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US4026835A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of preparing heat cured siloxane foams using rhodium catalyst and foams prepared therefrom

Assignee: Dow Silicones Corp
•
Filing: 1975-07-14
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Granted: 1977-05-31
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Expires: 1995-07-14
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Abstract

Abstract Siloxane foams which are activated and cured by heating can be prepared by mixing an organohydrogensiloxane, a hydroxylated organosiloxane and a rhodium catalyst in amounts such that the ratio of silicon-bonded hydrogen atoms to silicon-bonded hydroxyl radicals is from 2.5 to 40 and thereafter heating the mixture above 90° C. The rhodium catalyst provided a pot life of at least 8 hours when used in amounts of 0.0025 grams per 100 grams of hydroxylated organosiloxane. The siloxane foams can be made to have an increased fire retardant property by adding 0.01 to 2 parts by weight carbon black based on the weight of the total composition. Siloxane foams are also prepared from mixing an organohydrogensiloxane, a hydroxylated organosiloxane, a vinyl containing triorganosiloxy endblocked polydiorganosiloxane and a rhodium catalyst. These foams can be used for cushioning, in acoustical applications and protective filling or coating applications and especially applications wherein fire retarding is important.

Inventors

  • 👤 Chi-Long Lee
  • 👤 Gary M. Ronk

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 20:08
CPC Classifications
C; C08; C08J; C08J9/00; C08J9/02; C08K; C08K5/00; C08K5/0008; C08K5/0025; C08K5/0091; C08J2383/00; C08J2383/04

Claims Analysis

Total Claims: 27
Claim 1
Independent Claim 343 words
A method of preparing a heat cured organosiloxane foam comprising mixing an organohydrogensiloxane having an average of at least three silicon-bonded hydrogen atoms per molecule, an average of no more than one silicon-bonded hydrogen atom per silicon atom and organic radicals selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl and 3,3,3-trifluoropropyl, a hydroxylated organosiloxane having an average of from greater than 1.0 to 2.5 silicon-bonded hydroxyl radicals per molecule and having an average of at least one organic radical per silicon atom selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl and 3,3,3-trifluoropropyl and a rhodium catalyst selected from a rhodium complex of a formula selected from the group consisting of: RhCl 3 S(CH 2 CH 3 ){CH 2 Si(CH 3 ) 3 } 3 , RhCl 3 S(CH 2 CH 2 CH 2 CH 3 ){CH 2 Si(CH 3 ) 3 } 3 , RhCl{(CH 3 CH 2 ) 2 S} 3 , RhCl 3 {(CH 3 CH 2 CH 2 CH 2 ) 2 S} 3 , Rh 2 Cl 6 P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 3 , Rh 2 Cl 6 P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 4 , RhCl 3 P(C 6 H 5 ) 2 {CH 2 Si(CH 3 ) 3 } 3 , RhCl(CO) P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 2 and RhCl(CO){P(C 6 H 5 ) 3 } 2 , said rhodium catalyst being present in an amount of at least 0.0025 grams per 100 grams of the hydroxylated organosiloxane, said organohydrogensiloxane and said hydroxylated organosiloxane being present in sufficient amounts to provide a molar ratio of silicon-bonded hydrogen atoms to silicon-bonded hydroxyl radicals of 2.5 to 40, where a mixture is obtained having a viscosity of less than 100,000 cps. at 25° C. and a pot life of at least 8 hours, thereafter heating said mixture above 90° C. to form a foam.
Claim 2
Independent Claim 343 words
A method of preparing a heat cured organosiloxane foam comprising mixing an organohydrogensiloxane having an average of at least three silicon-bonded hydrogen atoms per molecule, an average of no more than one silicon-bonded hydrogen atom per silicon atom and organic radicals selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl and 3,3,3-trifluoropropyl, a hydroxylated organosiloxane having an average of from greater than 1.0 to 2.5 silicon-bonded hydroxyl radicals per molecule and having an average of at least one organic radical per silicon atom selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl and 3,3,3-trifluoropropyl and a rhodium catalyst selected from a rhodium complex of a formula selected from the group consisting of: RhCl 3 S(CH 2 CH 3 ){CH 2 Si(CH 3 ) 3 } 3 , RhCl 3 S(CH 2 CH 2 CH 2 CH 3 ){CH 2 Si(CH 3 ) 3 } 3 , RhCl{(CH 3 CH 2 ) 2 S} 3 , RhCl 3 {(CH 3 CH 2 CH 2 CH 2 ) 2 S} 3 , Rh 2 Cl 6 P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 3 , Rh 2 Cl 6 P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 4 , RhCl 3 P(C 6 H 5 ) 2 {CH 2 Si(CH 3 ) 3 } 3 , RhCl(CO) P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 2 and RhCl(CO){P(C 6 H 5 ) 3 } 2 , said rhodium catalyst being present in an amount of at least 0.0025 grams per 100 grams of the hydroxylated organosiloxane, said organohydrogensiloxane and said hydroxylated organosiloxane being present in sufficient amounts to provide a molar ratio of silicon-bonded hydrogen atoms to silicon-bonded hydroxyl radicals of 2.5 to 40, where a mixture is obtained having a viscosity of less than 100,000 cps. at 25° C. and a pot life of at least 8 hours, thereafter heating said mixture above 90° C. to form a foam.
Claim 3
Dependent Claim 47 words
The method in accordance with claim 1 in which the organohydrogensiloxane is a trimethylsiloxy endblocked polymethylhydrogensiloxane having a viscosity of less than 100 cps. at 25° C. and the hydroxylated organosiloxane is a hydroxyl endblocked polydimethylsiloxane having a viscosity of less than 25,000 cps. at 25° C.
Claim 4
Dependent Claim 49 words
The method in accordance with claim 2 in which the hydroxylated organosiloxane is a mixture of a hydroxyl endblocked polydimethylsiloxane having a viscosity of from 1000 to 25,000 cps. at 25° C. and a hydroxyl endblocked polydimethylsiloxane having a viscosity of from 20 to 200 cps. at 25° C.
Claim 5
Dependent Claim 32 words
The method in accordance with claim 1 in which carbon black is present in an amount of from 0.01 to 2 parts by weight based on the weight of the total composition.
Claim 6
Dependent Claim 32 words
The method in accordance with claim 2 in which carbon black is present in an amount of from 0.01 to 2 parts by weight based on the weight of the total composition.
Claim 7
Dependent Claim 32 words
The method in accordance with claim 3 in which carbon black is present in an amount of from 0.01 to 2 parts by weight based on the weight of the total composition.
Claim 8
Independent Claim 422 words
A method of preparing a heat cured organosiloxane foam comprising mixing an organohydrogensiloxane having an average of at least three silicon-bonded hydrogen atoms per molecule, an average of no more than one silicon-bonded hydrogen atom per silicon atom and organic radicals selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl and 3,3,3-trifluoropropyl, a hydroxylated organosiloxane having an average of from 1.5 to 2.5 silicon-bonded hydroxyl radicals per molecule and having an average of at least one organic radical per silicon atom selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl and 3,3,3-trifluoropropyl, a benzene-soluble vinyl containing triorganosiloxy endblocked polydiorganosiloxane having an average of about two vinyl radicals per molecule and present in an amount equal to no more than 85 weight percent of the combined weight of the hydroxylated organosiloxane and the benzene-soluble vinyl containing triorganosiloxy endblocked polydiorganosiloxane, the organic radicals of the benzene-soluble vinyl containing triorganosiloxy endblocked polydiorganosiloxane being selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl, vinyl and 3,3,3-trifluoropropyl and a rhodium catalyst selected from a rhodium complex of a formula selected from the group consisting of RhCl 3 S(CH 2 CH 3 ){CH 2 Si(CH 3 ) 3 } 3 , RhCl 3 S(CH 2 CH 2 CH 2 CH 3 ){CH 2 Si(CH 3 ) 3 } 3 , RhCl 3 {(CH 3 CH 2 ) 2 S} 3 , RhCl 3 {(CH 3 CH 2 CH 2 CH 2 ) 2 S} 3 , Rh 2 Cl 6 P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 3 , Rh 2 Cl 6 P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 4 , RhCl 3 P(C 6 H 5 ) 2 {CH 2 Si(CH 3 ) 3 } 3 , RhCl(CO) P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 2 and RhCl(CO){P(C 6 H 5 ) 3 } 2 , said rhodium catalyst being present in an amount of at least 0.0025 grams per 100 grams of the hydroxylated organosiloxane, said organohydrogensiloxane and said hydroxylated organosiloxane being present in sufficient amounts to provide a molar ratio of silicon-bonded hydrogen atoms to silicon-bonded hydroxyl radicals of 0.5 to 40, where a mixture is obtained having a viscosity of less than 100,000 cps. at 25° C. and a pot life of at least 8 hours, thereafter heating said mixture above 90° C. to form a foam.
Claim 9
Independent Claim 422 words
A method of preparing a heat cured organosiloxane foam comprising mixing an organohydrogensiloxane having an average of at least three silicon-bonded hydrogen atoms per molecule, an average of no more than one silicon-bonded hydrogen atom per silicon atom and organic radicals selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl and 3,3,3-trifluoropropyl, a hydroxylated organosiloxane having an average of from 1.5 to 2.5 silicon-bonded hydroxyl radicals per molecule and having an average of at least one organic radical per silicon atom selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl and 3,3,3-trifluoropropyl, a benzene-soluble vinyl containing triorganosiloxy endblocked polydiorganosiloxane having an average of about two vinyl radicals per molecule and present in an amount equal to no more than 85 weight percent of the combined weight of the hydroxylated organosiloxane and the benzene-soluble vinyl containing triorganosiloxy endblocked polydiorganosiloxane, the organic radicals of the benzene-soluble vinyl containing triorganosiloxy endblocked polydiorganosiloxane being selected from the group consisting of alkyl radicals having from one to six carbon atoms per radical, phenyl, vinyl and 3,3,3-trifluoropropyl and a rhodium catalyst selected from a rhodium complex of a formula selected from the group consisting of RhCl 3 S(CH 2 CH 3 ){CH 2 Si(CH 3 ) 3 } 3 , RhCl 3 S(CH 2 CH 2 CH 2 CH 3 ){CH 2 Si(CH 3 ) 3 } 3 , RhCl 3 {(CH 3 CH 2 ) 2 S} 3 , RhCl 3 {(CH 3 CH 2 CH 2 CH 2 ) 2 S} 3 , Rh 2 Cl 6 P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 3 , Rh 2 Cl 6 P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 4 , RhCl 3 P(C 6 H 5 ) 2 {CH 2 Si(CH 3 ) 3 } 3 , RhCl(CO) P(CH 3 ){CH 2 Si(CH 3 ) 3 } 2 2 and RhCl(CO){P(C 6 H 5 ) 3 } 2 , said rhodium catalyst being present in an amount of at least 0.0025 grams per 100 grams of the hydroxylated organosiloxane, said organohydrogensiloxane and said hydroxylated organosiloxane being present in sufficient amounts to provide a molar ratio of silicon-bonded hydrogen atoms to silicon-bonded hydroxyl radicals of 0.5 to 40, where a mixture is obtained having a viscosity of less than 100,000 cps. at 25° C. and a pot life of at least 8 hours, thereafter heating said mixture above 90° C. to form a foam.
Claim 10
Dependent Claim 32 words
The method in accordance with claim 7 in which carbon black is present in an amount of from 0.01 to 2 parts by weight based on the weight of the total composition.
Claim 11
Dependent Claim 68 words
The method in accordance with claim 8 in which the organohydrogensiloxane is a trimethylsiloxy endblocked polymethylhydrogensiloxane having a viscosity of less than 100 cps. at 25° C. and the hydroxylated organosiloxane is a mixture of a hydroxyl endblocked polydimethylsiloxane having a viscosity of from 100 to 25,000 cps. at 25° C. and a hydroxyl endblocked polydimethylsiloxane having a viscosity of from 20 to 200 cps. at 25° C.
Claim 12
Dependent Claim 32 words
The method in accordance with claim 9 in which the benzene-soluble vinyl containing triorganosiloxy endblocked polydiorganosiloxane is a phenylmethylvinylsiloxy endblocked polydimethylsiloxane having a viscosity of less than 25,000 cps. at 25° C.
Claim 13
Dependent Claim 12 words
The method in accordance with claim 1 in which fillers are present.
Claim 14
Dependent Claim 12 words
The method in accordance with claim 3 in which fillers are present.
Claim 15
Dependent Claim 12 words
The method in accordance with claim 4 in which fillers are present.
Claim 16
Dependent Claim 12 words
The method in accordance with claim 7 in which fillers are present.
Claim 17
Dependent Claim 12 words
The method in accordance with claim 9 in which fillers are present.
Claim 18
Dependent Claim 12 words
The method in accordance with claim 10 in which fillers are present.
Claim 19
Dependent Claim 9 words
A foam prepared by the method of claim 7.
Claim 20
Dependent Claim 9 words
A foam prepared by the method of claim 9.
Claim 21
Dependent Claim 9 words
A foam prepared by the method of claim 10.
Claim 22
Dependent Claim 9 words
A foam prepared by the method of claim 11.
Claim 23
Dependent Claim 9 words
A foam prepared by the method of claim 12.
Claim 24
Dependent Claim 9 words
A foam prepared by the method of claim 13.
Claim 25
Dependent Claim 9 words
A foam prepared by the method of claim 14.
Claim 26
Dependent Claim 9 words
A foam prepared by the method of claim 15.
Claim 27
Dependent Claim 9 words
A foam prepared by the method of claim 16.

References Cited (Backward Citations)

US3070555A Cited
US3425967A Cited
US3677981A Cited
US3923705A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1980-05-30 1980-11-29 1981-05-31 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1984-05-30 1984-11-29 1985-05-31 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1988-05-30 1988-11-29 1989-05-31 $7700.00 Window Closed / Lapsed

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