Patent EP0776925A2 successfully refreshed from Google Patents.
EP0776925A2
Expired / Lapsed
EP
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Coating film having water repellency and low refractive index
Assignee: Nissan Chemical Corp
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Filing: 1996-11-18
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Granted: —
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Expires: 2016-11-18
Abstract
Abstract A process for forming a coating film on a substrate surface, which comprises preparing a reaction mixture comprising a silicon compound (A) of the following formula (1): Si(OR 4 ) (1) wherein R is a C 1-5 alkyl group, a silicon compound (B) of the following formula (2): CF 3 (CF 2 )nCH 2 CH 2 Si(OR 1 ) 3 (2) wherein R 1 is a C 1-5 alkyl group, and n is an integer of from 0 to 12, an alcohol (C) of the following formula (3): R 2 CH 2 OH (3) wherein R 2 is a hydrogen atom, or an unsubstituted or substituted C 1-12 alkyl group, and oxalic acid (D), in a ratio of from 0.05 to 0.43 mol of the silicon compound (B) per mol of the silicon compound (A), in a ratio of from 0.5 to 100 mol of the alcohol (C) per mol of the total alkoxy groups contained in the silicon compounds (A) and (B), and in a ratio of from 0.2 to 2 mol of the oxalic acid (D) per mol of the total alkoxy groups contained in the silicon compounds (A) and (B); heating this reaction mixture at a temperature of from 50 to 180°C until the total amount of the silicon compounds (A) and (B) remaining in the reaction mixture becomes at most 5 mol%, while maintaining a SiO 2 concentration of from 0.5 to 10 wt% as calculated from silicon atoms in the reaction mixture and maintaining absence of water, to form a polysiloxane solution; then coating a coating fluid comprising the polysiloxane solution on a substrate surface to form a coating; and heat-curing the coating at a temperature of from 80 to 450°C to form a coating film having a refractive index of from 1.28 to 1.38 and a contact angle of water of from 90 to 115°, as adhered on the substrate surface.
Inventors
- 👤 Tatsuya Nissan Chem. Ind. Ltd. Nogami
- 👤 Takakazu Nissan Chem. Ind. Ltd. Nakada
- 👤 Rie Nissan Chem. Ind. Ltd. Sakai
- 👤 Takeshi Nissan Chem. Ind. Ltd. Hosoya
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-11-06 04:37
CPC Classifications
C; C09; C09D; C09D183/00; C09D183/04; C09D183/08; C03; C03C; C03C17/00; C03C17/34; C03C17/42; C08; C08G; C08G77/00; C08G77/04; C08G77/22; C08G77/24; C03C2217/00; C03C2217/70; C03C2217/73; C03C2217/732; Y; Y10; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31551; Y10T428/31609; Y10T428/31612; Y10T428/31652; Y10T428/31663; Y10T428/31667
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
317 words
A process for forming a coating film on a substrate surface, which comprises preparing a reaction mixture comprising a silicon compound (A) of the following formula (1): Si(OR 4 ) (1) wherein R is a C 1-5 alkyl group, a silicon compound (B) of the following formula (2): CF 3 (CF 2 )nCH 2 CH 2 Si(OR 1 ) 3 (2) wherein R 1 is a C 1-5 alkyl group, and n is an integer of from 0 to 12, an alcohol (C) of the following formula (3): R 2 CH 2 OH (3) wherein R 2 is a hydrogen atom, or an unsubstituted or substituted C 1-12 alkyl group, and oxalic acid (D), in a ratio of from 0.05 to 0.43 mol of the silicon compound (B) per mol of the silicon compound (A), in a ratio of from 0.5 to 100 mol of the alcohol (C) per mol of the total alkoxy groups contained in the silicon compounds (A) and (B), and in a ratio of from 0.2 to 2 mol of the oxalic acid (D) per mol of the total alkoxy groups contained in the silicon compounds (A) and (B); heating this reaction mixture at a temperature of from 50 to 180°C until the total amount of the silicon compounds (A) and (B) remaining in the reaction mixture becomes at most 5 mol%, while maintaining a SiO 2 concentration of from 0.5 to 10 wt% as calculated from silicon atoms in the reaction mixture and maintaining absence of water, to form a polysiloxane solution; then coating a coating fluid comprising the polysiloxane solution on a substrate surface to form a coating; and heat-curing the coating at a temperature of from 80 to 450°C to form a coating film having a refractive index of from 1.28 to 1.38 and a contact angle of water of from 90 to 115°, as adhered on the substrate surface.
Claim 2
Dependent Claim
28 words
The process according to Claim 1, wherein the silicon compound (A) is at least one silicon compound selected from the group consisting of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane and tetrabutoxysilane.
Claim 3
Dependent Claim
26 words
The process according to Claim 1, wherein the silicon compound (A) is at least one silicon compound selected from the group consisting of tetramethoxysilane and tetraethoxysilane.
Claim 4
Dependent Claim
35 words
The process according to any one of Claims 1 to 3, wherein the silicon compound (B) is at least one silicon compound selected from the group consisting of trifluoropropyltrimethoxysilane, trifluoropropyltriethoxysilane, tridecafluorooctyltrimethoxysilane, tridecafluorooctyltriethoxysilane, heptadecafluorodecyltrimethoxysilane and heptadecafluorodecyltriethoxysilane.
Claim 5
Dependent Claim
55 words
The process according to any one of Claims 1 to 4, wherein the alcohol (C) is at least one alcohol selected from the group consisting of methanol, ethanol, propanol, n-butanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, propylene glycol monomethyl ether and propylene glycol monoethyl ether.
Claim 6
Dependent Claim
17 words
The process according to any one of Claims 1 to 4, wherein the alcohol (C) is ethanol.
Claim 7
Dependent Claim
104 words
The process according to any one of Claims 1 to 6, wherein at least one alkyl alkoxysilane selected from the group consisting of methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, butyltrimethoxysilane, butyltriethoxysilane, pentyltrimethoxysilane, pentyltriethoxysilane, heptyltrimethoxysilane, heptyltriethoxysilane, octyltrimethoxysilane, octyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, hexadecyltrimethoxysilane, hexadecyltriethoxysilane, octadecyltrimethoxysilane, octadecyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, γ-methacryloxypropyltrimethoxysilane, γ-methacryloxypropyltriethoxysilane, dimethyldimethoxysilane and dimethyldiethoxysilane, is incorporated as a modifier (E) in an amount of from 0.02 to 0.2 mol per mol of the silicon compound (A) in addition to the silicon compound (A), the silicon compound (B), the alcohol (C) and the oxalic acid (D), in the preparation of the reaction mixture.
Claim 8
Dependent Claim
52 words
The process according to any one of Claims 1 to 7, wherein at least one sol selected from the group consisting of a silica sol, an alumina sol, a titania sol, a zirconia sol, a magnesium fluoride sol and a ceria sol, is incorporated as an additive (F) to the coating fluid.
Claim 9
Dependent Claim
306 words
A coating film having a refractive index of from 1.28 to 1.38 and a contact angle of water of from 90 to 115°, which is formed as adhered on a substrate surface, by preparing a reaction mixture comprising a silicon compound (A) of the following formula (1): Si(OR 4 ) (1) wherein R is a C 1-5 alkyl group, a silicon compound (B) of the following formula (2): CF 3 (CF 2 )nCH 2 CH 2 Si(OR 1 ) 3 (2) wherein R 1 is a C 1-5 alkyl group, and n is an integer of from 0 to 12, an alcohol (C) of the following formula (3): R 2 CH 2 OH (3) wherein R 2 is a hydrogen atom, or an unsubstituted or substituted C 1-12 alkyl group, and oxalic acid (D), in a ratio of from 0.05 to 0.43 mol of the silicon compound (B) per mol of the silicon compound (A), in a ratio of from 0.5 to 100 mol of the alcohol (C) per mol of the total alkoxy groups contained in the silicon compounds (A) and (B), and in a ratio of from 0.2 to 2 mol of the oxalic acid (D) per mol of the total alkoxy groups contained in the silicon compounds (A) and (B); heating this reaction mixture at a temperature of from 50 to 180°C until the total amount of the silicon compounds (A) and (B) remaining in the reaction mixture becomes at most 5 mol%, while maintaining a SiO 2 concentration of from 0.5 to 10 wt% as calculated from silicon atoms in the reaction mixture and maintaining absence of water, to form a polysiloxane solution; then coating a coating fluid comprising the polysiloxane solution on a substrate surface to form a coating; and heat-curing the coating at a temperature of from 80 to 450°C.
Claim 10
Dependent Claim
29 words
The coating film according to Claim 9, wherein the silicon compound (A) is at least one silicon compound selected from the group consisting of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane and tetrabutoxysilane.
Claim 11
Dependent Claim
27 words
The coating film according to Claim 9, wherein the silicon compound (A) is at least one silicon compound selected from the group consisting of tetramethoxysilane and tetraethoxysilane.
Claim 12
Dependent Claim
36 words
The coating film according to any one of Claims 9 to 11, wherein the silicon compound (B) is at least one silicon compound selected from the group consisting of trifluoropropyltrimethoxysilane, trifluoropropyltriethoxysilane, tridecafluorooctyltrimethoxysilane, tridecafluorooctyltriethoxysilane, heptadecafluorodecyltrimethoxysilane and heptadecafluorodecyltriethoxysilane.
Claim 13
Dependent Claim
56 words
The coating film according to any one of Claims 9 to 12, wherein the alcohol (C) is at least one alcohol selected from the group consisting of methanol, ethanol, propanol, n-butanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, propylene glycol monomethyl ether and propylene glycol monoethyl ether.
Claim 14
Dependent Claim
18 words
The coating film according to any one of Claims 9 to 12, wherein the alcohol (C) is ethanol.
Claim 15
Dependent Claim
105 words
The coating film according to any one of Claims 9 to 14, wherein at least one alkyl alkoxysilane selected from the group consisting of methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, butyltrimethoxysilane, butyltriethoxysilane, pentyltrimethoxysilane, pentyltriethoxysilane, heptyltrimethoxysilane, heptyltriethoxysilane, octyltrimethoxysilane, octyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, hexadecyltrimethoxysilane, hexadecyltriethoxysilane, octadecyltrimethoxysilane, octadecyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, γ-methacryloxypropyltrimethoxysilane, γ-methacryloxypropyltriethoxysilane, dimethyldimethoxysilane and dimethyldiethoxysilane, is incorporated as a modifier (E) in an amount of from 0.02 to 0.2 mol per mol of the silicon compound (A) in addition to the silicon compound (A), the silicon compound (B), the alcohol (C) and the oxalic acid (D), in the preparation of the reaction mixture.
Claim 16
Dependent Claim
53 words
The coating film according to any one of Claims 9 to 15, wherein at least one sol selected from the group consisting of a silica sol, an alumina sol, a titania sol, a zirconia sol, a magnesium fluoride sol and a ceria sol, is incorporated as an additive (F) to the coating fluid.
References Cited (Backward Citations)
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