US4707531A
Expired / Lapsed
US
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Method for producing organosilicon polymers and the polymers prepared thereby
Assignee: DuPont Toray Specialty Materials KK
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Filing: 1986-10-22
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Granted: 1987-11-17
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Expires: 2006-10-22
Abstract
Abstract The method of dripping an alkyl silicate into a mixture of an aqueous hydrochloric acid which contains at least 5 weight percent hydrogen chloride and a trialkylsilane or a disiloxane at a temperature of from 0 DEG to 90 DEG C. is a highly reproducible method for producing a three-dimensional structure of monofunctional siloxane units and tetrafunctional siloxane units. The organosilicon polymers produced are useful as tack agents, coating agents, and as additives in other compositions.
Inventors
- 👤 Akihiko Shirahata
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 04:43
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/02; C08G77/04; C08G77/06
Claims Analysis
Total Claims: 28
Claim 1
Independent Claim
159 words
A method for producing organosilicon polymer having a general average formula (R.sup.1 R.sup.2 R.sup.3 SiO.sub.1/2).sub.a (SiO.sub.4/2).sub.b in which each R 1 , R 2 , and R 3 is a hydrogen atom or a monovalent hydrocarbon radical and the ratio of a/b is from 0.2/1 to about 4/1 comprising dripping an alkyl silicate selected from the group consisting of alkyl orthosilicate and its partial hydrolysis condensate into a mixture of aqueous hydrochloric acid containing at least 5 weight percent hydrogen chloride and an organosilicon compound selected from the group consisting of a disiloxane of the formula (R.sup.1 R.sup.2 R.sup.3 Si).sub.2 O, an organosilane of the formula R.sup.1 R.sup.2 R.sup.3 SiX, and mixtures thereof in which R 1 , R 2 , and R 3 are defined above and X is a group selected from the group consisting of a halogen atom, an alkoxy group, and a hydroxyl group at a temperature of from 0° to 90° C. with stirring.
Claim 2
Independent Claim
159 words
A method for producing organosilicon polymer having a general average formula (R.sup.1 R.sup.2 R.sup.3 SiO.sub.1/2).sub.a (SiO.sub.4/2).sub.b in which each R 1 , R 2 , and R 3 is a hydrogen atom or a monovalent hydrocarbon radical and the ratio of a/b is from 0.2/1 to about 4/1 comprising dripping an alkyl silicate selected from the group consisting of alkyl orthosilicate and its partial hydrolysis condensate into a mixture of aqueous hydrochloric acid containing at least 5 weight percent hydrogen chloride and an organosilicon compound selected from the group consisting of a disiloxane of the formula (R.sup.1 R.sup.2 R.sup.3 Si).sub.2 O, an organosilane of the formula R.sup.1 R.sup.2 R.sup.3 SiX, and mixtures thereof in which R 1 , R 2 , and R 3 are defined above and X is a group selected from the group consisting of a halogen atom, an alkoxy group, and a hydroxyl group at a temperature of from 0° to 90° C. with stirring.
Claim 3
Dependent Claim
14 words
The method in accordance to claim 1 further comprising removing the low boiling components.
Claim 4
Dependent Claim
20 words
The method in accordance to claim 2 in which the low boiling components are removed by heating at reduced pressure.
Claim 5
Dependent Claim
16 words
The method in accordance to claim 1 further comprising an organic solvent present in the mixture.
Claim 6
Dependent Claim
14 words
The method in accordance to claim 4 further comprising removing the low boiling components.
Claim 7
Dependent Claim
20 words
The method in accordance to claim 5 in which the low boiling components are removed by heating at reduced pressure.
Claim 8
Dependent Claim
21 words
The method in accordance to claim 1 in which the aqueous hydrochloric acid contains at least 10 weight percent hydrogen chloride.
Claim 9
Dependent Claim
21 words
The method in accordance to claim 6 in which the aqueous hydrochloric acid contains at least 10 weight percent hydrogen chloride.
Claim 10
Dependent Claim
15 words
The method in accordance to claim 1 in which the organosilicon compound is a disiloxane.
Claim 11
Dependent Claim
15 words
The method in accordance to claim 7 in which the organosilicon compound is a disiloxane.
Claim 12
Dependent Claim
15 words
The method in accordance to claim 8 in which the organosilicon compound is a disiloxane.
Claim 13
Dependent Claim
82 words
The method in accordance to claim 11 in which the disiloxane is hexamethyldisiloxane, the aqueous hydrochloric acid is concentrated hydrochloric acid, the alkyl silicate is selected from the group consisting of ethyl polysilicate and tetraethoxysilane, the organic solvent is selected from the group consisting of ethanol and a mixture of ethanol and toluene, the mixture is heated to 50° to 90° C. before the tetraethoxysilane is dripped into it, and the ratio of (CH.sub.3).sub.3 SiO.sub.1/2 to SiO.sub.4/2 is from 1/1 to 1.6/1.
Claim 14
Dependent Claim
20 words
The method in accordance to claim 12 in which the alkyl silicate is tetraethoxysilane and the organic solvent is ethanol.
Claim 15
Dependent Claim
26 words
The method in accordance to claim 12 in which the alkyl silicate is ethyl polysilicate and the organic solvent is a mixture of ethanol and toluene.
Claim 16
Dependent Claim
25 words
The method in accordance to claim 12 in which the alkyl silicate is tetraethoxysilane and the organic solvent is a mixture of ethanol and toluene.
Claim 17
Dependent Claim
51 words
The method in accordance to claim 10 in which the alkyl silicate is tetramethoxysilane, the aqueous hydrochloric acid is concentrated hydrochloric acid, the disiloxane is 1,1,3,3-tetramethyldisiloxane, the mixture is at a temperature of from 0° to 35° C., and the ratio of H(CH.sub.3).sub.2 SiO.sub.1/2 to SiO.sub.4/2 is from 1.5/1 to 2/1.
Claim 18
Dependent Claim
84 words
The method in accordance to claim 11 in which the alkyl silicate is tetramethoxysilane, the aqueous hydrochloric acid is concentrate hydrochloric acid, the disiloxane is a mixture of hexamethyldisiloxane and 1,1,3,3-tetramethyldisiloxane, the organic solvent is ethanol, the mixture is at a temperature of from 0° to 35° C., the ratio of (CH.sub.3).sub.3 SiO.sub.1/2 +H(CH.sub.3).sub.2 SiO.sub.1/2 to SiO.sub.4/2 is from 1/1 to 2/1, and the amount of silicon bonded hydrogen atom is from 0.05 to 1 weight percent based on the weight of the polymer.
Claim 19
Dependent Claim
56 words
The method in accordance to claim 11 in which the alkyl silicate is tetraethoxysilane, the aqueous hydrochloric acid is concentrated hydrochloric acid, the disiloxane is 1,3-vinyl-1,1,3,3-tetramethyldisiloxane, the organic solvent is ethanol, the mixture is at a temperature of from 50° to 90° C., the ratio of (CH.sub.2 ═CH)(CH.sub.3).sub.2 SiO.sub.1/2 to SiO.sub.4/2 is from 1/1 to 3/1.
Claim 20
Dependent Claim
81 words
The method in accordance to claim 10 in which the alkyl silicate is tetraethoxysilane, the aqueous hydrochloric acid is concentrated hydrochloric acid, the disiloxane is a mixture of hexamethyldisiloxane and 1,3-vinyl-1,1,3,3-tetramethyldisiloxane, the organic solvent is ethanol, the mixture is at a temperature of from 50° to 90° C., the ratio of (CH.sub.2 ═CH)(CH.sub.3).sub.3 SiO.sub.178 +(CH.sub.3).sub.3 SiO.sub.1/2 to SiO.sub.4/2 is from 1/1 to 2/1, and the vinyl content is from 0.1 to 10 weight percent based on the weight of the polymer.
Claim 21
Dependent Claim
9 words
The composition obtained from the method of claim 1.
Claim 22
Dependent Claim
9 words
The composition obtained from the method of claim 2.
Claim 23
Dependent Claim
9 words
The composition obtained from the method of claim 4.
Claim 24
Dependent Claim
9 words
The composition obtained from the method of claim 6.
Claim 25
Dependent Claim
9 words
The composition obtained from the method of claim 12.
Claim 26
Dependent Claim
9 words
The composition obtained from the method of claim 16.
Claim 27
Dependent Claim
9 words
The composition obtained from the method of claim 18.
Claim 28
Dependent Claim
9 words
The composition obtained from the method of claim 19.
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