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US4360610A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of improving silicone rubber composition

Assignee: Dow Silicones Corp
•
Filing: 1981-03-23
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Granted: 1982-11-23
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Expires: 2001-03-23
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Abstract

Abstract A new method of producing a silicone rubber composition yields a unique composition. When the composition is further mixed with extending filler and vulcanized, the tensile strength of the vulcanized silicone rubber is improved over that obtained when the composition is not produced following the method of this invention. The method mixes polydiorganosiloxane gum, treated reinforcing silica filler, a portion of hydroxylated organosilicon compound having an average of from 1 to 20 percent by weight hydroxyl radicals and an average of from 1 to 31 percent by weight vinyl radicals; heating the mixture; then cooling and admixing another portion of the hydroxylated organosilicon compound.

Inventors

  • 👤 Milton C. Murray
  • 👤 Joan M. Donatelli

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 22:42
CPC Classifications
C; C08; C08L; C08L83/00; C08L83/04; C08G; C08G77/00; C08G77/04; C08G77/14; C08G77/16; C08G77/20; C08G77/22; C08G77/24; C08G77/70

Claims Analysis

Total Claims: 23
Claim 1
Independent Claim 276 words
A method of producing a silicone rubber composition comprising (I) mixing (A) 100 parts by weight of polydiorganosiloxane gum having a viscosity of greater than 1000 Pa.s at 25° C., wherein the organic radicals are selected from the group consisting of methyl, phenyl, vinyl, and 3,3,3-trifluoropropyl, at least 50 percent of the organic radicals being methyl and less than 2 percent being vinyl, (B) from 10 to 85 parts by weight of treated reinforcing silica filler having a surface area of greater than 50 m 2 /g, (C) from 0.1 to 5 parts by weight of a hydroxylated organosilicon compound having the average unit formula ##EQU3## in which R is methyl, phenyl or 3,3,3-trifluoropropyl, Vi is vinyl, x has a value from 1.0 to 2.0 inclusive, y has a value such that there is present an average of from 1 to 20 percent by weight hydroxyl radical, z has a value such that there is present an average of from 1 to 31 percent by weight vinyl radical, and the compound is soluble in (A); then (II) heating the mixture to a temperature of from 60° to 250° C. for a period of from 10 minutes to 10 days to provide a product that is stable upon storage, and then (III) cooling the mixture to room temperature, and admixing during the cooling process when the temperature of the mixture is below 125° C. or after room temperature has been reached from 0.1 to 2.5 parts by weight of the hydroxylated organosilicon compound of (C) and from 1 to 250 parts by weight of extending filler with a surface area of less than 50 m 2 /g.
Claim 2
Independent Claim 276 words
A method of producing a silicone rubber composition comprising (I) mixing (A) 100 parts by weight of polydiorganosiloxane gum having a viscosity of greater than 1000 Pa.s at 25° C., wherein the organic radicals are selected from the group consisting of methyl, phenyl, vinyl, and 3,3,3-trifluoropropyl, at least 50 percent of the organic radicals being methyl and less than 2 percent being vinyl, (B) from 10 to 85 parts by weight of treated reinforcing silica filler having a surface area of greater than 50 m 2 /g, (C) from 0.1 to 5 parts by weight of a hydroxylated organosilicon compound having the average unit formula ##EQU3## in which R is methyl, phenyl or 3,3,3-trifluoropropyl, Vi is vinyl, x has a value from 1.0 to 2.0 inclusive, y has a value such that there is present an average of from 1 to 20 percent by weight hydroxyl radical, z has a value such that there is present an average of from 1 to 31 percent by weight vinyl radical, and the compound is soluble in (A); then (II) heating the mixture to a temperature of from 60° to 250° C. for a period of from 10 minutes to 10 days to provide a product that is stable upon storage, and then (III) cooling the mixture to room temperature, and admixing during the cooling process when the temperature of the mixture is below 125° C. or after room temperature has been reached from 0.1 to 2.5 parts by weight of the hydroxylated organosilicon compound of (C) and from 1 to 250 parts by weight of extending filler with a surface area of less than 50 m 2 /g.
Claim 3
Dependent Claim 38 words
The method of claim 1 further comprising admixing from 0.1 to 5 parts by weight of organic peroxide vulcanizing agent suitable for vulcanizing the polydiorganosiloxane gum after the mixture is below the activation temperature of the organic peroxide.
Claim 4
Dependent Claim 25 words
The method of claim 1 in which (A), (B), and (C) of step (I) are combined by mixing (A) and (B) and thereafter admixing (C).
Claim 5
Dependent Claim 15 words
The method of claim 1 in which the polydiorganosiloxane gum of (A) contains vinyl radical.
Claim 6
Dependent Claim 28 words
The method of claim 1 in which the hydroxylated organosilicon compound of (C) is hydroxyl endblocked polymethylvinylsiloxane having a viscosity of less than 0.5 Pa.s at 25° C.
Claim 7
Dependent Claim 12 words
The method of claim 1 in which the extending filler is siliceous.
Claim 8
Dependent Claim 28 words
The method of claim 2 in which the hydroxylated organosilicon compound of (C) is hydroxyl endblocked polymethylvinylsiloxane having a viscosity of less than 0.5 Pa.s at 25° C.
Claim 9
Dependent Claim 86 words
The method of claim 1 further comprising admixing from greater than 0.1 to 1.5 parts by weight of an acryloxyalkylsilane of the formula ##STR2## in which R' is selected from the group consisting of hydrogen and methyl radical, R" is an alkylene radical of from 1 to 4 inclusive carbon atoms, X is a radical selected from the group consisting of lower alkoxy radicals of from 1 to 3 inclusive carbon atoms and acetoxy radical, and a is from 0 to 2 inclusive, after step (III).
Claim 10
Independent Claim 401 words
A method of producing a silicone rubber composition comprising (I) mixing (A) 100 parts by weight of polydiorganosiloxane gum having a viscosity of greater than 100 Pa.s at 25° C., wherein the organic radicals are selected from the group consisting of methyl, phenyl, and vinyl, at least 78 percent of the organic radicals being methyl and less than 2 percent being vinyl, there being an average of at least two vinyl radicals per molecule on at least 25 percent by weight based on the total weight of polydiorganosiloxane gum present, (B) from 20 to 60 parts by weight of reinforcing silica filler having a surface area of greater than 50 m 2 /g, (B') from 1 to 20 parts by weight of hydroxyl endblocked polydiorganosiloxane fluid having a viscosity of less than 1.0 Pa.s at 25° C., the organic radicals being selected from the group consisting of methyl and phenyl, then (I') admixing (C) from 0.1 to 5 parts by weight of a hydroxylated organosilicon compound having the average unit formula ##EQU4## in which R is methyl or phenyl, Vi is vinyl, x has a value from 1.0 to 2.0 inclusive, y has a value such that there is present an average of from 1 to 20 percent by weight hydroxyl radical, z has a value such that there is present an average of from 1 to 31 percent by weight vinyl radical, and the compound is soluble in (A), and (D) from 0.01 to 2 parts by weight of a material selected from the group consisting of ammonium carbonate, ammonium bicarbonate, and ammonia, thereafter (II) heating the mixture to a temperature of from 100° to 175° C. for a period of from 10 minutes to 4 hours to provide a product that is stable on storage, thereafter, (III) cooling the mixture to room temperature and admixing during the cooling process when the temperature of the mixture is below 125° C. or after room temperature has been reached from 0.1 to 2.5 parts by weight of the hydroxylated organosilicon compound of (C) of step (I') and from 1 to 250 parts by weight of siliceous extending filler with a surface area of less than 50 m 2 /g, then (IV) admixing from 0.1 to 5 parts by weight of organic peroxide vulcanizing agent suitable for vulcanizing the polydiorganosiloxane gum after the mixture is below the activation temperature of the organic peroxide.
Claim 11
Independent Claim 401 words
A method of producing a silicone rubber composition comprising (I) mixing (A) 100 parts by weight of polydiorganosiloxane gum having a viscosity of greater than 100 Pa.s at 25° C., wherein the organic radicals are selected from the group consisting of methyl, phenyl, and vinyl, at least 78 percent of the organic radicals being methyl and less than 2 percent being vinyl, there being an average of at least two vinyl radicals per molecule on at least 25 percent by weight based on the total weight of polydiorganosiloxane gum present, (B) from 20 to 60 parts by weight of reinforcing silica filler having a surface area of greater than 50 m 2 /g, (B') from 1 to 20 parts by weight of hydroxyl endblocked polydiorganosiloxane fluid having a viscosity of less than 1.0 Pa.s at 25° C., the organic radicals being selected from the group consisting of methyl and phenyl, then (I') admixing (C) from 0.1 to 5 parts by weight of a hydroxylated organosilicon compound having the average unit formula ##EQU4## in which R is methyl or phenyl, Vi is vinyl, x has a value from 1.0 to 2.0 inclusive, y has a value such that there is present an average of from 1 to 20 percent by weight hydroxyl radical, z has a value such that there is present an average of from 1 to 31 percent by weight vinyl radical, and the compound is soluble in (A), and (D) from 0.01 to 2 parts by weight of a material selected from the group consisting of ammonium carbonate, ammonium bicarbonate, and ammonia, thereafter (II) heating the mixture to a temperature of from 100° to 175° C. for a period of from 10 minutes to 4 hours to provide a product that is stable on storage, thereafter, (III) cooling the mixture to room temperature and admixing during the cooling process when the temperature of the mixture is below 125° C. or after room temperature has been reached from 0.1 to 2.5 parts by weight of the hydroxylated organosilicon compound of (C) of step (I') and from 1 to 250 parts by weight of siliceous extending filler with a surface area of less than 50 m 2 /g, then (IV) admixing from 0.1 to 5 parts by weight of organic peroxide vulcanizing agent suitable for vulcanizing the polydiorganosiloxane gum after the mixture is below the activation temperature of the organic peroxide.
Claim 12
Dependent Claim 12 words
The method of claim 9 in which the polydiorganosiloxane gum is polydimethylsiloxane.
Claim 13
Dependent Claim 26 words
The method of claim 9 in which the reinforcing silica filler is a precipitated silica having a surface area of greater than 100 m 2 /g.
Claim 14
Dependent Claim 28 words
The method of claim 9 in which the hydroxlyated organosilicon compound of (C) is hydroxyl endblocked polymethylvinylsiloxane having a viscosity of less than 0.5 Pa.s at 25° C.
Claim 15
Dependent Claim 23 words
The method of claim 11 in which the siliceous extending filler is selected from the group consisting of quartz, diatomaceous earth, and clay.
Claim 16
Dependent Claim 15 words
The method of claim 12 in which the organic peroxide vulcanizing agent is vinyl specific.
Claim 17
Dependent Claim 14 words
The method of claim 14 in which the vinyl specific organic peroxide is 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane.
Claim 18
Dependent Claim 86 words
The method of claim 14 further comprising admixing from greater than 0.1 to 1.5 parts by weight of an acryloxyalkylsilane of the formula ##STR3## in which R' is selected from the group consisting of hydrogen and methyl radical, R" is an alkylene radical of from 1 to 4 inclusive carbon atoms, X is a radical selected from the group consisting of lower alkoxy radicals of from 1 to 3 inclusive carbon atoms and acetoxy radical, and a is from 0 to 2 inclusive, after step (III).
Claim 19
Dependent Claim 30 words
A method of producing a cured silicone rubber elastomer comprising heating the silicone rubber composition of claim 2, 17, or 9 to a temperature sufficient to activate the vulcanizing agent.
Claim 20
Dependent Claim 51 words
A method of producing a cured silicone rubber comprising admixing from 0.1 to 5 parts by weight of organic peroxide vulcanizing agent suitable for vulcanizing the polydiorganosiloxane gum into the silicone rubber composition of claim 3, or 9 or 1, then heating to a temperature sufficient to activate the vulcanizing agent.
Claim 21
Dependent Claim 23 words
The method of claim 1 in which the extending filler is present in an amount of from 20 to 150 parts by weight.
Claim 22
Dependent Claim 23 words
The method of claim 9 in which the extending filler is present in an amount of from 20 to 150 parts by weight.
Claim 23
Dependent Claim 17 words
The product obtained by the method of claim 2, 3, 8, 16, 1, 9, 19, or 20.

References Cited (Backward Citations)

US2890188A Cited
US3268473A Cited
US3696068A Cited
US4052357A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1985-11-22 1986-05-24 1986-11-23 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1989-11-22 1990-05-24 1990-11-23 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1993-11-22 1994-05-24 1994-11-23 $7700.00 Window Closed / Lapsed

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