of removing the organic solvent from the emulsion in the presence of a crystal nucleus to induce crystallization to give an aqueous dispersion of 2,2-bis?4'-(2",3"-dibromopropoxy)-3',5'-dibromophenyl!propane. In accordance with this invention, crystallization is carried out in the state of an emulsion under assistance of a surfactant so that an ordinary stirrer can be used in production without resort to any special high-shear stirring equipment. Moreover, since a high-melting grade of 2,2-bis?4'-(2",3"-dibromopropoxy)-3',5'-dibromophenyl!propane is obtained as an aqueous dispersion, workability and safety in the subsequent processing are improved.Type: GrantFiled: September 26, 1995Date of Patent: January 20, 1998Assignee: Dai-Ichi Kogyo Seiyaku Co., Ltd.Inventors: Setsuo Nishibori, Hideaki Ohnishi, Tsuyoshi Furukawa
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Patent number: 5705714Abstract: An improved process for the purification of solid dihydric phenol, preferably bisphenol-A recovered from a polymer containing the reaction residue of dihydric phenol units in the polymer structure by essentially dry distilling dihydric phenol in the presence of about 0.005 to about 0.05 weight percent of hypophosphorous acid based on the weight of dihydric phenol.Type: GrantFiled: July 1, 1996Date of Patent: January 6, 1998Assignee: General Electric CompanyInventor: Srikanth Nanguneri
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Patent number: 5696295Abstract: The invention relates to a method for the purification by distillation of p,p-bisphenol A from the melt.The p,p-bisphenol A melt thus obtained is highly heat-stable, stable in storage and colour-stable, is free from high-boiling components and no longer contains any surface-active or non-distillable metal, salt, acid or polymer components and no sulphur-containing components; o,p-BPA and phenol are removed and the low-boiling components are scarcely detectable.Type: GrantFiled: April 6, 1995Date of Patent: December 9, 1997Assignee: Bayer AGInventors: Claus Wulff, Kaspar Hallenberger, Heinrich Steude, Kurt-Peter Meurer, Tony van Osselaer, Jurgen Hinz, Frank Quaeyhaegens, Johan Vaes, Ignace Hooftman
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Patent number: 5675044Abstract: A method of recovering dihydric phenol, particularly bisphenol-A, from compositions containing the reaction residue of bisphenol-A units which method comprises:a. granulating a bisphenol-A containing polymer;b. treating the particles with an alcohol, or any other organic swelling solvent miscible with water and easily distilled off from an aqueous solution, preferably a C.sub.1 -C.sub.10 alcohol for a time sufficient to swell the particles;c. contacting the swelled particles with a ammoniacal solution at a temperature of at least about 25.degree. C. depending on the swelling solvent employed in order to selectively sever the ester bonds of the bisphenol-A residue units;d. separating the liquid phase from the solid phase;e. distilling ammonia and swelling solvent from the liquid phase of d. above, thus obtaining an essentially aqueous solution with dissolved urea and partially precipitated bisphenol-A;f. adding sufficient water to the residue of e.Type: GrantFiled: July 1, 1996Date of Patent: October 7, 1997Assignee: General Electric CompanyInventors: Paul Eijsbouts, Jos De Heer, Gabrie Hoogland, Srikanth Nanguneri, Gert De Wit
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Patent number: 5663456Abstract: The present invention provides a method, which can be operated continuously and has a wide scope of application, for destructing part of fines in slurry in a crystallizer to obtain large crystals having high purity and large crystal size, characterized in that first and second filters are installed in the crystallizer, a part of slurry containing only fines of size smaller than the fines cut size is drawn from the crystallizer, through the first filter in the crystallizer to a fines destruction loop for destructing the fines and then to the crystallizer through the second filter in the crystallizer by using a circulating pump. The two filters are switched over at regular interval and washed with each other's effluent to ensure the cintinuous operation of the above process.The present invention also provides a method for preparing crystalline bisphenol A/phenol adduct and bisphenol A with high purity and large crystal size.Type: GrantFiled: December 26, 1995Date of Patent: September 2, 1997Assignees: China Petro-Chemical Corporation, Tianjin UniversityInventors: Minhua Zhang, Zongzhang Liu, Shenbo Yu, Chuanzhao Li, Shenghua Qian
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Patent number: 5648561Abstract: High purity and ultrapure bisphenol A is prepared in a novel process.Type: GrantFiled: October 11, 1995Date of Patent: July 15, 1997Assignees: China Petro-Chemical Corporation, Tianjin UniversityInventors: Qiu Tan, Minhua Zhang, Shenbo Yu, Zongzhang Liu, Shenghua Qian, Chuanzhao Li
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Patent number: 5629457Abstract: A process for producing high-quality polycarbonate grade bisphenol A directly by removing phenol from the adduct crystal of bisphenol A with phenol via a gas-solid reaction at low temperature comprises directly feeding the adduct crystal into a vacuum or pneumatic dephenolizing device under vacuum a inert gas stream, controlling the temperature of the adduct crystal below its melting point, decomposing the adduct crystal into gas phase and solid phase, removing the gas phase phenol and condensing phenol for recovery, well leaving the rest being the desirable bisphenol A. The process possesses easy operation, short procedure, low energy consumption, and high purity and good color of bisphenol A obtained. Bisphenol A produced according to the process of the invention may be used as the raw material for producing polycarbonates for optical use.Type: GrantFiled: September 29, 1995Date of Patent: May 13, 1997Assignees: Tianjin University, China Petro-Chemical CorporationInventors: Minhua Zhang, Zongzhang Liu, Shenbo Yu, Shenghua Qian, Chuanzhao Li
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Patent number: H1943Abstract: A process for producing a dihydric phenol preferably bisphenol-A consisting of the steps of (1) formulating reaction ingredients of phenol, acetone, recycle bisphenol A, impurities, an acid catalyst and water, (2) reacting the ingredients to form a product mix consisting of bisphenol-A, unreacted phenol, by-products, acetone and water, (3) crystallizing the product mix forming a slurry of bisphenol-A/phenol adduct crystals solid phase, (4) separating the solid phase from the liquid phase by filtration, (5) removing the phenol from the bisphenol-A/phenol adduct to obtain a crude bisphenol-A, and (6) purifying the crude bisphenol by fractional melt crystallization to obtain a bisphenol-A of at least 99.5% purity.Type: GrantFiled: December 15, 1998Date of Patent: February 6, 2001Assignee: General Electric Co.Inventors: Gaylord M. Kissinger, Ryozo Sato