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Low-temperature-resistant low-air-permeability silicon resin coating composition and preparation method thereof

A technology of silicone resin and hydroxy silicone oil, which is applied in the direction of coating, etc., can solve the problems of circuit boards, photoelectric devices, vulcanization failure, inability to prevent sulfur vapor penetration, inspection of use requirements, etc., to solve the problem of device failure, improve toughness, and improve The effect of air tightness

Active Publication Date: 2019-11-15
山东山科瑞森新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN103992738A reports a -40°C resistant coating prepared by grafted silicone resin, aluminum powder, solvent, additives, etc., but does not investigate the use requirements for lower temperatures
[0005] Silicone resin coating is a kind of material with high air permeability. When it is used as a protective coating for electronic equipment, it often cannot block the penetration of sulfur vapor, which will cause vulcanization failure of circuit boards and optoelectronic devices.
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Method used

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  • Low-temperature-resistant low-air-permeability silicon resin coating composition and preparation method thereof
  • Low-temperature-resistant low-air-permeability silicon resin coating composition and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Add 118 g of deionized water, 500 g of toluene, and 6 g of hydrochloric acid (concentration: 37%) into the reaction flask, stir evenly, and add 500 g of phenyltrimethoxysilane dropwise. After the addition, the temperature was raised to reflux, reacted for 2h, and then cooled to room temperature. The reaction solution was washed with deionized water until neutral. The organic phase was collected and dried overnight with anhydrous calcium chloride. Calcium chloride was filtered, and the filtrate was concentrated to remove toluene to obtain 310 g of trifunctional silicone resin prepolymer.

Embodiment 2

[0037] Get the prepolymer 80g prepared in Example 1, dimethyl hydroxy silicone oil (100mPa s) 15.3g, trifluoropropyl methyl hydroxy silicone oil (100mPa s) 32.24g, dissolve with 800g toluene, add reaction bottle, Furthermore, 0.3 g of trifluoromethanesulfonic acid was added. Heat to reflux for 1h, remove the generated water with a water separator; then add 15.3g of dimethyl hydroxy silicone oil (100mPa s), 32.24g of trifluoropropyl methyl hydroxy silicone oil (100mPa s), and continue to reflux to remove water; 2h Then add 15.3g of dimethyl hydroxy silicone oil (100mPa·s) and 32.24g of trifluoropropyl methyl hydroxy silicone oil (100mPa·s), remove the generated water and continue reflux aging for 6h. Cool down after the reaction, add 1.5g of calcium carbonate to neutralize, and filter. Filtrate decompression distillation removes solvent, obtains average unit formula as (PhSiO 1.5 ) 0.32 (Me 2 SiO) 0.32 (CF 3 CH 2 CH 2 MeSiO) 0.32 (OH) 0.04 of solid silicone.

Embodiment 3

[0039] Get the prepolymer 80g prepared in Example 1, dimethyl hydroxy silicone oil (100mPa s) 7.6g, trifluoropropyl methyl hydroxy silicone oil (100mPa s) 48.3g, dissolve with 800g toluene, add reaction flask, Furthermore, 0.5 g of trifluoromethanesulfonic acid was added. Heat to reflux for 1h, remove the generated water with a water separator; then add 7.6g of dimethyl hydroxy silicone oil (100mPa s), 48.3g of trifluoropropyl methyl hydroxy silicone oil (100mPa s), and continue to reflux to remove water; 2h Then add 7.6g of dimethyl hydroxy silicone oil (100mPa·s) and 48.3g of trifluoropropyl methyl hydroxy silicone oil (100mPa·s), remove the generated water and continue to reflux for 6.5h of aging. Cool down after the reaction, add 2.5g of calcium carbonate for neutralization, and filter. Filtrate decompression distillation removes solvent, obtains average unit formula as (PhSiO 1.5 ) 0.32 (Me 2 SiO) 0.16 (CF 3 CH 2 CH 2 MeSiO) 0.49 (OH) 0.03 of solid silicone.

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Abstract

The invention discloses a low-temperature-resistant low-air-permeability silicon resin coating composition and a preparation method thereof. The preparation method comprises the following steps: firstly, preparing a trifunctional aryl silicon resin prepolymer, and carrying out copolymerization on the trifunctional aryl silicon resin prepolymer, hydroxyl silicone oil and fluorine-containing hydroxyl silicone oil to prepare hydroxyl-terminated fluorine-containing aryl silicon resin (R1SiO1.5)a(R22SiO)b(R2R3SiO)c(OH)d, wherein the (R1SiO1.5)a(R22SiO)b(R2R3SiO)c(OH)d has a T-shaped aggregate polysiloxane-D type linear polysiloxane block structure; and after the silicon resin is diluted by using a diluent, adding trialkoxysilane as a cross-linking agent and a titanium-containing or tin-containing compound as a catalyst, and performing uniform mixing to obtain the low-temperature-resistant low-air-permeability silicon resin coating composition. The composition coats the surface of a base material in a spraying, brush coating or dip-coating manner, and a low-temperature-resistant low-air-permeability silicon resin coating is obtained after room-temperature curing. The coating provided bythe invention can resist the low temperature of -70 DEG C for a long time and can be subjected to hot and cold circulation for 300 times at the temperature of -70 DEG C to 140 DEG C, and the oxygen permeation amount is smaller than 100 cm<3> / (m<2>*24 h*0.1 MPa).

Description

technical field [0001] The invention relates to a low-temperature-resistant and low-breathability silicone resin coating composition and a preparation method thereof, belonging to the technical field of silicone polymers. Background technique [0002] There is a relatively stable molecular structure Si-O-Si similar to inorganic acid salts in the silicone resin molecule, and the outer layer has a layer of non-polar organic groups, so it has high heat resistance, chemical stability, and electrical insulation and hydrophobicity. Due to the above-mentioned good properties, the high-performance coating prepared with silicone resin as the matrix has become an indispensable protective material in the electronics, aerospace and defense industries. [0003] With the rapid development of applications in the field of polymer technology, coatings are inevitably exposed to low temperature conditions, and many destructive results in applications occur under low temperature conditions. S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/44C09D183/10
CPCC08G77/44C09D183/10
Inventor 彭丹牟秋红李金辉王峰张硕
Owner 山东山科瑞森新材料科技有限公司
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