Patent US4766823A successfully refreshed from Google Patents.
Patent US5010159A successfully refreshed from Google Patents.
US5010159A
Expired / Lapsed
US
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Process for the synthesis of soluble, condensed hydridosilicon resins containing low levels of silanol
Assignee: Dow Silicones Corp
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Filing: 1989-09-01
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Granted: 1991-04-23
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Expires: 2009-09-01
Abstract
Abstract This invention relates to an improved method of hydrolyzing hydridosilanes with 2 or more hydrolyzable groups which comprises forming an arylsulfonic acid hydrate containing reaction medium, adding the silane to the hydrolysis medium, facilitating hydrolysis of the silane to form the polyester, settling the hydrolysis medium and polymer into an acid layer and an organic layer containing the polymer, separating the organic layer from the acid layer, contacting the organic layer with a neutralizing agent, and removing the neutrailizing agent from the organic layer.
Inventors
- 👤 Howard M. Bank
- 👤 Martin E. Cifuentes
- 👤 Theresa E. Martin
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 05:10
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/12; C08G77/06
Claims Analysis
Total Claims: 40
Claim 1
Independent Claim
142 words
A method of hydrolyzing a silane of the formula H a SiX 4-a where a is 1 or 2 and X is a hydrolyzable group, to produce polymers containing units of the formula H a SiO.sub.( 4-a)/2, the method comprising: forming a hydrolysis medium containing an arylsulfonic acid hydrate. adding a the silane to the agitated hydrolysis medium, facilitating hydrolysis of the silane in the hydrolysis medium to form the polymer, settling the hydrolysis medium and polymer into immiscible layers comprising an acid layer and an organic layer where the organic layer contains the polymer, separating the organic layer from the acid layer, contacting the organic layer with a neutralizing agent sufficiently basic to neutralize the remaining acid species but insufficiently basic to catalyze rearrangement of the polymer or solvolysis of silicon hydrides, and separating the organic layer from the neutralizing agent.
Claim 2
Independent Claim
142 words
A method of hydrolyzing a silane of the formula H a SiX 4-a where a is 1 or 2 and X is a hydrolyzable group, to produce polymers containing units of the formula H a SiO.sub.( 4-a)/2, the method comprising: forming a hydrolysis medium containing an arylsulfonic acid hydrate. adding a the silane to the agitated hydrolysis medium, facilitating hydrolysis of the silane in the hydrolysis medium to form the polymer, settling the hydrolysis medium and polymer into immiscible layers comprising an acid layer and an organic layer where the organic layer contains the polymer, separating the organic layer from the acid layer, contacting the organic layer with a neutralizing agent sufficiently basic to neutralize the remaining acid species but insufficiently basic to catalyze rearrangement of the polymer or solvolysis of silicon hydrides, and separating the organic layer from the neutralizing agent.
Claim 3
Dependent Claim
19 words
The method of claim 1 wherein the resultant polymer contains 100-2000 ppm hydroxyl groups attached to the silicon atom.
Claim 4
Dependent Claim
52 words
The method of claim 1 wherein the liquid containing the silane further comprises one or more organosilanes of the formulas RaSiX4-a or R'RSiX 2 where a is one or two, X is a hydrolyzable group, R is alkyl, aryl, unsaturated hydrocarbon, substituted alkyl or substituted aryl and R' is R or H.
Claim 5
Dependent Claim
78 words
The method of claim 3 wherein the liquid containing the silane comprises mixtures of silanes selected from the group consisting of: HSiX3 and RSiX3; HSiX3 and RR'SiX 2 ; HSiX3, RR'SiX 2 and H 2 SiX 2; and HSiX3 and H 2 SiX 2 wherein R is alkyl, a cycloalkyl, a cycloalkenyl, an aryl, an unsaturated hydrocarbon, or any of the above groups substituted with halogens, alkyls or aryls, R' is R or H and X=a hydrolyzable group.
Claim 6
Dependent Claim
20 words
The method of claim 1 wherein the liquid containing the silane consists essentially of the silane and a hydrocarbon solvent.
Claim 7
Dependent Claim
30 words
The method of claim 5 wherein the hydrocarbon solvent consists of one or more solvents selected from the group consisting of the aliphatics, aromatics, cycloaliphatics, halogenated aliphatics and halogenated aromatics.
Claim 8
Dependent Claim
11 words
The method of claim 6 wherein the hydrocarbon solvent is toluene.
Claim 9
Dependent Claim
32 words
The method of claim 1 wherein the hydrolyzable groups are independently selected from the group consisting of (a) organic groups linked to the silicon atom by an oxygen bond and (b) halogens.
Claim 10
Dependent Claim
32 words
The method of claim 6 wherein the hydrolyzable groups are independently selected from the group consisting of (a) organic groups linked to the silicon atom by an oxygen bond and (b) halogens.
Claim 11
Dependent Claim
10 words
The method of claim 6 wherein the silane is trichlorosilane.
Claim 12
Dependent Claim
10 words
The method of claim 7 wherein the silane is trichlorosilane.
Claim 13
Dependent Claim
20 words
The method of claim 1 wherein the hydrolysis medium is formed by combining an aromatic hydrocarbon and concentrated sulfuric acid.
Claim 14
Dependent Claim
20 words
The method of claim 9 wherein the hydrolysis medium is formed by combining an aromatic hydrocarbon and concentrated sulfuric acid.
Claim 15
Dependent Claim
20 words
The method of claim 1 wherein the hydrolysis medium is formed by diluting an arylsulfonic acid hydrate in a solvent.
Claim 16
Dependent Claim
20 words
The method of claim 12 wherein the aromatic hydrocarbon is selected from the group consisting of benzene, toluene and xylene.
Claim 17
Dependent Claim
20 words
The method of claim 13 wherein the aromatic hydrocarbon is selected from the group consisting of benzene, toluene and xylene.
Claim 18
Dependent Claim
11 words
The method of claim 13 wherein the aromatic hydrocarbon is toluene.
Claim 19
Dependent Claim
23 words
The method of claim 12 wherein the concentrated sulfuric acid is treated with fuming sulfuric acid to consume the bulk of water present.
Claim 20
Dependent Claim
23 words
The method of claim 16 wherein the concentrated sulfuric acid is treated with fuming sulfuric acid to consume the bulk of water present.
Claim 21
Dependent Claim
18 words
The method of claim 1 wherein the hydrolysis medium is formed prior to the addition of the silane.
Claim 22
Dependent Claim
17 words
The method of claim 19 wherein the hydrolysis medium is formed prior to the addition of silane.
Claim 23
Dependent Claim
19 words
The method of claim 1 wherein the separated organic layer is washed with aqueous sulfuric acid prior to neutralization.
Claim 24
Dependent Claim
19 words
The method of claim 21 wherein the separated organic layer is washed with aqueous sulfuric acid prior to neutralization.
Claim 25
Dependent Claim
27 words
The method of claim 1 wherein the neutralizing agent is selected from the group consisting of calcium carbonate, sodium carbonate, sodium bicarbonate, calcium oxide and calcium hydroxide.
Claim 26
Dependent Claim
27 words
The method of claim 9 wherein the neutralizing agent is selected from the group consisting of calcium carbonate, sodium carbonate, sodium bicarbonate, calcium oxide and calcium hydroxide.
Claim 27
Dependent Claim
27 words
The method of claim 13 wherein the neutralizing agent is selected from the group consisting of calcium carbonate, sodium carbonate, sodium bicarbonate, calcium oxide and calcium hydroxide.
Claim 28
Dependent Claim
27 words
The method of claim 23 wherein the neutralizing agent is selected from the group consisting of calcium carbonate, sodium carbonate, sodium bicarbonate, calcium oxide and calcium hydroxide.
Claim 29
Dependent Claim
12 words
The method of claim 23 wherein the neutralizing agent is calcium carbonate.
Claim 30
Dependent Claim
33 words
The method of claim 1 further comprising drying or filtering the neutralized organic layer with an agent which insures that any water soluble salts formed during neutralization or any other insolubles are removed.
Claim 31
Dependent Claim
33 words
The method of claim 16 further comprising drying or filtering the neutralized organic layer with an agent which insures that any water soluble salts formed during neutralization or any other insolubles are removed.
Claim 32
Dependent Claim
33 words
The method of claim 27 further comprising drying or filtering the neutralized organic layer with an agent which insures that any water soluble salts formed during neutralization or any other insolubles are removed.
Claim 33
Dependent Claim
14 words
The method of claim 29 further comprising recovering the polymer by evaporating the solvents.
Claim 34
Dependent Claim
14 words
The method of claim 30 further comprising recovering the polymer by evaporating the solvents.
Claim 35
Dependent Claim
14 words
The method of claim 31 further comprising recovering the polymer by evaporating the solvents.
Claim 36
Dependent Claim
15 words
The method of claim 29 further comprising performing a solvent exchange in the organic layer.
Claim 37
Dependent Claim
15 words
The method of claim 30 further comprising performing a solvent exchange in the organic layer.
Claim 38
Dependent Claim
15 words
The method of claim 31 further comprising performing a solvent exchange in the organic layer.
Claim 39
Independent Claim
148 words
A method of hydrolyzing a silane of the formula HSiCl 3 to produce a polymer containing units of the formula HSiO 3/2 , the method comprising: forming a toluenesulfonic acid hydrate hydrolysis medium by combining toluene and concentrated sulfuric acid, adding trichlorosilane dissolved in toluene to the agitated hydrolysis medium, facilitating hydrolysis of the silane in the hydrolysis medium to form the polymer, settling the hydrolysis medium and polymer into immiscible layers comprising an acid layer and an organic layer where the organic layer contains the polymer and toluene, separating the organic layer from the acid layer and washing the organic layer with aqueous sulfuric acid, contacting the organic layer with calcium carbonate to neutralize the remaining acid species, separating the organic layer from the calcium carbonate, contacting the neutralized organic layer with a drying agent, separating the organic layer from the drying agent, and evaporating the solvent.
Claim 40
Independent Claim
148 words
A method of hydrolyzing a silane of the formula HSiCl 3 to produce a polymer containing units of the formula HSiO 3/2 , the method comprising: forming a toluenesulfonic acid hydrate hydrolysis medium by combining toluene and concentrated sulfuric acid, adding trichlorosilane dissolved in toluene to the agitated hydrolysis medium, facilitating hydrolysis of the silane in the hydrolysis medium to form the polymer, settling the hydrolysis medium and polymer into immiscible layers comprising an acid layer and an organic layer where the organic layer contains the polymer and toluene, separating the organic layer from the acid layer and washing the organic layer with aqueous sulfuric acid, contacting the organic layer with calcium carbonate to neutralize the remaining acid species, separating the organic layer from the calcium carbonate, contacting the neutralized organic layer with a drying agent, separating the organic layer from the drying agent, and evaporating the solvent.
References Cited (Backward Citations)
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| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1994-04-22 | 1994-10-22 | 1995-04-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1998-04-22 | 1998-10-22 | 1999-04-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2002-04-22 | 2002-10-22 | 2003-04-23 | $7700.00 | Window Closed / Lapsed |