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Method for grafting modifying silicone resin

A technology of graft modification and silicone, which is applied in the field of polymer modification, and can solve the problems of high temperature resistance and wave transmission performance of materials.

Active Publication Date: 2007-06-06
WUXI HAITE NEW MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for grafting modified silicone resin to solve the problem that the existing technology cannot adapt to the development of rocket and aerospace technology and has high requirements for high temperature resistance and wave transmission performance of materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach 1

[0004] Specific embodiment 1: The steps of this embodiment are: 1. Drop the monomer mixture of alkyl chlorosilane, aryl chlorosilane and vinyl-containing silane coupling agent into the mixed solution of toluene and water through the dropping funnel , carry out hydrolysis and polycondensation reaction at 50-80°C; 2. Pour the reaction product into a separatory funnel, let it stand to separate the water layer, rinse the solvent layer repeatedly with distilled water, and then neutralize the solvent layer with NaOH until neutral to obtain Vinylmethylphenyl silicone resin prepolymer; 3. Distill the prepolymer of vinylmethylphenyl silicone resin under reduced pressure. Pressure distillation until no water is distilled out, add toluene to the obtained vinylmethylphenyl silicone resin prepolymer to make vinylmethylphenyl silicone resin with toluene as solvent; Add vinyl-containing cyclic nano-scale cage polyhedral silsesquioxane and peroxide initiator to the phenyl silicone resin to ma...

specific Embodiment approach 2

[0005] Specific embodiment two: the steps of this embodiment are: one, the 250ml four-necked flask that agitator, dropping funnel, reflux condenser and thermometer are housed is placed in water bath, adds 100g water, 65g in four-necked flask Toluene, stir evenly; Two, add 8g Ph in the dropping funnel 2 SiCl 2 , 18g PhSiCl 3 , 9g (CH 3 ) 2 SiCl 2 , 15g (CH 3 ) SiCl 3 , Mix these monomers evenly; 3. Raise the temperature of the four-necked flask to 50°C, start adding the monomer mixture dropwise, control the temperature between 50-70°C, and complete the dropwise addition in 1 hour; 4. Add dropwise Continue to stir for 30 minutes after completion; 5. Pour the reaction product into a separatory funnel, let it stand to separate the water layer, wash the solvent layer with 60°C distilled water for 4 times, and then neutralize it with 0.01-0.05ml of NaOH with a concentration of 20-40wt%. Solvent layer to neutral to obtain the prepolymer of silicone resin; 6. Distill the silico...

specific Embodiment approach 3

[0006] Specific embodiment three: the difference between this embodiment and specific embodiment two is that the added monomer is 8g Ph 2 SiCl 2 , 18g PhSiCl 3 , 9g (CH 3 ) 2 SiCl 2 , 15g (CH 3 ) SiCl 3 , 4gKH-570, other steps are the same as in the second embodiment. The synthesized in this embodiment is a vinyl-containing methylphenyl silicone resin, which has an initial thermal decomposition temperature of 400°C in an air atmosphere, a weight loss rate of 15% at 500°C, and a weight loss rate of 19.5% at 600°C. The weight loss rate is 23.5% at 700°C.

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Abstract

A process for modifying organic silica resin by graft in order to improve its high temp resistance and electromagnetic wave penetrability includes dripping the mixture of alkyl chlorosilane, aryl chlorosilane and vinyl silane coupling agent into the mixture of tulene solution and water, hydrolyzing, polycondensating, vacuum distilling to obtain vinylmethylphenyl silicon resin, adding nano-class cyclic cage-shaped polygonal sesquisiloxane and peroxide as trigger, and graft reaction.

Description

Technical field: [0001] The invention relates to a modification technology of high molecular polymer. Background technique: [0002] With the development and progress of rocket and aerospace technology, the flight Mach number of aerospace vehicles continues to increase, and the radome at the maximum aerodynamic heating position of the aircraft needs to withstand higher and higher temperatures and thermal shocks. The high temperature resistance of aerospace wave-transparent materials The requirements are getting higher and higher, which is more closely dependent on the research and development of high temperature resistant wave transparent resin matrix. Therefore, improving the heat resistance of the resin matrix has become a priority development direction of aerospace wave-transparent materials. The resin matrix of early aerospace wave-transparent composite materials mainly includes phenolic resin, epoxy resin, unsaturated resin, vinyl resin, polybutadiene resin, styrene-bu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/42
Inventor 黄玉东刘玉荣刘丽胡立江刘立询
Owner WUXI HAITE NEW MATERIAL RES INST
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