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EP0133975B1 Expired / Lapsed EP ⏱️ 0.0 years remaining

Method and novel catalyst compositions for preparing polyorganosiloxanes

Assignee: Dow Silicones Corp
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Filing: 1984-07-28
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Granted: 1988-11-23
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Expires: 2004-07-28
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Abstract

No abstract record available.

Inventors

  • 👤 Charles Fleming Kohl

Bibliographic Details

Application Number —
Jurisdiction EP
Data Source google_patents
Last Synchronized 2026-11-05 18:32
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/42; C08G77/44; C08G77/04; C08G77/06; C08G77/08; C08K; C08K5/00

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 236 words
A method for preparing a polyorganosiloxane, said method comprising the steps of (I) forming a liquid reaction mixture comprising (A) at least one hydroxyl-containing organosiloxane reactant containing repeating units of the formula where each R 1 is individually selected from the group consisting of monovalent inertly substituted and monovalent unsubstituted hydrocarbon radicals containing from 1 to 6 carbon atoms and a has an average value of from 1 to 2; (B) a catalytically effective amount of a catalyst composition, and (C) an inert liquid reaction medium; (II) heating said reaction mixture at a temperature of from 30°C to the boiling point of the reaction mixture while removing the by-produced water from the reaction mixture; and (III) maintaining said temperature for a period of time sufficient to form said polyorganosiloxane, characterized in that, the catalyst composition (B) consists essentially of (1) at least one salt derived from substantially equivalent amounts of an organic mono- or polyfunctional amine and an acid selected from the group consisting of mono- and polyfunctional organosulfonic acids, phosphoric acid and sulfuric acid; and (2) at least one unreacted acid selected from the group consisting of fluorinated alkanesulfonic acids and sulfuric acid, the salt component (1) being employed at a concentration of from 10 to 500 parts by weight per million parts (ppm) of total organosiloxane reactants while the ratio of salt component (1) to unreacted acid component (2) is from 1:30 to 50:1.
Claim 2
Independent Claim 236 words
A method for preparing a polyorganosiloxane, said method comprising the steps of (I) forming a liquid reaction mixture comprising (A) at least one hydroxyl-containing organosiloxane reactant containing repeating units of the formula where each R 1 is individually selected from the group consisting of monovalent inertly substituted and monovalent unsubstituted hydrocarbon radicals containing from 1 to 6 carbon atoms and a has an average value of from 1 to 2; (B) a catalytically effective amount of a catalyst composition, and (C) an inert liquid reaction medium; (II) heating said reaction mixture at a temperature of from 30°C to the boiling point of the reaction mixture while removing the by-produced water from the reaction mixture; and (III) maintaining said temperature for a period of time sufficient to form said polyorganosiloxane, characterized in that, the catalyst composition (B) consists essentially of (1) at least one salt derived from substantially equivalent amounts of an organic mono- or polyfunctional amine and an acid selected from the group consisting of mono- and polyfunctional organosulfonic acids, phosphoric acid and sulfuric acid; and (2) at least one unreacted acid selected from the group consisting of fluorinated alkanesulfonic acids and sulfuric acid, the salt component (1) being employed at a concentration of from 10 to 500 parts by weight per million parts (ppm) of total organosiloxane reactants while the ratio of salt component (1) to unreacted acid component (2) is from 1:30 to 50:1.
Claim 3
Dependent Claim 36 words
A method according to claim 1 where said salt (B) is derived from a monoalkylamine or a 1,1,3,3 - tetraalkylguanidine wherein the alkyl radicals of the monoalkylamine and tetraalkylguanidine contain from 1 to 8 carbon atoms.
Claim 4
Dependent Claim 24 words
A method according to claim 1 where said salt (B) is derived from sulfuric acid, a polyfluorinated carboxylic acid or a polyfluorinated alkanesulfonic acid.
Claim 5
Dependent Claim 25 words
A method according to claim 3 where said polyfluorinated carboxylic acid is trifluoroacetic acid and the polyfluorinated alkanesulfonic acid is trifluoromethanesulfonic acid or tetrafluoroethanesulfonic acid.
Claim 6
Dependent Claim 13 words
A method according to claim 1 where said unreacted acid is sulfuric acid.
Claim 7
Dependent Claim 62 words
A method according to claim 1 where said unreacted acid is a fluorinated alkanesulfonic acid represented by the formula R,S0 3 H where R f represents a perfluoroalkyl radical containing from 1 to 12 carbon atoms, a H(CF 2 ) d CF 2 - radical or a F(CF 2 ) d CFHCF 2 - radical and d is 0, 1, or 2.
Claim 8
Dependent Claim 17 words
A method according to claim 6 where said fluorinated alkanesulfonic acid is trifluoromethanesulfonic acid or tetrafluoroethanesulfonic acid.
Claim 9
Dependent Claim 52 words
A method according to claim 1 where the salt component of said catalyst composition is a trifluoroacetate or trifluoromethanesulfonate of a lower N-alkyl amine and is present at a concentration of from 50 to 200 parts by weight per million parts by weight of total organosiloxane reactants present in said reaction mixture.
Claim 10
Dependent Claim 43 words
A method according to claim 1 wherein the unreacted acid component (2) of said catalyst composition is present at a concentration of from 10 to 300 parts by weight per million parts by weight of total organosiloxane reactants present in said reaction mixture.
Claim 11
Dependent Claim 91 words
A catalyst composition for preparing polyorganosiloxanes by the reaction of at least one polyorganosiloxane containing a plurality of silicon-bonded hydroxyl groups, characterized in that, said composition consists essentially of (1) at least one salt derived from equimolar amounts of an organic amine and an acid selected from the group consisting of mono- and polyfunctional carboxylic acids, mono-and polyfunctional organosulfonic acids, phosphoric acid and sulfonic acid, and (2) at least one unreacted fluorinated alkanesulfonic acid while the ratio of salt component (1) to unreacted acid component (2) is from 1:30 to 50:1.
Claim 12
Dependent Claim 91 words
A catalyst composition for preparing polyorganosiloxanes by the reaction of at least one polyorganosiloxane containing a plurality of silicon-bonded hydroxyl groups, characterized in that, said composition consists essentially of (1) at least one salt derived from equimolar amounts of an organic amine and an acid selected from the group consisting of mono- and polyfunctional carboxylic acids, mono-and polyfunctional organosulfonic acids, phosphoric acid and sulfonic acid, and (2) at least one unreacted fluorinated alkanesulfonic acid while the ratio of salt component (1) to unreacted acid component (2) is from 1:30 to 50:1.

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