US5391673A
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US
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Silicon resins and methods for their preparation
Assignee: Dow Silicones Corp
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Filing: 1993-12-30
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Granted: 1995-02-21
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Expires: 2013-12-30
Abstract
Abstract The present invention relates to methods for making silicone resins. More particularly, the present invention relates to methods for producing silicone resins comprising monofunctional units in the form of R 3 SiO 1/2 units and tetrafunctional units in the form of SiO 4/2 units. The methods of the present invention are characterized by a continuous process for producing silicone resins while maintaining a constant ratio of reactants thus producing less variation in the final product. The present invention is further related to the compositions produced by the methods of this invention.
Inventors
- 👤 Robert A. Ekeland
- 👤 II Leslie E. Carpenter
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 22:59
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/06
Claims Analysis
Total Claims: 32
Claim 1
Independent Claim
200 words
A method for making a silicone resin, the method comprising the steps of: (I) mixing in a continuous manner a silane selected from the group consisting of: (a) a silane having the formula SiX 4 wherein X is a halogen atom or a group having the formula OR wherein R is a group selected from the group consisting of alkyl groups having from 1 to 6 carbon atoms, aryl groups, and arylalkyl groups; (b) alcohol treated halogenated silanes; and (c) alkyl silicates having units of the formula ##EQU4## or a partial hydrolysis condensate thereof, wherein R 1 is a group selected from the group consisting of alkyl groups having from 1 to 6 carbon atoms, aryl groups, and arylalkyl groups, and d has a value of from 1 to 3, with a condensation catalyst; (II) adding a quenching agent to the reaction mixture of (I), whereby an aqueous layer or condensation catalyst layer and an organic-silicone resin containing layer are formed; (III) separating the aqueous layer or condensation catalyst layer from the organic-silicone resin containing layer; and (IV) stripping the organic-silicone resin containing layer; wherein the weight ratio of said silane to said condensation catalyst is constant throughout said method.
Claim 2
Independent Claim
200 words
A method for making a silicone resin, the method comprising the steps of: (I) mixing in a continuous manner a silane selected from the group consisting of: (a) a silane having the formula SiX 4 wherein X is a halogen atom or a group having the formula OR wherein R is a group selected from the group consisting of alkyl groups having from 1 to 6 carbon atoms, aryl groups, and arylalkyl groups; (b) alcohol treated halogenated silanes; and (c) alkyl silicates having units of the formula ##EQU4## or a partial hydrolysis condensate thereof, wherein R 1 is a group selected from the group consisting of alkyl groups having from 1 to 6 carbon atoms, aryl groups, and arylalkyl groups, and d has a value of from 1 to 3, with a condensation catalyst; (II) adding a quenching agent to the reaction mixture of (I), whereby an aqueous layer or condensation catalyst layer and an organic-silicone resin containing layer are formed; (III) separating the aqueous layer or condensation catalyst layer from the organic-silicone resin containing layer; and (IV) stripping the organic-silicone resin containing layer; wherein the weight ratio of said silane to said condensation catalyst is constant throughout said method.
Claim 3
Dependent Claim
10 words
A method according to claim 1, wherein X is chlorine.
Claim 4
Dependent Claim
19 words
A method according to claim 1, wherein (a) is selected from the group consisting of tetramethoxysilane, tetraethoxysilane, or tetrapropoxysilane.
Claim 5
Dependent Claim
86 words
A method according to claim 1, wherein the halogenated silane of (b) is a compound having the formula R 2 R 3 R 4 SiY wherein R 2 , R 3 and R 4 are selected from hydrogen, alkyl groups having from 1 to 12 carbon atoms, alkenyl groups having from 2 to 12 carbon atoms, aryl groups, arylalkyl groups, or perfluoroalkylethyl groups having the formula C n F 2n+1 CH 2 CH 2 where n is 1 to 6, and Y is a halogen atom.
Claim 6
Dependent Claim
28 words
A method according to claim 4, wherein the halogenated silane of (b) is selected from the group consisting of trimethylchlorosilane, triethylchlorosilane, trimethylbromosilane, triethylbromosilane, trimethylfluorosilane, triethylfluorosilane, dimethylvinylchlorosilane, and dimethyl-5-hexenylchlorosilane.
Claim 7
Dependent Claim
22 words
A method according to claim 1, wherein the alcohol of (b) is selected from the group consisting of ethanol, methanol, and isopropanol.
Claim 8
Dependent Claim
10 words
A method according to claim 1, wherein (c) is ethylpolysilicate.
Claim 9
Dependent Claim
24 words
A method according to claim 1, wherein the condensation catalyst is selected from the group consisting of hydrochloric acid, sulfuric acid, and sulfonic acids.
Claim 10
Dependent Claim
142 words
A method according to claim 1, wherein the quenching agent is selected from the group consisting of (i) a disiloxane having the formula (R 5 R 6 R 7 Si) 2 O and (ii) a silane having the formula R 5 R 6 R 7 SiZ wherein R 5 , R 6 and R 7 are selected from hydrogen, alkyl groups having from 1 to 12 carbon atoms, alkenyl groups having from 2 to 12 carbon atoms, aryl groups, arylalkyl groups, and perfluoroalkylethyl groups having the formula C n F 2n+1 CH 2 CH 2 where n is 1 to 6, and Z is a halogen atom or is a group having the formula OR 8 wherein R 8 is a group selected from the group consisting of alkyl groups having from 1 to 6 carbon atoms, aryl groups, and arylalkyl groups.
Claim 11
Dependent Claim
10 words
A method according to claim 9, wherein Z is chlorine.
Claim 12
Dependent Claim
25 words
A method according to claim 9, wherein the disiloxane is selected from the group consisting of tetramethyldisiloxane, hexamethyldisiloxane, tetramethyldivinylsiloxane, tetramethyldi-5-hexenylsiloxane, tetramethyl-3,3,3-trifluoropropyldisiloxane, tetramethyldiethylsiloxane, tetramethyldiphenyldisiloxane, and diethyldiphenyldivinyldisiloxane.
Claim 13
Dependent Claim
15 words
A method according to claim 1, wherein the quenching agent further comprises an organic solvent.
Claim 14
Dependent Claim
20 words
A method according to claim 12, wherein the organic solvent is selected from the group consisting of heptane and xylene.
Claim 15
Independent Claim
131 words
A method for making a silicone resin, the method comprising the steps of: (I) mixing in a continuous manner a silane selected from the group consisting of: (i) alkoxysilanes, (ii) halogenated silanes, and (iii) alkyl silicates with a silicon compound selected from the group consisting of: (iv) trialkylhalosilanes and (v) disiloxanes; (II) adding an alcohol to the mixture of (I); (III) adding water or a mixture of water and a condensation catalyst to the mixture of (II) whereby an aqueous layer and an organic-silicone resin containing layer are formed; (IV) separating the aqueous layer from the organic-silicone resin containing layer; (V) stripping the organic-silicone resin containing layer; wherein the weight ratio of said silane to said water or to said mixture of water and condensation catalyst is constant throughout said method.
Claim 16
Independent Claim
131 words
A method for making a silicone resin, the method comprising the steps of: (I) mixing in a continuous manner a silane selected from the group consisting of: (i) alkoxysilanes, (ii) halogenated silanes, and (iii) alkyl silicates with a silicon compound selected from the group consisting of: (iv) trialkylhalosilanes and (v) disiloxanes; (II) adding an alcohol to the mixture of (I); (III) adding water or a mixture of water and a condensation catalyst to the mixture of (II) whereby an aqueous layer and an organic-silicone resin containing layer are formed; (IV) separating the aqueous layer from the organic-silicone resin containing layer; (V) stripping the organic-silicone resin containing layer; wherein the weight ratio of said silane to said water or to said mixture of water and condensation catalyst is constant throughout said method.
Claim 17
Dependent Claim
41 words
A method according to claim 14, wherein (i) is a silane having the formula Si(OR) 4 wherein R is a group selected from the group consisting of alkyl groups having from 1 to 6 carbon atoms, aryl groups, and arylalkyl groups.
Claim 18
Dependent Claim
19 words
A method according to claim 15, wherein (i) is selected from the group consisting of tetramethoxysilane, tetraethoxysilane, and tetrapropoxysilane.
Claim 19
Dependent Claim
21 words
A method according to claim 14, wherein (ii) is a compound having the formula SiX 4 wherein X is a halogen.
Claim 20
Dependent Claim
10 words
A method according to claim 17, wherein X is chlorine.
Claim 21
Dependent Claim
60 words
A method according to claim 14, wherein (iii) is an alkyl silicate having units of the formula ##EQU5## or a partial hydrolysis condensate thereof, wherein R 1 is a group selected from the group consisting of alkyl groups having from 1 to 6 carbon atoms, aryl groups, and arylalkyl groups, and a has a value of from 1 to 3.
Claim 22
Dependent Claim
10 words
A method according to claim 19, wherein (iii) is ethylpolysilicate.
Claim 23
Dependent Claim
82 words
A method according to claim 14, wherein (iv) is a compound having the formula R 2 R 3 R 4 SiY wherein R 2 , R 3 and R 4 are selected from hydrogen, alkyl groups having from 1 to 12 carbon atoms, alkenyl groups having from 2 to 12 carbon atoms, aryl groups, arylalkyl groups, or perfluoroalkylethyl groups having the formula C n F 2n+1 CH 2 CH 2 where n is 1 to 6, and Y is a halogen atom.
Claim 24
Dependent Claim
10 words
A method according to claim 21, wherein Y is chlorine.
Claim 25
Dependent Claim
24 words
A method according to claim 21, wherein (iv) is selected from the group consisting of trimethylchlorosilane, triethylchlorosilane, trimethylbromosilane, triethylbromosilane, trimethylfluorosilane, triethylfluorosilane, dimethylvinylchlorosilane, and dimethyl-5-hexenylchlorosilane.
Claim 26
Dependent Claim
78 words
A method according to claim 14, wherein (v) is a disiloxane having the formula (R 5 R 6 R 7 Si) 2 O wherein R 5 , R 6 and R 7 are selected from hydrogen, alkyl groups having from 1 to 12 carbon atoms, alkenyl groups having from 2 to 12 carbon atoms, aryl groups, arylalkyl groups, and perfluoroalkylethyl groups having the formula C n F 2n+1 CH 2 CH 2 where n is 1 to 6.
Claim 27
Dependent Claim
25 words
A method according to claim 24, wherein the disiloxane is selected from the group consisting of tetramethyldisiloxane, hexamethyldisiloxane, tetramethyldivinylsiloxane, tetramethyldi-5-hexenylsiloxane, tetramethyl-3,3,3-trifluoropropyldisiloxane, tetramethyldiethylsiloxane, tetramethyldiphenyldisiloxane, and diethyldiphenyldivinyldisiloxane.
Claim 28
Dependent Claim
20 words
A method according to claim 14, wherein the alcohol is selected from the group consisting of ethanol, methanol, and isopropanol.
Claim 29
Dependent Claim
24 words
A method according to claim 14, wherein the condensation catalyst is selected from the group consisting of hydrochloric acid, sulfuric acid, and sulfonic acids.
Claim 30
Dependent Claim
8 words
A composition produced in accordance with claim 1.
Claim 31
Dependent Claim
8 words
A composition produced in accordance with claim 14.
Claim 32
Dependent Claim
14 words
A method according to claim 14, further comprising heating the mixture after step (III).
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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) | 1998-02-20 | 1998-08-22 | 1999-02-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2002-02-20 | 2002-08-22 | 2003-02-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2006-02-20 | 2006-08-22 | 2007-02-21 | $7700.00 | Window Closed / Lapsed |