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US4130599A Expired / Lapsed US ⏱️ 0.0 years remaining

Silanol-free resins

Assignee: General Electric Co
•
Filing: 1976-06-16
•
Granted: 1978-12-19
•
Expires: 1996-06-16
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Abstract

Abstract A silicone molding composition with improved thermal shock resistance having a plasticizing amount of a silicone resin comprising chemically combined RSiO 3/2 units and R 2 SiO units where the R to Si ratio may vary from 1.0 to 1.9 and the ratio of RSiO 3/2 units to R 2 SiO units may vary from 1:2.5 to 1:5.0 and containing less than 0.5 weight percent of silanol groups and preferably being substantially free of silanol groups where R is a monovalent hydrocarbon radical. There is also provided by the present invention a process for improving the thermal shock resistance of a silicone molding composition by having in said composition the aforesaid resin.

Inventors

  • 👤 Duane F. Merrill
  • 👤 Richard C. Cooke, Jr.

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 19:08
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/06; C08L; C08L83/00; C08L83/04; C08G77/14; C08G77/16; C08G77/22; C08G77/24; Y; Y10; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31652; Y10T428/31663

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 348 words
A silicone molding composition with improved thermal shock resistance having therein a base silicone resin having R 1 SiO 3/2 unit and R 2 1 SiO units where R 1 is selected from the class consisting of monovalent hydrocarbon radicals and halogenated monovalent hydrocarbon radicals, a filler and comprising the improvement in which there is present a plasticizing amount of a low-silanol content silicone resin having less than 0.5 weight silanol groups and an R to Si ratio that varies from 1.0:1 to 1.9:1 that is produced by the process comprising (a) adding a mixture of hydrolyzable silanes of the formula, R.sub.a SiX.sub.4-a to water where there is present at least 2 parts of water per part of said silanes and 1 to 5 parts of a water-immiscible organic solvent per part of said silanes at a temperature range of 25° C. to 85° C. and where the silanes are added to said water slowly so as to form a hydrolyzate; (b) continually agitating said mixture; (c) separating the organic layer and adjusting it to 10-40% solids; (d) within 24 hours from the formation of said hydrolyzate catalyzing said organic layer with 300-600 ppm of an alkali metal hydroxide per part of solid, and refluxing the resulting mixture at 100°-160° C.; (e) neutralizing the alkali metal hydroxide in the refluxed mixture with acetic acid; and (f) stripping from the organic layer excess acetic acid and solvent, where R is selected from the group consisting of alkyl radicals of 1 to 8 carbon atoms, cycloalkyl radicals of 5 to 7 carbon atoms, alkenyl radicals of 2 to 8 carbon atoms, mononuclear aryl radicals, mononuclear aryl lower alkyl radicals where the alkyl portion is 1 to 6 carbon atoms and halogenated derivatives of the above radicals, where X is a chlorine radical and a is a whole number that varies from 1 to 2 and such that 40 mole percent to 60 mole percent of the R radicals are selected from the class consisting of mononuclear aryl radicals and mononuclear aryl lower radicals and halogenated derivatives of the foregoing radicals.
Claim 2
Dependent Claim 348 words
A silicone molding composition with improved thermal shock resistance having therein a base silicone resin having R 1 SiO 3/2 unit and R 2 1 SiO units where R 1 is selected from the class consisting of monovalent hydrocarbon radicals and halogenated monovalent hydrocarbon radicals, a filler and comprising the improvement in which there is present a plasticizing amount of a low-silanol content silicone resin having less than 0.5 weight silanol groups and an R to Si ratio that varies from 1.0:1 to 1.9:1 that is produced by the process comprising (a) adding a mixture of hydrolyzable silanes of the formula, R.sub.a SiX.sub.4-a to water where there is present at least 2 parts of water per part of said silanes and 1 to 5 parts of a water-immiscible organic solvent per part of said silanes at a temperature range of 25° C. to 85° C. and where the silanes are added to said water slowly so as to form a hydrolyzate; (b) continually agitating said mixture; (c) separating the organic layer and adjusting it to 10-40% solids; (d) within 24 hours from the formation of said hydrolyzate catalyzing said organic layer with 300-600 ppm of an alkali metal hydroxide per part of solid, and refluxing the resulting mixture at 100°-160° C.; (e) neutralizing the alkali metal hydroxide in the refluxed mixture with acetic acid; and (f) stripping from the organic layer excess acetic acid and solvent, where R is selected from the group consisting of alkyl radicals of 1 to 8 carbon atoms, cycloalkyl radicals of 5 to 7 carbon atoms, alkenyl radicals of 2 to 8 carbon atoms, mononuclear aryl radicals, mononuclear aryl lower alkyl radicals where the alkyl portion is 1 to 6 carbon atoms and halogenated derivatives of the above radicals, where X is a chlorine radical and a is a whole number that varies from 1 to 2 and such that 40 mole percent to 60 mole percent of the R radicals are selected from the class consisting of mononuclear aryl radicals and mononuclear aryl lower radicals and halogenated derivatives of the foregoing radicals.
Claim 3
Dependent Claim 23 words
The composition of claim 1 wherein the water-immiscible organic solvent is selected from the group consisting of toluene, xylene, heptane, octance and cyclohexane.
Claim 4
Dependent Claim 13 words
The composition of claim 1 wherein the alkali metal hydroxide is potassium hydroxide.
Claim 5
Dependent Claim 13 words
The composition of claim 1 where R is selected from methyl and phenyl.
Claim 6
Dependent Claim 24 words
The composition of claim 1 wherein the low-silanol content resin is substantially silanol-free and has an R to Si ratio of 1.5:1 to 1.9:1.
Claim 7
Dependent Claim 329 words
A process for improving the thermal shock resistance of a silicone resin molding composition comprising adding to a base silicone resin having R 1 SiO 3/2 unit and R 2 1 SiO unit wherein R 1 is selected from the class consisting of monovalent hydrocarbon radicals and halogenated monovalent hydrocarbon radicals and a filler and a plasticizing amount of a low-silanol content silicone resin produced by the process comprising (a) adding a mixture of hydrolyzable silanes of the formula, R.sub.a SiX.sub.4-a to water where there is present at least 2 parts of water per part of said silanes and 1 to 5 parts of a water-immiscible organic solvent per part of said silanes at a temperature in the range of 25° C. to 85° C. and where the silanes are added to said water slowly so as to form a hydrolyzate; (b) continually agitating said mixture; (c) separating the organic layer and adjusting it to 10-40% solids; (d) within 24 hours from the formation of said hydrolyzate catalyzing said organic layer with 300-600 ppm of an alkali metal hydroxide per part of solid, and refluxing the resulting mixture at 100°-160° C.; (e) neutralizing the alkali metal hydroxide in the refluxed mixture with acetic acid; and (f) stripping from the organic layer excess acetic acid and solvent, where R is selected from the group consisting of alkyl radicals of 1 to 8 carbon atoms, cycloalkyl radicals of 5 to 7 carbon atoms, alkenyl radicals of 2 to 8 carbon atoms, mononuclear aryl radicals, mononuclear aryl lower alkyl radicals where the alkyl portion is 1 to 6 carbon atoms and halogenated derivatives of the above radicals, where X is a chlorine radical and a is a whole number that varies from 1 to 2 and such that 40 mole percent to 60 mole percent of the R radicals are selected from the class consisting of mononuclear aryl radicals and mononuclear aryl lower alkyl radicals and halogenated derivatives of the foregoing radicals.
Claim 8
Dependent Claim 329 words
A process for improving the thermal shock resistance of a silicone resin molding composition comprising adding to a base silicone resin having R 1 SiO 3/2 unit and R 2 1 SiO unit wherein R 1 is selected from the class consisting of monovalent hydrocarbon radicals and halogenated monovalent hydrocarbon radicals and a filler and a plasticizing amount of a low-silanol content silicone resin produced by the process comprising (a) adding a mixture of hydrolyzable silanes of the formula, R.sub.a SiX.sub.4-a to water where there is present at least 2 parts of water per part of said silanes and 1 to 5 parts of a water-immiscible organic solvent per part of said silanes at a temperature in the range of 25° C. to 85° C. and where the silanes are added to said water slowly so as to form a hydrolyzate; (b) continually agitating said mixture; (c) separating the organic layer and adjusting it to 10-40% solids; (d) within 24 hours from the formation of said hydrolyzate catalyzing said organic layer with 300-600 ppm of an alkali metal hydroxide per part of solid, and refluxing the resulting mixture at 100°-160° C.; (e) neutralizing the alkali metal hydroxide in the refluxed mixture with acetic acid; and (f) stripping from the organic layer excess acetic acid and solvent, where R is selected from the group consisting of alkyl radicals of 1 to 8 carbon atoms, cycloalkyl radicals of 5 to 7 carbon atoms, alkenyl radicals of 2 to 8 carbon atoms, mononuclear aryl radicals, mononuclear aryl lower alkyl radicals where the alkyl portion is 1 to 6 carbon atoms and halogenated derivatives of the above radicals, where X is a chlorine radical and a is a whole number that varies from 1 to 2 and such that 40 mole percent to 60 mole percent of the R radicals are selected from the class consisting of mononuclear aryl radicals and mononuclear aryl lower alkyl radicals and halogenated derivatives of the foregoing radicals.
Claim 9
Dependent Claim 23 words
The process of claim 6 wherein the water-immiscible organic solvent is selected from the group consisting of toluene, xylene, heptane, octane and cyclehexane.
Claim 10
Dependent Claim 13 words
The process of claim 6 wherein the alkali metal hydroxide is potassium hydroxide.
Claim 11
Dependent Claim 13 words
The process of claim 6 where R is selected from methyl and phenyl.
Claim 12
Dependent Claim 25 words
The process of claim 6 wherein the low silanol content resin is substantially silanol-free and has an R to Si ratio of 1.5:1 to 1.9:1.

References Cited (Backward Citations)

US2528615A Cited
US2929830A Cited
US3017386A Cited
US3120500A Cited
US3234179A Cited
US3489782A Cited
US3634297A Cited
US3759867A Cited
US3919344A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-12-18 1982-06-19 1982-12-19 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-12-18 1986-06-19 1986-12-19 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-12-18 1990-06-19 1990-12-19 $7700.00 Window Closed / Lapsed

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