US5527873A
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US
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Method for the preparation of silicone resins
Assignee: DuPont Toray Specialty Materials KK
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Filing: 1995-02-17
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Granted: 1996-06-18
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Expires: 2015-02-17
Abstract
Abstract The present invention relates to a method for the preparation of silicone resins, the method comprising the steps of (I) mixing (a) a silicone resin, (b) an organic solvent, and (c) an acid catalyst to form a reaction product, and (II) reacting a diorganopolysiloxane or tetraorganodisiloxane with the reaction product of (I) at a temperature of 50° C. to 150° C. The present invention also relates to resins produced by the method of the present invention.
Inventors
- 👤 Hideki Kobayashi
- 👤 Wataru Nishiumi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 23:42
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/06; C08G77/12
Claims Analysis
Total Claims: 23
Claim 1
Independent Claim
149 words
A method for the preparation of silicone resins, the method comprising the steps of: (I) mixing: (a) a silicone resin having the average unit formula (R 3 SiO 1/2 ) x (SiO 4/2 ); (b) an organic solvent; and (c) an acid catalyst; wherein each R is independently selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, and x has a value of from 0.2 to 3 to form a dehydration condensation reaction product; and (II) reacting the reaction product of (I) at a temperature of 50° C. to 150° C. with: (d) a diorganopolysiloxane having the average unit formula (R 1 HSiO 2/2 ) y (R 1 SiO 2/2 ) z wherein R 1 is independently selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, y has a value of 1 to 100, and z has a value of 0 to 100.
Claim 2
Independent Claim
149 words
A method for the preparation of silicone resins, the method comprising the steps of: (I) mixing: (a) a silicone resin having the average unit formula (R 3 SiO 1/2 ) x (SiO 4/2 ); (b) an organic solvent; and (c) an acid catalyst; wherein each R is independently selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, and x has a value of from 0.2 to 3 to form a dehydration condensation reaction product; and (II) reacting the reaction product of (I) at a temperature of 50° C. to 150° C. with: (d) a diorganopolysiloxane having the average unit formula (R 1 HSiO 2/2 ) y (R 1 SiO 2/2 ) z wherein R 1 is independently selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, y has a value of 1 to 100, and z has a value of 0 to 100.
Claim 3
Dependent Claim
26 words
A method according to claim 1, wherein R is selected from the group consisting of alkyl groups, alkenyl groups, aryl groups, aralkyl groups, and haloalkyl groups.
Claim 4
Dependent Claim
22 words
A method according to claim 2, wherein the alkyl group is methyl, and the alkenyl group is selected from vinyl or hexenyl.
Claim 5
Dependent Claim
15 words
A method according to claim 1, wherein x has a value of 0.6 to 1.1.
Claim 6
Dependent Claim
23 words
A method according to claim 1, wherein (b) is selected from the group consisting of aromatic hydrocarbons, alkanes, ethers, ketones, halohydrocarbons, and alcohols.
Claim 7
Dependent Claim
65 words
A method according to claim 5, wherein the aromatic hydrocarbons are selected from benzene, toluene, or xylene, the alkanes are selected from hexane or heptane, the ethers are selected from diethyl ether or tetrahydrofuran, the ketones are selected from acetone or methyl isobutyl ketone, the halohydrocarbons are selected from 1,1,2-trichlorotrifluoroethane, 1,1,1-trichloroethane, dichloromethane, alpha,alpha,alpha-trifluorotoluene, or hexafluoroxylene, and the alcohols are selected from methanol, ethanol, or isopropanol.
Claim 8
Dependent Claim
29 words
A method according to claim 1, wherein (c) is selected from the group consisting of sulfuric acid, trifluoromethanesulfonic acid, dodecylbenzenesulfonic acid, acid clay, and sulfonic acid group-containing organic resins.
Claim 9
Dependent Claim
60 words
A silicone resin having the average unit formula: (R.sup.2.sub.3 SiO.sub.1/2).sub.a (R.sup.2 HSiO.sub.2/2).sub.b (R.sup.2.sub.2 SiO.sub.2/2).sub.c (SiO.sub.4/2) wherein R 2 is selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, a has a value of 0.2 to 3, b has a value of from greater than zero to 2, and c has a value of from 0 to 2.
Claim 10
Dependent Claim
60 words
A silicone resin having the average unit formula: (R.sup.2.sub.3 SiO.sub.1/2).sub.a (R.sup.2 HSiO.sub.2/2).sub.b (R.sup.2.sub.2 SiO.sub.2/2).sub.c (SiO.sub.4/2) wherein R 2 is selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, a has a value of 0.2 to 3, b has a value of from greater than zero to 2, and c has a value of from 0 to 2.
Claim 11
Dependent Claim
27 words
A resin according to claim 8, wherein R 2 is selected from the group consisting of alkyl groups, alkenyl groups, aryl groups, aralkyl groups, and haloalkyl groups.
Claim 12
Dependent Claim
22 words
A resin according to claim 9, wherein the alkyl group is methyl, and the alkenyl group is selected from vinyl or hexenyl.
Claim 13
Independent Claim
143 words
A method for the preparation of silicone resins, the method comprising the steps of: (I) mixing: (a) a silicone resin having the average unit formula (R 3 SiO 1/2 ) x (SiO 4/2 ); (b) an organic solvent; and (c) an acid catalyst; wherein each R is independently selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, and x has a value of from 0.2 to 3 to form a dehydration condensation reaction product; and (II) reacting the reaction product of (I) at a temperature of 50° C. to 150° C. with: (d) a tetraorganodisiloxane having the average unit formula (R 3 2 HSi) 2 O wherein R 3 is independently selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, y has a value of 1 to 100, and z has a value of 0 to 100.
Claim 14
Independent Claim
143 words
A method for the preparation of silicone resins, the method comprising the steps of: (I) mixing: (a) a silicone resin having the average unit formula (R 3 SiO 1/2 ) x (SiO 4/2 ); (b) an organic solvent; and (c) an acid catalyst; wherein each R is independently selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, and x has a value of from 0.2 to 3 to form a dehydration condensation reaction product; and (II) reacting the reaction product of (I) at a temperature of 50° C. to 150° C. with: (d) a tetraorganodisiloxane having the average unit formula (R 3 2 HSi) 2 O wherein R 3 is independently selected from the group consisting of monovalent hydrocarbon groups and haloalkyl groups, y has a value of 1 to 100, and z has a value of 0 to 100.
Claim 15
Dependent Claim
26 words
A method according to claim 11, wherein R is selected from the group consisting of alkyl groups, alkenyl groups, aryl groups, aralkyl groups, and haloalkyl groups.
Claim 16
Dependent Claim
22 words
A method according to claim 12, wherein the alkyl group is methyl, and the alkenyl group is selected from vinyl or hexenyl.
Claim 17
Dependent Claim
23 words
A method according to claim 11, wherein (b) is selected from the group consisting of aromatic hydrocarbons, alkanes, ethers, ketones, halohydrocarbons, and alcohols.
Claim 18
Dependent Claim
65 words
A method according to claim 14, wherein the aromatic hydrocarbons are selected from benzene, toluene, or xylene, the alkanes are selected from hexane or heptane, the ethers are selected from diethyl ether or tetrahydrofuran, the ketones are selected from acetone or methyl isobutyl ketone, the halohydrocarbons are selected from 1,1,2-trichlorotrifluoroethane, 1,1,1-trichloroethane, dichloromethane, alpha,alpha,alpha-trifluorotoluene, or hexafluoroxylene, and the alcohols are selected from methanol, ethanol, or isopropanol.
Claim 19
Dependent Claim
29 words
A method according to claim 11, wherein (c) is selected from the group consisting of sulfuric acid, trifluoromethanesulfonic acid, dodecylbenzenesulfonic acid, acid clay, and sulfonic acid group-containing organic resins.
Claim 20
Dependent Claim
35 words
A method according to claim 11, wherein (d) is a compound having its average unit formula selected from: (HMe 2 Si) 2 O or (HMeEtSi) 2 O wherein Me denotes methyl and Et denotes ethyl.
Claim 21
Dependent Claim
100 words
A method according to claim 1, wherein (a) is a compound having its average unit formula selected from the groups consisting of: (Me 3 SiO 1/2 ) 0 .4 (SiO 4/2 ), (Me 3 SiO 1/2 ) 0 .3 (CH 2 ═CHSiMe 2 O 1/2 ) 0 .1 (SiO 4/2 ), (Me 3 SiO 1/2 ) 0 .4 (CH 2 ═CHC 4 H 8 SiMe 2 O 1/2 ) 0 .1 (SiO 4/2 ), and (Me 3 SiO 1/2 ) 0 .4 (C 8 H 17 SiMe 2 O 1/2 ) 0 .1 (SiO 4/2 ) wherein Me denotes methyl.
Claim 22
Dependent Claim
89 words
A method according to claim 1, wherein (d) is a compound having its average unit formula selected from the group consisting of: Me 3 SiO(HMeSiO 2/2 ) 20 SiMe 3 , Me 3 SiO(HMe 3 SiO 2/2 ) 15 (Me 2 SiO 2/2 ) 5 SiMe 3 , Me 3 SiO(HMeSiO 2/2 ) 10 (C 3 H 7 Me 2 SiO 2/2 ) 3 SiMe 3 , (HMe 2 SiO 2/2 ) 4 , and (HMeSiO 2/2 ) 2 (Me 2 SiO 2/2 ) 2 wherein Me denotes methyl.
Claim 23
Dependent Claim
100 words
A method according to claim 11, wherein (a) is a compound having its average unit formula selected from the groups consisting of: (Me 3 SiO 1/2 ) 0 .4 (SiO 4/2 ), (Me 3 SiO 1/2 ) 0 .3 (CH 2 ═CHSiMe 2 O 1/2 ) 0 .1 (SiO 4/2 ), (Me 3 SiO 1/2 ) 0 .4 (CH 2 ═CHC 4 H 8 SiMe 2 O 1/2 ) 0 .1 (SiO 4/2 ), and (Me 3 SiO 1/2 ) 0 .4 (C 8 H 17 SiMe 2 O 1/2 ) 0 .1 (SiO 4/2 ) wherein Me denotes methyl.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1999-06-18 | 1999-12-18 | 2000-06-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2003-06-18 | 2003-12-18 | 2004-06-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2007-06-18 | 2007-12-18 | 2008-06-18 | $7700.00 | Window Closed / Lapsed |