Processes Patents (Class 556/466)
  • Patent number: 5616755
    Abstract: The present invention relates to a process for preparing low-chloride or chloride-free aminofunctional organosilanes by reacting chlorofunctional organosilanes with organic amines or ammonia and separating off the organic hydrochlorides or ammonium chloride thus formed, wherein further amounts of organic hydrochlorides or ammonium chloride present are reacted by addition of metal alkoxides dissolved in alcohols and the metal chlorides formed are separated off, and also to aminofunctional organosilanes prepared thereby.
    Type: Grant
    Filed: September 14, 1995
    Date of Patent: April 1, 1997
    Assignee: Huels Aktiengesellschaft
    Inventors: Claus-Dietrich Seiler, Hartwig Rauleder, Hans-Joachim Koetzsch, Hans-Guenther Srebny
  • Patent number: 5608097
    Abstract: The present invention relates to a process for preparation of silane compound represented by general formula (I) of which one or two hydrogens have been substituted, comprising a reaction of silane compound represented by general formula (II) with trichlorosilane in the presence of metal or metal compound as a catalyst. ##STR1## whereby, R.sup.1, R.sup.2 and R.sup.3 respectively represent chlorine or methyl group, and Z and Z' respectively represent hydrogen or chlorine, and as a result, the process of the present invention is industrially useful because trichlorosilane having relatively low price is employed.
    Type: Grant
    Filed: May 1, 1996
    Date of Patent: March 4, 1997
    Assignee: Korea Institute of Science and Technology
    Inventors: Il N. Jung, Eun J. Cho, Joon S. Han, Yon S. Cho
  • Patent number: 5576453
    Abstract: Compositions of Formula (I): ##STR1## wherein R is a group selected in accordance with an intended application; R.sub.1 and R.sub.2 are protecting groups; and P is a substrate are provided. Methods of producing these compositions are also provided.
    Type: Grant
    Filed: July 18, 1994
    Date of Patent: November 19, 1996
    Assignee: ES Industries
    Inventor: Mark A. Buese
  • Patent number: 5569775
    Abstract: A process for separating dimethyldichlorosilane from methyltrichlorosilane in a mixture. The process comprises contacting a mixture comprising methyltrichlorosilane and dimethyldichlorosilane with silica gel, where the dimethyldichlorosilane is selectively retained by the silica gel. The process provides for the recovery of a methyltrichlorosilane fraction reduced in dimethyldichlorosilane concentration. The present process is especially useful for removing low levels of dimethyldichlorosilane present as a contaminate in methyltrichlorosilane.
    Type: Grant
    Filed: November 29, 1995
    Date of Patent: October 29, 1996
    Assignee: Dow Corning Corporation
    Inventors: Michael Diaz, Roland L. Halm, Michael A. McIntyre, Oliver K. Wilding
  • Patent number: 5567836
    Abstract: A process for separating methyltrichlorosilane from dimethyldichlorosilane in a mixture. The process comprises contacting a mixture comprising methyltrichlorosilane and dimethyldichlorosilane with activated carbon, where the methyltrichlorosilane is selectively adsorbed by the activated carbon. The process allows for the recovery of a dimethyldichlorosilane fraction reduced in methyltrichlorosilane concentration. The methyltrichlorosilane can be recovered by desorption from the activated carbon. The present process is especially useful for removing low levels of methyltrichlorosilane present as a contaminate in dimethyldichlorosilane.
    Type: Grant
    Filed: November 29, 1995
    Date of Patent: October 22, 1996
    Assignee: Dow Corning Corporation
    Inventors: Michael Diaz, Roland L. Halm, Michael A. McIntyre, Oliver K. Wilding
  • Patent number: 5550260
    Abstract: A process for the production of a cyclopentenol compound represented by the formula I: ##STR1## wherein R.sub.1 represents a 2-propenyl group or a 2-propynyl group from a cyclopentenolone compound represented by the formula II: ##STR2## by protecting the hydroxyl group of the compound II, reacting the protected compound II with a reagent system obtained from TiCl.sub.4, Zn and CH.sub.2 Br.sub.2 or CH.sub.2 I.sub.2 and removing the protecting group from the resulting reaction product.
    Type: Grant
    Filed: June 2, 1994
    Date of Patent: August 27, 1996
    Assignee: Sumitomo Chemical Company, Limited
    Inventors: Kazunori Tsushima, Tomonori Iwasaki, Masaya Suzuki, Noritada Matsuo
  • Patent number: 5545743
    Abstract: An improved process for the heat-fractionation of a mixture comprising an organosilane and a borane or borane forming compound. The improvement comprises the presence of a tertiary organoamine or tertiary phosphorous compound at a concentration sufficient to reduce modification of the organosilane during the heat-fractionation process.
    Type: Grant
    Filed: November 2, 1995
    Date of Patent: August 13, 1996
    Assignee: Dow Corning Corporation
    Inventors: John P. Cannady, John M. Gohndrone, Ming-Shin Tzou
  • Patent number: 5543540
    Abstract: A process for producing compounds of the formula (CH.sub.3).sub.3 SiORLi, wherein R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms, by reacting, optionally in the presence of a catalyst, in an inert atmosphere, a haloalcohol of the formula HORX, wherein R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms and X is selected from chlorine or bromine, is reacted with neat hexamethyldisilazane at a temperature between 20.degree. C. and 200.degree. C., optionally in the presence of a catalyst, after which the resulting product, a trimethylsilyloxyalkylhalide compound, is reacted at a temperature between 50.degree. C. and 160.degree. C., with powdered lithium metal, in an inert hydrocarbon medium, to produce the (CH.sub.3).sub.3 SiORLi compound.
    Type: Grant
    Filed: November 21, 1994
    Date of Patent: August 6, 1996
    Assignee: FMC Corporation
    Inventor: James A. Schwindeman
  • Patent number: 5523447
    Abstract: A process for preparing easily separable solutions of organolithium compounds comprising the steps of reacting lithium metal, in the form of cast or extruded ingots or pieces cut therefrom, with an organo halide in mole ratios ranging from 3:1 to 20:1 in a solvent selected form a group of liquid hydrocarbons, alkyl ethers, and mixtures thereof under an inert atmosphere for one to ten hours with moderate stirring, cooling the resulting product, and separating the solution of the organolithium compound from the reacted lithium metal and by-product lithium chloride in the reactor.
    Type: Grant
    Filed: June 7, 1995
    Date of Patent: June 4, 1996
    Assignee: FMC Corporation
    Inventors: Conrad W. Kamienski, James A. Schwindeman, B. Troy Dover, Robert C. Morrison
  • Patent number: 5516871
    Abstract: There is disclosed a diphenylsiloxane oligomer functionalized at both terminals and methods for the preparation thereof, said oligomer having the following general formulaG-(OSiPh.sub.2).sub.m O-G (i)wherein Ph denotes a phenyl radical, m is 3 to 50 and G has a formula independently selected from the group consisting of ##STR1## in which R, R.sup.4 and R.sup.5 are independently selected from the group consisting of methyl, phenyl and R.sup.1, R.sup.1 is selected from the group consisting of hydrogen and a monovalent hydrocarbon group having 2 to 8 carbon atoms excluding phenyl, tolyl, xylyl, and ethylphenyl radicals, Q is a divalent hydrocarbon group and k is independently 0 to 3 at each terminus of said oligomer with the proviso that k is >0 at one terminus of said oligomer, at least one substituent among R, R.sup.4 and R.sup.5 in formula (ii) is R.sup.1 and, when both R.sup.4 and R.sup.5 groups at one terminus of said oligomer are phenyl, groups R.sup.4 and R.sup.
    Type: Grant
    Filed: March 21, 1995
    Date of Patent: May 14, 1996
    Assignee: Dow Corning Asia, Ltd.
    Inventors: Brian R. Harkness, Mamoru Tachikawa
  • Patent number: 5493042
    Abstract: A process for treating a by-product stream, resulting from the commercial manufacture of methylchlorosilanes, to remove residual silanes where the residual silanes comprise low-boiling hydrosilanes. The process comprises a first step where the by-product stream is contacted with hydrogen chloride in the presence of a chlorination catalyst to convert the low-boiling hydrosilanes to chlorosilanes. In a second step, the modified by-product stream comprising the chlorosilanes is contacted with activated carbon which adsorbs higher-boiling silanes including chlorosilanes, thereby forming a final by-product stream reduced in lower-boiling hydrosilanes and in total silanes. The present process is especially useful for removing silanes from by-product streams intended for incineration, thus reducing silica during combustion of the by-product stream in the incinerator.
    Type: Grant
    Filed: June 15, 1995
    Date of Patent: February 20, 1996
    Assignee: Dow Corning Corporation
    Inventors: Andrew L. Ault, David H. Bramer, Steven K. Freeburne
  • Patent number: 5493038
    Abstract: A process for quickly preparing easily separable solutions of lithium alkylamides, as exemplified by the formula(R.sub.3 M).sub.x NLi(R1).sub.y.(LB).sub.z (I)wherein M is silicon or carbon, R and R.sup.1 are C.sub.1 -C.sub.8 alkyl, cycloalkyl or alkylene groups, LB is a Lewis base, x and y are integers equaling 2, and z is greater than 1, comprising the steps of reacting lithium metal in bulk form with an alkylamine in mole ratios of metal to alkylamine ranging from 2 to 1 to 10 to 1 in a solvent selected from ethereal or selected from the group consisting of conjugated dienes, vinyl aromatic and polycyclic aromatic compounds, under an inert atmosphere at elevated temperatures for 1 to 10 hours, cooling the product and separating the product solution from the unreacted lithium metal in the reactor.
    Type: Grant
    Filed: March 2, 1994
    Date of Patent: February 20, 1996
    Assignee: FMC Corporation
    Inventors: Randy W. Hall, Conrad W. Kamienski, Robert C. Morrison, John F. Engel
  • Patent number: 5491250
    Abstract: A crude vinylically unsaturated product formed from a palladium-complex-catalyzed reaction of a reactant halide selected from the group consisting of aryl, allyl, vinyl, and benzyl halides, and a reactant olefin having a vinylic hydrogen, wherein the reaction is carried out in the presence of a hydrogen halide acceptor, is purified by first contacting the crude product with a base that is stronger than the hydrogen halide acceptor, then heating the stronger base-contacted product. The purified product shows a marked reduction in concentration bromine and palladium impurities. The product can then be further purified by such methods as chromatography, crystallization, or distillation to achieve a product that is more suitable for applications where very low levels of inorganic impurities are required.
    Type: Grant
    Filed: March 23, 1995
    Date of Patent: February 13, 1996
    Assignee: The Dow Chemical Company
    Inventors: Edmund J. Stark, John A. Schultz, Ernest L. Ecker, Robert A. DeVries
  • Patent number: 5476916
    Abstract: The present invention describes a process wherein dimethyldichlorosilane is reacted, in a first step, with water present in hydrochloric acid to give a crude hydrolysate comprising cyclic and linear, chlorine-containing polydimethylsiloxanes and gaseous hydrogen chloride and, in a second step, the crude hydrolysate is treated with steam to reduce the chlorine content and form hydrochloric acid, with the hydrochloric acid formed in the second step being used in the first step.
    Type: Grant
    Filed: November 29, 1994
    Date of Patent: December 19, 1995
    Assignee: Wacker-Chemie GmbH
    Inventors: Bernd Pachaly, Gerhard Nagy, Wolfgang Jacques, Robert Christa
  • Patent number: 5476958
    Abstract: In the process for the removal of olefins from the silanes or silane mixtures obtained during methylchlorosilane synthesis, the olefins are reacted with hydrogen in the presence of hydrogenation catalysts.
    Type: Grant
    Filed: April 6, 1995
    Date of Patent: December 19, 1995
    Assignee: Wacker-Chemie GmbH
    Inventors: Konrad Mautner, Anton Schinabeck
  • Patent number: 5474716
    Abstract: Disclosed are processes for the preparation of new bridged cyclopentadienylmagnesium compounds of the general formula Q(CpR.sub.a)(Cp'R'.sub.a ')Mg, and the use thereof for preparing bridged metallocenes.
    Type: Grant
    Filed: February 22, 1995
    Date of Patent: December 12, 1995
    Assignee: Witco GmbH
    Inventor: Richard Lisowsky
  • Patent number: 5453221
    Abstract: Disclosed are new bridged cyclopentadienylmagnesium compounds of the general formula Q(CpR.sub.a) (Cp'R'.sub.a')Mg, processes for the preparation thereof, and the use thereof for preparing bridged metallocenes.
    Type: Grant
    Filed: February 22, 1995
    Date of Patent: September 26, 1995
    Assignee: Witco GmbH
    Inventor: Richard Lisowsky
  • Patent number: 5436361
    Abstract: A process for synthesizing enediynes is provided. Specifically, the formed enediynes contain a hex-3-ene-1,5-diynyl group. Production of the enediynes involves adding a base to a propargylic halide in the presence of a chelating agent, which causes a carbenoid coupling-elimination sequence of the propargylic halides. A carbenoid destabilizing agent can also be added to the reaction mixture in order to enhance yield. Acyclic and cyclic enediynes can be synthesized according to this process. The enediynes are useful compounds that can be used in a variety of applications including use in the production of anti-tumor agents.
    Type: Grant
    Filed: April 22, 1994
    Date of Patent: July 25, 1995
    Assignee: Clemson University
    Inventors: Graham B. Jones, Robert S. Huber
  • Patent number: 5403946
    Abstract: A process for producing compounds of the formula (CH.sub.3).sub.3 SiORLi where in R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms by reacting, in an inert atmosphere, in a hydrocarbon solvent, a haloalcohol of the formula HORX wherein R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms and X is selected from chlorine or bromine, is reacted with hexamethyldisilazane at a temperature between 20.degree. C. and the reflux temmperature of the solvent after which the resulting product, a trimethylsilyloxyalkylhalide compound, is reacted at a temperature between 50.degree. and 160.degree. C., with powdered lithium metal to produce the (CH.sub.3).sub.3 SiORLi compound.
    Type: Grant
    Filed: July 25, 1994
    Date of Patent: April 4, 1995
    Assignee: FMC Corporation
    Inventor: James A. Schwindeman
  • Patent number: 5399290
    Abstract: A compound of the general formulaM--(CH.sub.2).sub.n --(O).sub.m --[--D--B--].sub.q --Y, (I)in which M represents a silicon radical having 2 to 5 silicon atoms which are linked together by bridging elements A, and the remaining valencies of the silicon atoms are saturated with radicals R; A is a bridging element selected from the group consisting of C.sub.1 - to C.sub.8 -alkylene radicals and oxygen with the proviso that at least one radical A per M radical is a C.sub.1 - to C.sub.8 -alkylene radical; R represents optionally fluorine or chlorine atom- or cyano group-substituted straight-chain C.sub.1 - to C.sub.10 -alkyl or C.sub.2 - to C.sub.10 -alkenyl radicals, branched chain C.sub.3 - to C.sub.10 -alkyl or C.sub.3 - to C.sub.10 -alkenyl radicals, optionally C.sub.1 - to C.sub.4 -alkyl- , C.sub.1 - to C.sub.4 -alkoxy radicals, fluorine, chlorine, bromine atom, cyano, trifluoromethyl or nitro radical substituted C.sub.6 - to C.sub.12 -cycloalkyl, C.sub.6 - to C.sub.12 -cycloalkenyl, C.sub.6 - to C.sub.
    Type: Grant
    Filed: December 2, 1992
    Date of Patent: March 21, 1995
    Assignee: Consortium fur elektrochemische Industrie GmbH
    Inventors: Norman Haberle, Franz-Heinrich Kreuzer, Benno Krueger, Ingo Zahn
  • Patent number: 5347026
    Abstract: A Process is disclosed comprising reacting an alkali metal salt of Z with MX.sub.4 to form a trihalo compound; reacting the trihalo compound with an alkali metal salt of Z' to form a dihalo compound; and reacting the dihalo compound with at least one alkali metal organic compound to form Z-MR.sub.2 -Z', where Z is a substituted or unsubstituted fluorenyl radical, M is Ge, Si, or Sn, X is Cl, Br, F, or I, each R is a hydrocarbyl radical containing 1 to 20 carbon atoms, and Z' is an unsubstituted cyclopentadienyl, substituted cyclopentadienyl, unsubstituted indenyl, substituted indenyl, unsubstituted fluorenyl, or a substituted fluorenyl. Also new fluorene compounds are disclosed.
    Type: Grant
    Filed: June 11, 1993
    Date of Patent: September 13, 1994
    Assignee: Phillips Petroleum Company
    Inventors: Konstantinos Patsidis, H. G. Alt, Syriac J. Palackal
  • Patent number: 5336799
    Abstract: Silanes containing hydrogen atoms bonded directly to silicon produced as by-products during methylchlorosilane synthesis are reacted with chlorohydrocarbons in the presence of palladium or platinum as catalysts to give the corresponding chlorosilanes.
    Type: Grant
    Filed: November 1, 1993
    Date of Patent: August 9, 1994
    Assignee: Wacker-Chemie GmbH
    Inventors: Wilfried Kalchauer, Bernd Pachaly
  • Patent number: 5326896
    Abstract: The present invention is a process for converting a high-boiling component resulting from the reaction of an organochloride with silicon into commercially more desirable monosilanes. The process comprises contacting the high-boiling component with hydrogen gas at a temperature within a range having a lower limit greater than 250.degree. C. and an upper limit of 1000.degree. C. Yield of the present process may be improved by use of a catalyst selected from a group consisting of activated carbon, platinum metal, platinum supported on alumina, palladium supported on carbon, SbCl.sub.5, H.sub.2 PtCl.sub.6, BCl.sub.3, AlCl.sub.3, and AlCl.sub.3 supported on a support material selected from a group consisting of carbon, alumina, and silica. In a preferred embodiment of the present process the process is run at a pressure within a range of about 250-1000 psig. The present process is preferential for the production of diorganodichlorosilane in relation to organotrichlorosilane in the monosilane product.
    Type: Grant
    Filed: July 14, 1993
    Date of Patent: July 5, 1994
    Assignee: Dow Corning Corporation
    Inventors: Kirk M. Chadwick, Ajay K. Dhaul, Roland L. Halm, Richard G. Johnson
  • Patent number: 5321148
    Abstract: A process for preparing functionalized alkyllithium compounds comprising reacting a fine particle size lithium metal of not more than 300 microns average particle size with an organosiloxyalkyl halide of the formula R.sup.1 R.sup.2 R.sup.3 SiORX wherein R.sup.1, R.sup.2 and R.sup.3 are independently selected from alkyl groups containing 1 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms, R is selected from alkyl groups containing 1 to 8 carbon atoms either straight chain or substituted by alkyl or aryl groups, X is selected from chlorine or bromine, the reaction temperature is above 50.degree. C., the reaction medium is a hydrocarbon solvent and the reaction is conducted in an inert atmosphere.
    Type: Grant
    Filed: December 30, 1993
    Date of Patent: June 14, 1994
    Assignee: FMC Corporation
    Inventor: James A. Schwindeman
  • Patent number: 5321147
    Abstract: The present invention is a process for converting a high-boiling component resulting from the reaction of an organochloride with silicon into commercially more desirable monosilanes. The process comprises contacting the high-boiling component with chlorine at a temperature within a range of about 250.degree. C. to 1000.degree. C. Improved yield of monosilanes can be obtained in the process by the use of a catalyst selected from a group consisting of alumina, silica. activated carbon, AlCl.sub.3, and AlCl.sub.3 supported on a support selected from a group consisting of alumina, silica, and carbon.
    Type: Grant
    Filed: July 16, 1993
    Date of Patent: June 14, 1994
    Assignee: Dow Corning Corporation
    Inventors: Kirk M. Chadwick, Ajay K. Dhaul, Roland L. Halm, Richard G. Johnson, Robert D. Steinmeyer
  • Patent number: 5317072
    Abstract: The present invention is a process for the preparation of organofunctional-terminated polydiorganosiloxane polymers and organofunctional polydiorganosiloxane copolymers. The process comprises reacting a hydroxyl-terminated polydiorganosiloxane polymer with: (1) an organofunctional chlorosilane end-blocker to form an organofunctional terminated polydiorganosiloxane polymer and (2) a mixture of organochlorosilane end-blocker and organofunctional dichlorosilane to form an organofunctional polydiorganosiloxane copolymer. The process can be conducted in the presence of an aqueous solution of hydrogen chloride, where the water is present in stoichiometric excess in relation to the hydrolyzable silicon-bonded chlorine.The present process is particularly useful for producing 5-hexenyl-terminated polydimethylsiloxane polymers and for producing siloxane copolymers comprising poly-5-hexenylmethylsiloxy and polydimethylsiloxy blocks.
    Type: Grant
    Filed: July 31, 1992
    Date of Patent: May 31, 1994
    Assignee: Dow Corning Corporation
    Inventors: Gary N. Bokerman, David E. Puckett, Larry H. Wood
  • Patent number: 5302736
    Abstract: The present invention is a process wherein silanes containing hydrogen atoms bonded directly to silicon are removed from silanes of the general formulaR.sub.x Cl.sub.3-x Si--[SiR.sub.y Cl.sub.2-y ].sub.n --A (I)and mixtures thereof, in which R denotes an optionally halogen-substituted hydrocarbon radical having 1 to 18 carbon atoms which is free from ethylenic double bonds, A denotes a chlorine atom or a radical R, x has the value of 0, 1, 2 or 3, y has the value of 0, 1 or 2 and n has the value of 0 or 1. The silanes containing hydrogen atoms bonded directly to silicon are reacted with hydrogen chloride in the presence of silver or gold as catalysts to give the corresponding chlorosilanes.
    Type: Grant
    Filed: November 1, 1993
    Date of Patent: April 12, 1994
    Assignee: Wacker-Chemie GmbH
    Inventors: Wilfried Kalchauer, Bernd Pachaly
  • Patent number: 5300614
    Abstract: Chloromethyltrichlorosilane is converted to polychlorocarbosilane and in turn to a polycarbosilane polymer that has utility as a precursor to silicon carbide ceramics.
    Type: Grant
    Filed: December 22, 1992
    Date of Patent: April 5, 1994
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Michael J. Michalczyk
  • Patent number: 5300608
    Abstract: The present invention relates to a process for preparing an alkoxy silyl-terminated material, which has at least one alkoxy group on at least one terminal end, said process comprising reacting in the presence of a catalytically effective amount of an organo-lithium reagent an alkoxysilyl-terminated first reactant with a second reactant having at least one end of its chain terminating in silanol groups. The alkoxy silyl-terminated material may have a variety of polymer backbone types such as silicone, polyurethane, polyamide and the like. These materials are intended to cure by either moisture cure or by dual moisture and photo cure mechanisms. The alkoxy silyl-terminated material is preferably an organopoly-siloxane having alkoxy groups at its terminal ends. The resultant alkoxy-terminated organopolysiloxanes are substantially stable materials as measured by preservation and maintenance of viscosity values (cps) over time.
    Type: Grant
    Filed: February 19, 1993
    Date of Patent: April 5, 1994
    Assignee: Loctite Corporation
    Inventors: Hsien-Kun Chu, Robert P. Cross, Patrick J. Courtney, David I. Crossan
  • Patent number: 5292909
    Abstract: The present invention is a process for converting a high-boiling component resulting from the reaction of an organochloride with silicon into commercially more desirable monosilanes. The process comprises contacting the high-boiling component with hydrogen chloride and hydrogen gas at a temperature within a range of about 250.degree. C. to 1000.degree. C. in the presence of a catalyst selected from a group consisting of activated carbon, alumina, silica, zeolite, AlCl.sub.3, AlCl.sub.3 supported on a support selected from a group consisting of carbon, silica, and alumina; platinum supported on a support selected from a group consisting of carbon, silica, and alumina; and palladium supported on a support selected from a group consisting of carbon, silica, and alumina.
    Type: Grant
    Filed: July 14, 1993
    Date of Patent: March 8, 1994
    Assignee: Dow Corning Corporation
    Inventors: Kirk M. Chadwick, Ajay K. Dhaul, Roland L. Halm, Richard G. Johnson
  • Patent number: 5292912
    Abstract: The present invention is a process for converting a high-boiling component resulting from the reaction of an organochloride with silicon into commercially more desirable monosilanes. The process comprises contacting the high-boiling component with hydrogen chloride at a temperature within a range of about 250.degree. C. to 1000.degree. C. in the presence of a catalyst selected from a group consisting of activated carbon, platinum supported on alumina, zeolite, AlCl.sub.3, and AlCl.sub.3 supported on a support selected from a group consisting of carbon, alumina, and silica.
    Type: Grant
    Filed: July 19, 1993
    Date of Patent: March 8, 1994
    Assignee: Dow Corning Corporation
    Inventors: Kirk M. Chadwick, Ajay K. Dhaul, Roland L. Halm, Richard G. Johnson
  • Patent number: 5290901
    Abstract: The present invention is a method for the preparation of carbinol-functional organosiloxanes and carbinol-functional organosiloxane resins. The method comprises contacting a cyclic silyl ether with an organosiloxane or an organosiloxane resin at a temperature within a range of about 25.degree. C. to 150.degree. C. The method may be conducted in the presence of an inert organic solvent to facilitate dissolution and contact of the reactants.
    Type: Grant
    Filed: June 14, 1993
    Date of Patent: March 1, 1994
    Assignee: Dow Corning Corporation
    Inventors: Gary T. Burns, Gary T. Decker, Aroop K. Roy
  • Patent number: 5288892
    Abstract: A process for separating methylchlorosilanes from high boiling residues from the methylchlorosilane synthesis, in which cleavable methylchlorodisilanes which are present in the residues and which have at least two chlorine atoms attached to one silicon atom are cleaved with hydrogen chloride in the presence of a catalyst which remains in the reaction mixture, which comprises cleaving the methylchlorodisilanes in the presence of by-products which are more volatile than the cleavable methylchlorodisilanes in the high boiling residues from the methylchlorosilane synthesis which have a boiling point of at least 70.degree. C. under normal conditions and continuously removing the more volatile by-products from the reaction mixture along with the methylchlorosilanes and the noncleavable methylchlorodisilanes.
    Type: Grant
    Filed: April 19, 1993
    Date of Patent: February 22, 1994
    Assignee: Wacker-Chemie GmbH
    Inventors: Bernd Pachaly, Anton Schinabeck
  • Patent number: 5262556
    Abstract: The invention relates to a process for the reaction of fluorinated or chlorinated aromatics with electrophiles at the ortho position relative to the fluorine or chlorine atom, characterized in that a strong base is added to a mixture of the fluorinated or chlorinated aromatic and the electrophile.
    Type: Grant
    Filed: May 6, 1992
    Date of Patent: November 16, 1993
    Assignee: Merck Patent Gesellschaft mit beschrankter Haftung
    Inventors: Bernard Riefling, Jurgen Seubert, Volker Reiffenrath, Reinhard Hittich
  • Patent number: 5260470
    Abstract: A method of purifying alkoxysilanes contaminated by organosilicon compounds with hydrolyzable chlorine atoms is disclosed wherein the alkoxysilanes are reacted in a pressure reactor with an alcohol, preferably in the presence of an HCl acceptor, at a temperature of 5.degree. C. to 160.degree. C. above the boiling point of the alcohol used and at the pressure which develops in the reactor.
    Type: Grant
    Filed: September 2, 1992
    Date of Patent: November 9, 1993
    Assignee: Degussa Aktiengesellschaft
    Inventors: Thomas Goebel, Peter Panster, Werner Will, Peter Kleinschmit
  • Patent number: 5247043
    Abstract: Low-molecular-weight phenylpolysilsesquioxanes that have narrow molecular weight distribution and a method for the preparation of the same.
    Type: Grant
    Filed: July 24, 1992
    Date of Patent: September 21, 1993
    Assignee: Dow Corning Toray Silicone Co., Ltd.
    Inventor: Hisataka Nakashima
  • Patent number: 5247045
    Abstract: The present invention is novel chlorine end-terminated organosiloxanes and a hydrosilylation process for their preparation. The process comprises contacting a chlorine end-terminated (organohydrogen)siloxane and an .alpha.-olefin in the presence of a platinum catalyst, at a temperature of 50.degree. C. to 200.degree. C. The products of this process are chlorine end-terminated organosiloxanes.
    Type: Grant
    Filed: July 13, 1992
    Date of Patent: September 21, 1993
    Assignee: Dow Corning Corporation
    Inventors: Loren D. Durfee, Terrence K. Hilty
  • Patent number: 5247117
    Abstract: A process for removing acidic impurities from alkoxysilanes obtained from halogenosilanes and alcohols which inevitable contain small amounts of acidic impurities is described. In the process, at least one member selected from alkali metal salts of alcohols and amines having a great steric hindrance as having a bulky substituent is added to the alkoxysilane for a time sufficient to neutralize the acidic impurities and the mixture is purified by distillation to obtain a substantially acidic impurity-free alkoxysilane.
    Type: Grant
    Filed: November 13, 1991
    Date of Patent: September 21, 1993
    Assignee: Shin-Etsu Chemical Co., Ltd.
    Inventors: Toshio Yamazaki, Masaaki Yamaya, Hideyoshi Yanagisawa, Masayuki Takahashi
  • Patent number: 5245067
    Abstract: A process for purifying organopolysiloxanes, which comprises treating organopolysiloxanes after their preparation with an elemental metal. Impurities which are related to the preparation of organopolysiloxanes and cause changes in color, in particular during storage under the influence of heat, subsequent clouding, inhibition of catalysts, a lack of heat stability, a lack of dielectric strength or the formation of odors, especially after exposure to light, are removed by the process of this invention.
    Type: Grant
    Filed: June 29, 1992
    Date of Patent: September 14, 1993
    Assignee: Wacker-Chemie GmbH
    Inventors: Otto Schneider, Johann Schuster, Ludwig Hager
  • Patent number: 5231205
    Abstract: The magnesium complexes of cyclic hydrocarbons, such as 1,2-dimethylenecycloalkanes, are readily prepared in high yields using highly reactive magnesium. Reactions of these (2-butene-1,4-diyl)magnesium reagents with electrophiles such as dibromoalkanes, alkylditosylates, or bromoalkylnitriles serve as a convenient method for synthesizing spirocyclic systems. Significantly, spirocarbocycles prepared by thisThe present invention was made with Government support under Contract No. GM35153 awarded by the National Institute of Health. The Government has certain rights in the invention.
    Type: Grant
    Filed: September 23, 1991
    Date of Patent: July 27, 1993
    Assignee: Board of Regents of the University of Nebraska
    Inventor: Reuben D. Rieke
  • Patent number: 5225510
    Abstract: A composition which is an anhydrous organic solvent free mixture of a hydrolyzable silane monomer; silanols formed by hydrolysis of the silane monomer; alkoxy functional oligomers formed by condensation of the silanols such as dimers and trimers; and higher alkoxy functional oligomers such as tetramers. Methods of making and using the composition are described.
    Type: Grant
    Filed: July 15, 1992
    Date of Patent: July 6, 1993
    Assignee: Dow Corning Corporation
    Inventors: Howard M. Bank, Richard D. Meindertsma
  • Patent number: 5211877
    Abstract: The present invention relates to liquid-crystalline compounds and to a process for preparing liquid-crystalline polyorganosiloxanes having methacryloxy and/or acryloxy groups by the reaction of organosiloxanes having hydrogen atoms bonded directly to silicon atoms and/or organosilanes which can be condensed to form organosiloxanes having hydrogen atoms bonded directly to silicon atoms, with alkenes and/or alkynes having mesogenic groups, which comprises reacting in a first step the organosiloxanes with an alkene and/or alkyne having at least one non-enolic hydroxyl group protected by a protective group, and in a second step the protective group is removed and the hydroxyl group which is now free is esterified with (meth)acrylic acid, esters, anhydrides and/or halides thereof and thereafter optionally condensing the organosilanes to organosiloxanes.
    Type: Grant
    Filed: August 31, 1989
    Date of Patent: May 18, 1993
    Assignee: Consortium fur elektrochemische Industrie GmbH
    Inventors: Dirk Andrejewski, Magdi Gohary, Hans-Joachim Luckas, Rainer Winkler, Franz-Heinrich Kreuzer
  • Patent number: 5210250
    Abstract: A simple but very effective and reliable method is proposed for the decolorizing purification of a halogenated silane compound, e.g., methyl trichlorosilane, colored by containing a very small amount of heavy metal impurities such as iron. The method comprises: contacting the halogenated silane compound with a small amount of a cationic surface active agent which is solid and insoluble in the silane such as a quaternary ammonium salt, e.g., trimethyl octadecyl ammonium chloride, for 2 to 240 minutes; and then separating the silane compound from the cationic surface active agent.
    Type: Grant
    Filed: August 27, 1992
    Date of Patent: May 11, 1993
    Assignee: Shin-Etsu Chemical Co. Ltd.
    Inventors: Isao Watanuki, Hiroshi Tsumura, Nobuhiko Kodana, Kazushi Satoh, Masanori Fukuhira, Hidehiko Aonuma
  • Patent number: 5210254
    Abstract: A method for reducing the level of acidic halide contamination in alkoxysilanes by contacting the silane with a stoichiometric excess of (i) a basic reagent, such as in particular, a metal alkoxide and (ii) an acid salt.
    Type: Grant
    Filed: March 31, 1992
    Date of Patent: May 11, 1993
    Assignee: Union Carbide Chemicals & Plastics Technology Corporation
    Inventors: James S. Ritscher, Scot M. Turner
  • Patent number: 5202405
    Abstract: Chloromethyltrichlorosilane is converted to polychlorocarbosilane and in turn to a polycarbosilane polymer that has utility as a precursor to silicon carbide ceramics.
    Type: Grant
    Filed: August 29, 1991
    Date of Patent: April 13, 1993
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Michael J. Michalczyk
  • Patent number: 5200487
    Abstract: Disclosed is a process for the synthesizing of polysilsesquioxane, including a first step for the hydrolysis, in the presence of ether, of trichlorosilane with the general formula RSiCl.sub.3 where R represents an organic radical, notably an alkyl, an aryl, a vinyl or an allyl, said process further including the following steps;2nd step: the dissolving of the solid product obtained at the end of the first step in an anhydrous ketonic solvent and the addition of a base, the reaction taking place under heat, a solid product being obtained after evaporation and drying;3rd step: the dissolving of the solid product obtained at the end of the second step in an anyhydrous ketone, the addition of a chain-terminating agent, the reaction taking place under heat and the solution obtained being filtered, evaporated and dried to give the desired polysilsesquioxane,wherein the second step is repeated several times.
    Type: Grant
    Filed: December 20, 1990
    Date of Patent: April 6, 1993
    Assignee: Thomson-CSF
    Inventors: Marc Lagarde, Dominique Broussoux, Jean-Claude Dubois
  • Patent number: 5196497
    Abstract: The present invention relates to a process for the production of diorganyloxyorganosilyl- or triorganyloxysilyl-terminated poly(di-organosiloxanes) by reaction of .alpha.,.omega.-dihydroxypoly(diorganosiloxanes) with alkoxysilanes in the presence of catalytically active strong alkali metal bases.
    Type: Grant
    Filed: July 8, 1991
    Date of Patent: March 23, 1993
    Assignee: Bayer Aktiengesellschaft
    Inventors: Wilhelm Weber, Theo Achtenberg, Karl-Heinz Sockel, Hans Sattlegger
  • Patent number: 5166384
    Abstract: In a trimethoxysilane preparation from silicon metal and methanol which preparation uses a solvent, a method for removing a siloxane dissolved in the solvent, which method comprises contacting the solvent with a boron-oxygen compound, and optionally an alkali metal alkoxide such as sodium methoxide.
    Type: Grant
    Filed: April 7, 1992
    Date of Patent: November 24, 1992
    Assignee: Union Carbide Chemicals & Plastics Technology Corporation
    Inventors: Donald L. Bailey, Thomas E. Childress, Robert L. Ocheltree, James S. Ritscher
  • Patent number: 5138081
    Abstract: A process for purifying an impure vinylically-unsaturated organosilicon product compound prepared by reaction between a vinylically-unsaturated organosilicon precursor and a halogenated organic compound in the presence of a homogeneous zerovalent palladium catalyst complex, the catalyst complex including an organophosphine or organoarsine ligand, in the presence of a hydrogen halide acceptor in an essentially anhydrous diluent, comprising treating a mixture containing the impure vinylically-unsaturated organosilicon product compound with a peroxide for a time sufficient to oxidize organophosphine or organoarsine impurities present in a mixture being treated. The peroxide can be selected from aqueous hydrogen peroxide or organic peroxides. The thus-treated mixture can be further treated by chromatography over silica gel or alumina. In optional embodiments, chromatography over silica gel or alumina can precede treatment with the peroxide.
    Type: Grant
    Filed: April 30, 1991
    Date of Patent: August 11, 1992
    Assignee: The Dow Chemical Company
    Inventors: Robert A. DeVries, Mary L. Ash, Hughie R. Frick, deceased
  • Patent number: 5122356
    Abstract: A process for purification of hydrochloric acid containing hydrogen fluoride, which process comprises steps of:contacting the hydrochloric acid containing hydrogen fluoride with at least one silicon compound of the formula:R.sup.1 R.sup.2 R.sup.3 SiX (1)wherein X is chlorine, hydroxyl or OSiR.sup.4 R.sup.5 R.sup.6, and R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5 and R.sup.6 are the same or different and alkyl groups having 1 to 4 of carbon atoms, andrecovering a trialkylfluorosilane compound produced in said contacting step of the formula:R.sup.1 R.sup.2 R.sup.3 SiF (2)wherein R.sup.1, R.sup.2 and R.sup.3 are the same as defined above,said recovering step comprising sub-steps of: hydrolyzing the produced trialkylfluorosilane compound (2) after the recovery thereof to convert to a trialkylsilanol compound of the formula:R.sup.1 R.sup.2 R.sup.3 SiOH (3)wherein R.sup.1, R.sup.2 and R.sup.
    Type: Grant
    Filed: March 20, 1991
    Date of Patent: June 16, 1992
    Assignee: Daikin Industries Ltd.
    Inventors: Takuo Kawamura, Tomizo Sota