CN102304323A - Room-temperature cured phenyl silicon resin conformal coating - Google Patents
Room-temperature cured phenyl silicon resin conformal coating Download PDFInfo
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Abstract
The invention discloses a room-temperature cured phenyl silicon resin conformal coating which comprises components A) a segmented copolymer of phenyl silicon resin and linear polyorganosiloxane or methyl phenyl silicon resin and linear polyorganosiloxane, B) alkoxy silane, C) a silane coupling agent containing amino or epoxy group, D) an organic titanium compound, E) organic phosphate flame retardant synergist, and (F) an organic hydrocarbon solvent or low molecular weight siloxane, wherein the organic hydrocarbon solvent is one or multiple of methylbenzene, dimethylbenzene, petroleum ether, cyclohexane and normal heptane; and the low molecular weight siloxane is a mixture of octamethyl-trisiloxan, octamethyl cyclotetrasiloxane or methyl cyclosiloxane. A product produced by the cured resin conformal coating of the invention has the advantages of very high transparency, good elasticity, tough and wearable surfaces as well as excellent high/low temperature performance, waterproofing, heat resistance, cold resistance, weathering resistance, ultraviolet ray resistance, medium resistance, irradiation resistance, flame retarding and the like.
Description
Technical field
The present invention relates to a kind of cold coating, be specifically related to a kind of phenyl polysiloxane coating type paint of ambient temperature curable.
Background technology
Along with science and technology development, existing nowadays meticulously in the harsh electronics applications sensitive circuit and component element long period, reliable protection are become more and more important with requiring numerous.As everyone knows, organosilicon material (like silicon rubber, silicon gel and silicone resin etc.) is widely used in the various electronic devices and components to play insulation, protection against the tide, the shockproof and relevant provide protection to electronic devices and components owing to having good comprehensive performances; One-component silicone rubber can at room temperature solidify, and dielectric properties are also better, but curing rear surface intensity and hardness are all lower, uses and receives certain restriction; Two-component silicone rubber applies or the embedding operation after the metering of two components need being mixed, and is unfavorable for the construction of efficient activity, also receives the constraint of operating time; Silicon gel transparency is very high, but curing rear surface hardness is lower, and very easily dust suction can't be applied in the severe environment of open air or exposure; Silicone resin can reach higher surface hardness and intensity after solidifying; But it is relatively poor that most of silicone resin (like methyl silicon resin, silicone glass resin etc.) solidify back toughness; Be prone to when being subjected to high/low-temperature impact be full of cracks, with device phenomenon such as come off; Most of in addition silicone resin needs hot setting (more than 150 ℃ even 200 ℃) usually; The top temperature that this not only can bear considerably beyond some electron device (like various printed circuit board assemblies), and high-temperature operation brings very large trouble also can for assembling production.The phenyl polysiloxane coating type paint of single-component ambient temperature curable is not only operated and is constructed simply, and the coating after solidifying simultaneously has the excellent comprehensive performance, is very ideal insulation protection material of various electronic circuit boards and components and parts.
Summary of the invention
The object of the present invention is to provide a kind of transparent phenyl polysiloxane coating type paint of ambient temperature curable.
The present invention realizes through following technical scheme:
This resin coating type paint mainly is made up of following component:
A) segmented copolymer of phenyl polysiloxane or methyl phenyl silicone resin and linear polysiloxane, phenyl polysiloxane wherein or methyl phenyl silicone resin are preferably made by phenyl trialkoxy silane or phenyl trialkoxy silane and the polycondensation of aminomethyl phenyl dialkoxy silicane cohydrolysis.
Linear polysiloxane viscosity wherein is 50～5000mpa.s, and its structural formula can be A1
Also can be A2
Preferred viscosities is 50～3000mpa.s, and structural formula is the linear polysiloxane of A1, and wherein n is the integer greater than zero; R
1, R
2Be methyl or phenyl, R
3Be methyl or ethyl.
B) have the organoalkoxysilane of following general structure:
Wherein R1 is methyl, ethyl, propyl group or carbonatoms more than or equal to 4 alkyl, preferred R
1Be methyl or ethyl; R
2Be methyl, ethyl or propyl group, preferred R
2Be methyl or ethyl; X is 3 or 4.
C) contain the silane coupling agent of amino or epoxy group(ing); Like γ-An Bingjisanjiayangjiguiwan, γ-An Bingjisanyiyangjiguiwan, γ-aminopropyl methyl dimethoxysilane, γ-aminopropyl methyldiethoxysilane, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan, N-(β-aminoethyl)-γ-An Bingjisanyiyangjiguiwan, γ-glycidyl ether oxygen propyl trimethoxy silicane, wherein preferred γ-An Bingjisanyiyangjiguiwan and γ-glycidyl ether oxygen propyl trimethoxy silicane.The mass fraction of Compound C in this coating type paint is 0.2%～5%.
D) organic titanic compound; Like isopropyl titanate, butyl (tetra) titanate, poly(tributoxy titanium), metatitanic acid four different monooctyl esters, purity titanium tetraethoxide, n-propyl titanate or organic titanium mixture; Like ethylacetoacetate titanium mixture, metatitanic acid four tert-butyl ester mixtures, titanium acetylacetone mixture; Wherein preferred isopropyl titanate, consumption is 0.05%～3% of this coating type paint mass fraction.
E) organophosphorus compounds retardant synergist; Like trichloroethyl phosphate, three (1; 3-two chloropropyls) phosphoric acid ester, tributyl phosphate, trioctyl phosphate, Tritolyl Phosphate, cumyl phenyl phosphate ester, wherein preferably phosphoric acid front three phenyl ester, cumyl phenyl phosphate ester.
F) organic hydrocarbon solvent such as toluene, xylenes, sherwood oil, hexanaphthene, normal heptane or low-molecular-weight siloxane be as solvent, wherein preferred toluene of organic hydrocarbon solvent or xylenes; Preferred octamethyltrisiloxane or octamethylcyclotetrasiloxane when low-molecular-weight siloxane is used as solvent.
A is own synthetic among the present invention, and B, C, D, E, F can obtain through known method.
Product after resin coating type paint provided by the invention solidifies has very high transparency, good elasticity and tough and tensile, attrition resistant surface; Have excellent high temperature performance, waterproof, heat-resisting, cold-resistant, weather-proof, UV resistant, media-resistant, anti-irradiation, characteristic such as fire-retardant simultaneously; This resin coating type paint has suitable viscosity in addition; Being easy to adopt multiple operating method such as spraying, dip-coating, brushing or flow coat, is very ideal insulation protection material of various electronic circuit boards and components and parts.
Embodiment
The present invention can further specify through following embodiment, but content of the present invention is not limited only to content related among the embodiment.
Embodiment 1
Add 300g phenyltrimethoxysila,e and 300g toluene in the 1L three-neck flask; At normal temperature and to stir fast down in flask dropping 60g mass fraction be 0.01% aqueous hydrochloric acid solution; The dropping time is controlled at about 20min; After aqueous hydrochloric acid solution dropwises temperature risen to 75 ℃ of back flow reaction 3h; After finishing, back flow reaction cools the temperature to 50 ℃ and add 1.06g HMDS stirring reaction 0.5h; Stop reaction afterwards; After leaving standstill, the reactant liquor cooling filters; With the reactant liquor after filtering be warming up to 120 ℃ distill out behind by-product carbinol and the partial solvent translucent phenyl polysiloxane 352g, the solid content of resin is 60%.
, the 1L three-necked flask of nitrogen protection and division box adds 190g in being housed by the phenyl polysiloxane of above-mentioned preparation, hydroxyl endblocked polydimethylsiloxane and the 278g toluene that 63g viscosity is 80mpa.s; In the presence of 110 ℃, nitrogen protection and catalyzer, carry out copolycondensation; Collect the water that polycondensation generates through water trap in the reaction process; Sustained reaction after 5～7 hours again underpressure distillation go out partial solvent and adjust reactant to certain solid content, final that viscosity be the phenyl polysiloxane and the linear polysiloxane segmented copolymer of 400mpa.s and transparent homogeneous.
Get 00 part of above-mentioned phenyl polysiloxane that makes and linear polysiloxane copolymer 1, add 5 parts of methyltrimethoxy silanes, 2 parts of γ-An Bingjisanyiyangjiguiwans, 0.1 part of Tritolyl Phosphate, 0.5 part of isopropyl titanate and 30 parts of toluene and mix the phenyl polysiloxane coating type paint I that obtains ambient temperature curable.
Embodiment 2
Add 220g phenyltrimethoxysila,e, 64g aminomethyl phenyl dimethoxy silane and 295g toluene in the 1L three-neck flask; At normal temperature and to stir fast down in flask dropping 73.3g mass fraction be 0.01% aqueous hydrochloric acid solution; The dropping time is controlled at about 20min; After aqueous hydrochloric acid solution dropwises temperature risen to 75 ℃ of back flow reaction 4.5h; After finishing, back flow reaction cools the temperature to 50 ℃ and add 1.29g HMDS stirring reaction 0.5h; Stop reaction afterwards; After leaving standstill, the reactant liquor cooling filters; With the reactant liquor after filtering be warming up to 120～130 ℃ of air-distillations go out behind by-product carbinol and the partial solvent translucent phenyl polysiloxane 325g, wherein the solid content of resin is about 55%.
, the 1L three-necked flask of nitrogen protection and division box adds 210g in being housed by the methyl phenyl silicone resin of above-mentioned preparation, hydroxyl endblocked polydimethylsiloxane and the 265g toluene that 70.4g viscosity is 80mpa.s; In the presence of 110 ℃, nitrogen protection and catalyzer, carry out copolycondensation; Collect the water that polycondensation generates through water trap in the reaction process; Sustained reaction after 6 hours underpressure distillation go out partial solvent and adjust reactant to certain solid content, final that viscosity be the methyl phenyl silicone resin of 350mpa.s and transparent homogeneous and the segmented copolymer of linear polysiloxane.
Get 00 part of the copolymer 1 of above-mentioned methyl phenyl silicone resin that makes and linear polysiloxane, add 5 parts of methyltrimethoxy silanes, 2 parts of γ-An Bingjisanyiyangjiguiwans, 0.1 part of Tritolyl Phosphate, 0.5 part of isopropyl titanate and 30 parts of toluene and mix the phenyl polysiloxane coating type paint II that obtains ambient temperature curable.
Embodiment 3
Adopt prepared phenyl polysiloxane among the embodiment 1, the hydroxyl endblocked polydimethylsiloxane of 80mpa.s viscosity among the embodiment 1 is replaced with the hydroxyl endblocked polydimethylsiloxane of 200mpa.s viscosity, all the other conditions are constant, make the coating type paint III.
Embodiment 4
Adopt prepared phenyl polysiloxane among the embodiment 1, the hydroxyl endblocked polydimethylsiloxane of 80mpa.s viscosity among the embodiment 1 is replaced with the hydroxyl endblocked polydimethylsiloxane of 1000mpa.s viscosity, all the other conditions are constant, make the coating type paint IV.
Embodiment 5
Phenyl polysiloxane consumption among the embodiment 1 is adjusted into 150g, and the hydroxyl endblocked polydimethylsiloxane consumption is adjusted into 72g, and all the other conditions are constant, makes the coating type paint V.
Embodiment 6
Phenyl polysiloxane consumption among the embodiment 1 is adjusted into 135g, and the hydroxyl endblocked polydimethylsiloxane consumption is adjusted into 86.6g, and all the other conditions are constant, makes the coating type paint VI.
Embodiment 7
All the other conditions are constant among the embodiment 1, and the consumption of methyltrimethoxy silane is adjusted into 8 parts, and the isopropyl titanate consumption is adjusted into 1.0 parts of whiles and does not add Tritolyl Phosphate, makes the coating type paint VII.
Embodiment 8
All the other conditions are constant among the embodiment 1, methyltrimethoxy silane is replaced with tetraethoxy do not add Tritolyl Phosphate simultaneously, make the coating type paint VIII.
Following table 1 has been listed the performance of 8 kinds of phenyl polysiloxane coating type paints of method for preparing.
*25 ℃/50%RH and 0.2mm thickness coatings
Claims (10)
1. the phenyl polysiloxane coating type paint of an ambient temperature curable, it is characterized in that: said coating comprises following component in percentage by weight:
A) segmented copolymer of the segmented copolymer of phenyl polysiloxane and linear polysiloxane or methyl phenyl silicone resin and linear polysiloxane; Wherein the mass ratio of phenyl polysiloxane or methyl phenyl silicone resin and linear polysiloxane is 0.5～3.0, and the mass fraction of above-mentioned segmented copolymer in this coating type paint is 40%～88%;
B) have the organoalkoxysilane of following general structure:
R wherein
1For methyl, ethyl, propyl group or carbonatoms more than or equal to 4 alkyl, preferred R
1Be methyl or ethyl; R
2Be methyl, ethyl or propyl group, preferred R
2Be methyl or ethyl; X is 3 or 4; The mass fraction of compd B in this coating type paint is 1%～10%;
C) contain the silane coupling agent of amino or epoxy group(ing); The mass fraction of Compound C in this coating type paint is 0.2%～5%;
D) organic titanic compound, consumption are 0.05%～3% of this coating type paint mass fraction;
E) organophosphorus compounds retardant synergist; The mass fraction of compd E in this coating type paint is 0.02%～0.2%;
F) organic hydrocarbon solvent or low-molecular-weight siloxane; One or more in organic hydrocarbon solvent such as toluene, xylenes, sherwood oil, hexanaphthene, the normal heptane wherein; The mixture of low-molecular-weight siloxane such as octamethyltrisiloxane, octamethylcyclotetrasiloxane or methyl cyclosiloxane, its consumption are 10%～58% of this coating type paint mass fraction.
2. according to the said coating of claim 1, it is characterized in that: said phenyl polysiloxane or methyl phenyl silicone resin are made by phenyl trialkoxy silane or phenyl trialkoxy silane and the polycondensation of aminomethyl phenyl dialkoxy silicane cohydrolysis.
3. according to the said coating of claim 1, it is characterized in that: described linear polysiloxane can be hydroxy-end capped polydimethylsiloxane or alkoxy end-capped polydimethylsiloxane, also can be the methyl phenyl silicone of above-mentioned two kinds of closed-end structures.
4. according to the said coating of claim 3, it is characterized in that: described linear polysiloxane viscosity is 50～5000mpa.s, and its structural formula can be A1
Also can be A2
Wherein preferred viscosities is 50～3000mpa.s, and structural formula is the linear polysiloxane of A1, and wherein n is the integer greater than zero, R
1, R
2Be methyl or phenyl, R
3Be methyl or ethyl.
5. according to the said coating of claim 1, it is characterized in that: the described silane coupling agent that contains amino or epoxy group(ing) is one or more in γ-An Bingjisanjiayangjiguiwan, γ-An Bingjisanyiyangjiguiwan, γ-aminopropyl methyl dimethoxysilane, γ-aminopropyl methyldiethoxysilane, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan, N-(β-aminoethyl)-γ-An Bingjisanyiyangjiguiwan, the γ-glycidyl ether oxygen propyl trimethoxy silicane.
6. according to the said coating of claim 5, it is characterized in that: the described preferred γ-An Bingjisanyiyangjiguiwan of silane coupling agent or the γ-glycidyl ether oxygen propyl trimethoxy silicane that contains amino or epoxy group(ing).
7. according to the said coating of claim 1; It is characterized in that: described organic titanic compound is isopropyl titanate, butyl (tetra) titanate, poly(tributoxy titanium), metatitanic acid four different monooctyl esters, purity titanium tetraethoxide, n-propyl titanate or organic titanium mixture, like in ethylacetoacetate titanium mixture, metatitanic acid four tert-butyl ester mixtures, the titanium acetylacetone mixture one or more.
8. according to the said coating of claim 7, it is characterized in that: preferred isopropyl titanate of described organic titanic compound or butyl (tetra) titanate.
9. according to the said coating of claim 1; It is characterized in that: described organophosphorus compounds retardant synergist is one or more in trichloroethyl phosphate, three (1,3-two chloropropyls) phosphoric acid ester, tributyl phosphate, trioctyl phosphate, Tritolyl Phosphate, the cumyl phenyl phosphate ester.
10. according to the said coating of claim 9, it is characterized in that: one or both the composite uses in described machine phosphoric acid ester retardant synergist preferably phosphoric acid front three phenyl ester, the cumyl phenyl phosphate ester.
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| CN 201110206283 CN102304323B (en) | 2011-07-22 | 2011-07-22 | Room-temperature cured phenyl silicon resin conformal coating |
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|---|---|---|---|
| CN 201110206283 CN102304323B (en) | 2011-07-22 | 2011-07-22 | Room-temperature cured phenyl silicon resin conformal coating |
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Cited By (16)
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|---|---|---|---|---|
| CN102898944A (en) * | 2012-10-12 | 2013-01-30 | 上海宜瓷龙新材料科技有限公司 | Anti-corrosion and high-gloss paint and preparation method and use thereof |
| WO2013154718A1 (en) * | 2012-03-21 | 2013-10-17 | Dow Corning Corporation | Compositions comprising resin- linear organosiloxane block copolymers and organopolysiloxanes |
| CN104927491A (en) * | 2015-07-02 | 2015-09-23 | 龚灿锋 | Antibacterial flame retardant coating and preparation method thereof |
| CN110452389A (en) * | 2019-08-23 | 2019-11-15 | 山东省科学院新材料研究所 | Low temperature resistant low ventilative silicone coatings composition of one kind and preparation method thereof |
| CN110591557A (en) * | 2019-09-26 | 2019-12-20 | 杭州之江新材料有限公司 | Organic silicon coating adhesive and preparation method thereof |
| CN110643281A (en) * | 2019-08-30 | 2020-01-03 | 宿迁市同创化工科技有限公司 | Preparation method of high-low temperature resistant elastic organic silicon three-proofing paint |
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| US11078112B2 (en) | 2017-05-25 | 2021-08-03 | Corning Incorporated | Silica-containing substrates with vias having an axially variable sidewall taper and methods for forming the same |
| US11114309B2 (en) * | 2016-06-01 | 2021-09-07 | Corning Incorporated | Articles and methods of forming vias in substrates |
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| CN113773505A (en) * | 2013-12-27 | 2021-12-10 | 陶氏东丽株式会社 | Room temperature curable silicone rubber composition, use thereof, and method for repairing electronic device |
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| WO2013154718A1 (en) * | 2012-03-21 | 2013-10-17 | Dow Corning Corporation | Compositions comprising resin- linear organosiloxane block copolymers and organopolysiloxanes |
| CN104245797A (en) * | 2012-03-21 | 2014-12-24 | 道康宁公司 | Compositions comprising resin- linear organosiloxane block copolymers and organopolysiloxanes |
| US9150727B2 (en) | 2012-03-21 | 2015-10-06 | Dow Corning Corporation | Compositions comprising resin-linear organosiloxane block copolymers and organopolysiloxanes |
| CN104245797B (en) * | 2012-03-21 | 2017-03-01 | 道康宁公司 | Comprise resin linear Organosiloxane block copolymer and the compositionss of organopolysiloxane |
| CN102898944A (en) * | 2012-10-12 | 2013-01-30 | 上海宜瓷龙新材料科技有限公司 | Anti-corrosion and high-gloss paint and preparation method and use thereof |
| CN113773505A (en) * | 2013-12-27 | 2021-12-10 | 陶氏东丽株式会社 | Room temperature curable silicone rubber composition, use thereof, and method for repairing electronic device |
| CN104927491A (en) * | 2015-07-02 | 2015-09-23 | 龚灿锋 | Antibacterial flame retardant coating and preparation method thereof |
| US11114309B2 (en) * | 2016-06-01 | 2021-09-07 | Corning Incorporated | Articles and methods of forming vias in substrates |
| US11774233B2 (en) | 2016-06-29 | 2023-10-03 | Corning Incorporated | Method and system for measuring geometric parameters of through holes |
| US11078112B2 (en) | 2017-05-25 | 2021-08-03 | Corning Incorporated | Silica-containing substrates with vias having an axially variable sidewall taper and methods for forming the same |
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| CN110591557A (en) * | 2019-09-26 | 2019-12-20 | 杭州之江新材料有限公司 | Organic silicon coating adhesive and preparation method thereof |
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| CN112480816B (en) * | 2020-11-30 | 2022-05-06 | 山东东岳有机硅材料股份有限公司 | Room-temperature-curing solvent-free conformal coating and preparation method thereof |
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