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Emulsions of reinforced polydiorganosiloxane latex

Assignee: Dow Silicones Corp
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Filing: 1984-06-26
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Granted: 1986-01-28
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Expires: 2004-06-26
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Abstract

Abstract This invention is a method of producing a latex of crosslinked polydiorganosiloxane reinforced with colloidal silica. The method allows the production of a latex having a relatively high amount of silica present in relation to the polymer because the water used to form the emulsion can be that present in the acidic colloidal silica sol used in the method. The high solids latex can be useful as a caulking material. The method homogenizes a hydroxyl endblocked polydiorganosiloxane, a silane of the formula R' a Si(OR 3 ) 4-a where R' is a monovalent hydrocarbon radical of up to 12 carbon atoms, R 3 is an alkyl radical of 1 to 6 carbon atoms, a partial hydrolyzate, or mixture of silane and hydrolyzate, and a is 0 or 1; a surface active anionic catalyst of the formulae R 2 C 6 H 4 SO 3 H wherein R 2 is a monovalent hydrocarbon radical of at least 6 carbon atoms, R 2 OSO 2 OH, or ##STR1## wherein R 4 is H or R 2 ; and greater than 1 part by weight of colloidal silica present as an acidic sol in water. This homogenized mixture is an oil-in-water emulsion. This emulsion is maintained at a temperature of 15° to 30° C. for at least 5 hours at a pH of less than 5 until a crosslinked polymer is formed. The product is a latex which produces an elastomer upon removal of the water at room temperature. Shelf stable products are produced by adjusting the pH to from 7 to 12.5.

Inventors

  • 👤 David J. Huebner
  • 👤 John C. Saam

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 09:33
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/02; C08J3/03; C08G; C08G77/00; C08G77/04; C08G77/06; C08G77/08; C08K; C08K5/00; C08K5/36; C08K5/41; C08K5/42; C08J2383/00; C08J2383/04

Claims Analysis

Total Claims: 22
Claim 1
Independent Claim 320 words
A method of producing an aqueous latex of crosslinked polydiorganosiloxane consisting essentially of (A) homogenizing immediately after admixing, a mixture consisting essentially of (1) 100 parts by weight of polydiorganosiloxane of the formula HO(R.sub.2 SiO).sub.x H wherein each R is a radical selected from the group consisting of methyl, ethyl, propyl, phenyl, vinyl, allyl, and 3,3,3-trifluoropropyl, and x is an average value in the range of from 3 to 100 inclusive (2) 0.5 to 15 parts by weight of an alkoxy silicon compound selected from the group consisting of silane of the formula R'.sub.a Si(OR.sup.3).sub.4-a where R' is a monovalent hydrocarbon radical having up to 12 carbon atoms, R 3 is an alkyl radical having from 1 to 6 inclusive carbon atoms, and a is 0 or 1; a partial hydrolyzate of the silane where the partial hydrolyzate is soluble in the polydiorganosiloxane (1); and mixtures of silane and partial hydrolyzate, (3) from 15 to 100 millimoles of surface active anionic catalyst per kilogram of polydiorganosiloxane, where said catalyst is selected from the group consisting of a compound of the formula R 2 C 6 H 4 SO 3 H wherein R 2 is a monovalent hydrocarbon radical of at least 6 carbon atoms; a compound of the formula R 2 OSO 2 OH wherein R 2 is as defined above; a compound of the formula ##STR6## wherein R 2 is as defined above and R 4 is hydrogen or R 2 ; and mixtures thereof, and (4) greater than 1 part by weight of colloidal silica present as an acidic sol in water, to yield an oil-in-water emulsion, then (B) maintaining the emulsion produced in (A) at a temperature of from 15° to 30° C. for at least 5 hours at a pH of less than 5 until a crosslinked polymer is formed to yield a latex which produces an elastomer upon removal of the water at room temperature.
Claim 2
Independent Claim 320 words
A method of producing an aqueous latex of crosslinked polydiorganosiloxane consisting essentially of (A) homogenizing immediately after admixing, a mixture consisting essentially of (1) 100 parts by weight of polydiorganosiloxane of the formula HO(R.sub.2 SiO).sub.x H wherein each R is a radical selected from the group consisting of methyl, ethyl, propyl, phenyl, vinyl, allyl, and 3,3,3-trifluoropropyl, and x is an average value in the range of from 3 to 100 inclusive (2) 0.5 to 15 parts by weight of an alkoxy silicon compound selected from the group consisting of silane of the formula R'.sub.a Si(OR.sup.3).sub.4-a where R' is a monovalent hydrocarbon radical having up to 12 carbon atoms, R 3 is an alkyl radical having from 1 to 6 inclusive carbon atoms, and a is 0 or 1; a partial hydrolyzate of the silane where the partial hydrolyzate is soluble in the polydiorganosiloxane (1); and mixtures of silane and partial hydrolyzate, (3) from 15 to 100 millimoles of surface active anionic catalyst per kilogram of polydiorganosiloxane, where said catalyst is selected from the group consisting of a compound of the formula R 2 C 6 H 4 SO 3 H wherein R 2 is a monovalent hydrocarbon radical of at least 6 carbon atoms; a compound of the formula R 2 OSO 2 OH wherein R 2 is as defined above; a compound of the formula ##STR6## wherein R 2 is as defined above and R 4 is hydrogen or R 2 ; and mixtures thereof, and (4) greater than 1 part by weight of colloidal silica present as an acidic sol in water, to yield an oil-in-water emulsion, then (B) maintaining the emulsion produced in (A) at a temperature of from 15° to 30° C. for at least 5 hours at a pH of less than 5 until a crosslinked polymer is formed to yield a latex which produces an elastomer upon removal of the water at room temperature.
Claim 3
Dependent Claim 25 words
The method of claim 1 in which step (B) is followed by (C) adjusting the pH of the product of (B) to greater than 3.
Claim 4
Dependent Claim 26 words
The method of claim 1 in which step (B) is followed by (C) adjusting the pH of the product of (B) to from 3 to 7.
Claim 5
Dependent Claim 30 words
The method of claim 1 in which step (B) is followed by (C) admixing sufficient base to raise the pH of the product of (B) to from 7 to 12.5.
Claim 6
Dependent Claim 14 words
The method of claim 4 in which the pH is from 9.5 to 11.
Claim 7
Dependent Claim 34 words
The method of claim 1 in which R' is selected from the group consisting of methyl, ethyl, propyl, and phenyl and R 3 is selected from the group consisting of methyl, ethyl, and propyl.
Claim 8
Dependent Claim 16 words
The method of claim 1 in which R 2 has an average of 12 carbon atoms.
Claim 9
Dependent Claim 37 words
The method of claim 1 in which the alkoxy silicon compound is present in an amount of from 1 to 5 parts by weight and is chosen from the group consisting of ethylorthosilicate, ethylpolysilicate, methyltrimethoxysilane, and phenyltrimethoxysilane.
Claim 10
Dependent Claim 24 words
The method of claim 8 in which the surface active agent is selected from the group consisting of dodecylbenzenesulfonic acid, hydrogenlaurylsulfate, and dodecyldiphenyloxidedisulfonic acid.
Claim 11
Dependent Claim 18 words
The method of claim 9 in which (4) is 10 to 50 parts by weight of colloidal silica.
Claim 12
Dependent Claim 66 words
The method of claim 3 in which the alkoxy silicon compound is present in an amount of from 1 to 5 parts by weight and is chosen from the group consisting of ethylorthosilicate, ethylpolysilicate, methyltrimethoxysilane, and phenyltrimethoxysilane; the surface active agent is selected from the group consisting of dodecylbenzenesulfonic acid, hydrogenlaurylsulfate, and dodecyldiphenyloxidedisulfonic acid; and (4) is 10 to 50 parts by weight of colloidal silica.
Claim 13
Dependent Claim 66 words
The method of claim 4 in which the alkoxy silicon compound is present in an amount of from 1 to 5 parts by weight and is chosen from the group consisting of ethylorthosilicate, ethylpolysilicate, methyltrimethoxysilane, and phenyltrimethoxysilane; the surface active agent is selected from the group consisting of dodecylbenzenesulfonic acid, hydrogenlaurylsulfate, and dodecyldiphenyloxidedisulfonic acid; and (4) is 10 to 50 parts by weight of colloidal silica.
Claim 14
Dependent Claim 66 words
The method of claim 5 in which the alkoxy silicon compound is present in an amount of from 1 to 5 parts by weight and is chosen from the group consisting of ethylorthosilicate, ethylpolysilicate, methyltrimethoxysilane, and phenyltrimethoxysilane; the surface active agent is selected from the group consisting of dodecylbenzenesulfonic acid, hydrogenlaurylsulfate, and dodecyldiphenyloxidedisulfonic acid; and (4) is 10 to 50 parts by weight of colloidal silica.
Claim 15
Dependent Claim 10 words
The aqueous latex produced by the method of claim 1.
Claim 16
Dependent Claim 10 words
The aqueous latex produced by the method of claim 10.
Claim 17
Dependent Claim 10 words
The aqueous latex produced by the method of claim 11.
Claim 18
Dependent Claim 10 words
The aqueous latex produced by the method of claim 13.
Claim 19
Dependent Claim 13 words
The elastomer produced by removing the water from the latex of claim 14.
Claim 20
Dependent Claim 13 words
The elastomer produced by removing the water from the latex of claim 15.
Claim 21
Dependent Claim 13 words
The elastomer produced by removing the water from the latex of claim 16.
Claim 22
Dependent Claim 13 words
The elastomer produced by removing the water from the latex of claim 17.

References Cited (Backward Citations)

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US3697469A Cited
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US4066594A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1989-01-27 1989-07-29 1990-01-28 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1993-01-27 1993-07-29 1994-01-28 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1997-01-27 1997-07-29 1998-01-28 $7700.00 Window Closed / Lapsed

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