US4399266A
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Laddery lower alkylpolysilsesquioxane having heat-resistant thin film-formability and process for preparing same
Assignee: JSR Corp
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Filing: 1982-03-02
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Granted: 1983-08-16
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Expires: 2002-03-02
Abstract
Abstract A laddery lower alkylpolysilsesquioxane represented by the formula: ##STR1## wherein R and R' represent same or different lower alkyl groups, and n represents an average degree of polymerization, said laddery lower alkylpolysilsesquioxane having a heat-resistant thin film-formability, characterized in that 15 to 30% by weight of the lower alkylpolysilsesquioxane is occupied by the portion having a standard polystyrene-reduced molecular weight of 20,000 or less as measured by gel permeation chromatography. Said silicone resin in which R and R' are methyl is prepared by dissolving CH 3 SiCl 3 in a ketone or an ether, adding water to this solution with stirring to hydrolyze CH 3 SiCl 3 , condensing the hydrolyzate and, if necessary, subjecting the resulting condensate to a treatment for adjusting the proportion of the low molecular weight portion in the product.
Inventors
- 👤 Yoshio Matsumura
- 👤 Ikuo Nozue
- 👤 Osahiko Tomomitsu
- 👤 Takashi Ukachi
- 👤 Taro Suminoe
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 17:14
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/06; C08G77/32
Claims Analysis
Total Claims: 30
Claim 1
Independent Claim
71 words
A laddery lower alkylpolysilsesquioxane having a heat resistant thin film-formability represented by the formula: ##STR3## wherein R and R' represent same or different lower alkyl groups, and n is an average degree of polymerization, characterized in that 15 to 30% by weight of the laddery lower alkylpolysilsesquioxane is occupied by the low molecular weight portion having a standard polystyrene-reduced molecular weight of 20,000 or less as measured by gel permeation chromatography.
Claim 2
Dependent Claim
71 words
A laddery lower alkylpolysilsesquioxane having a heat resistant thin film-formability represented by the formula: ##STR3## wherein R and R' represent same or different lower alkyl groups, and n is an average degree of polymerization, characterized in that 15 to 30% by weight of the laddery lower alkylpolysilsesquioxane is occupied by the low molecular weight portion having a standard polystyrene-reduced molecular weight of 20,000 or less as measured by gel permeation chromatography.
Claim 3
Dependent Claim
24 words
The laddery lower alkylpolysilsesquioxane according to claim 1, wherein R and R' in the formula are independently methyl groups, ethyl groups or n-propyl groups.
Claim 4
Dependent Claim
20 words
The laddery lower alkylpolysilsesquioxane according to claim 1 or 2, wherein R and R' in the formula are the same.
Claim 5
Dependent Claim
19 words
The laddery lower alkylpolysilsesquioxane according to claim 1, wherein R and R' in the formula are both methyl groups.
Claim 6
Dependent Claim
31 words
The laddery lower alkylpolysilsesquioxane according to claim 1, 2, or 4, wherein the standard polystyrene-reduced weight average molecular weight of the whole of the laddery lower alkylpolysilsesquioxane is 40,000 to 500,000.
Claim 7
Dependent Claim
29 words
The laddery lower alkylpolysilsesquioxane according to claim 1, 2, or 4, wherein the standard polystyrene-reduced weight average molecular weight of the whole of the laddery lower alkylpolysilsesquioxane is 50,000-300,000.
Claim 8
Dependent Claim
24 words
The laddery lower alkylpolysilsesquioxane according to claim 5, wherein the low molecular weight portion has a standard polystyrene-reduced molecular weight of 800 to 20,000.
Claim 9
Dependent Claim
122 words
A process for preparing a laddery methylpolysilsesquioxane represented by the formula: ##STR4## wherein n is a degree of polymerization, which comprises dissolving CH 3 SiCl 3 in an organic solvent mixture comprising a ketone or an ether in an amount of 50% by volume or more, adding water to the resulting organic solvent solution with stirring to hydrolyze CH 3 SiCl 3 , then condensing the hydrolyzate and adjusting the molecular weight distribution of the product by a fractionation, a fractional gel permeation chromatography or a blending method so that the low molecular weight portion having a standard polystyrene-reduced molecular weight of 20,000 or less as measured by gel permeation chromatography is contained in a proportion of 15 to 30% by weight.
Claim 10
Dependent Claim
122 words
A process for preparing a laddery methylpolysilsesquioxane represented by the formula: ##STR4## wherein n is a degree of polymerization, which comprises dissolving CH 3 SiCl 3 in an organic solvent mixture comprising a ketone or an ether in an amount of 50% by volume or more, adding water to the resulting organic solvent solution with stirring to hydrolyze CH 3 SiCl 3 , then condensing the hydrolyzate and adjusting the molecular weight distribution of the product by a fractionation, a fractional gel permeation chromatography or a blending method so that the low molecular weight portion having a standard polystyrene-reduced molecular weight of 20,000 or less as measured by gel permeation chromatography is contained in a proportion of 15 to 30% by weight.
Claim 11
Dependent Claim
22 words
The process according to claim 8, wherein the low molecular weight portion has a standard polystyrene-reduced molecular weight of 800 to 20,000.
Claim 12
Dependent Claim
27 words
The process according to claim 8 or 9, wherein the laddery methylpolysilsesquioxane as the whole has a standard polystyrene-reduced weight average molecular weight of 40,000 to 500,000.
Claim 13
Dependent Claim
31 words
The process according to claim 8, or 9, wherein CH 3 SiCl 3 is dissolved in an organic solvent comprising a ketone in an amount of 50% by volume or more.
Claim 14
Dependent Claim
26 words
The process according to claim 8, or 9, wherein the organic solvent is composed only of a ketone or a mixture of two or more ketones.
Claim 15
Dependent Claim
25 words
The process according to claim 11, wherein the ketones are selected from the group consisting of methyl ethyl ketone, diethyl ketone and methyl isobutyl ketone.
Claim 16
Dependent Claim
31 words
The process according to claim 8, or 9, wherein CH 3 SiCl 3 is dissolved in an organic solvent comprising an ether in an amount of 50% by volume or more.
Claim 17
Dependent Claim
26 words
The process according to claim 8, or 9, wherein the organic solvent is composed only of an ether or a mixture of two or more ethers.
Claim 18
Dependent Claim
29 words
The process according to claim 14, wherein the ethers are selected from the group consisting of ethylene glycol dimethyl ether, di-normal propyl ether, dioxane, and diethylene glycol dimethyl ether.
Claim 19
Dependent Claim
42 words
The process according to claim 8, or 9, wherein the organic solvent mixture further comprises an aliphatic hydrocarbon, an aromatic hydrocarbon, a halogenated hydrocarbon, an aliphatic alcohol or a fatty acid alkyl ester in an amount of less than 50% by volume.
Claim 20
Dependent Claim
32 words
The process according to claim 8, or 9, wherein the amount of the ketone used is 5 to 20 parts by volume per part by volume of CH 3 SiCl 3 .
Claim 21
Dependent Claim
32 words
The process according to claim 8, or 9, wherein the amount of the ether used is 5 to 20 parts by volume per part by volume of CH 3 SiCl 3 .
Claim 22
Dependent Claim
28 words
The process according to claim 8, or 9, wherein water is used in an amount of 3 to 30 moles per mole of CH 3 SiCl 3 .
Claim 23
Dependent Claim
17 words
The process according to claim 8, or 9, wherein the condensation temperature is 130° C. or below.
Claim 24
Dependent Claim
18 words
The process according to claim 8, or 9, wherein the condensation temperature is from 80° to 120° C.
Claim 25
Dependent Claim
21 words
The process according to claim 22, wherein the condensation reaction is carried out for a period of 2 to 6 hours.
Claim 26
Dependent Claim
21 words
The process according to claim 8, or 9, wherein the condensation reaction is carried out in the presence of an amine.
Claim 27
Dependent Claim
19 words
The process according to claim 24, wherein the amine is triethylamine, tri-normal propylamine, triisopropylamine, diethylamine, ethylamine, pyridine or ethylenediamine.
Claim 28
Dependent Claim
13 words
The process according to claim 24, wherein the amine is triethylamine or diethylamine.
Claim 29
Dependent Claim
28 words
The process according to claim 24, wherein the amine is used in an amount of about 3 moles or less per mole of CH 3 SiCl 3 .
Claim 30
Dependent Claim
27 words
The process according to claim 24, wherein the amine is used in an amount of 0.3 to 2 mols per mole of CH 3 SiCl 3 .
References Cited (Backward Citations)
US3000858A
Cited
US3017385A
Cited
US3234179A
Cited
US3318844A
Cited
US3372133A
Cited
US3355399A
Cited
US4273420A
Cited
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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) | 1986-08-15 | 1987-02-14 | 1987-08-16 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-08-15 | 1991-02-14 | 1991-08-16 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-08-15 | 1995-02-14 | 1995-08-16 | $7700.00 | Window Closed / Lapsed |