Modified silicone resin and preparation method thereof

A technology for modifying silicon and resin, which is applied in the field of modified silicone resin and its preparation, which can solve the problems of reduced electrical insulation, influence on dielectric properties, and decreased transparency of silicone resin, and achieve improved toughness and strength, and excellent insulation performance effect

Inactive Publication Date: 2009-09-30
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the modification reaction of hydroxy silicone oil and the reaction with silicone resin need to add catalysts containing metal ions. The metal ions remaining in the system after curing will affect its dielectric properties and reduce electrical insulation.
Moreover, the commonly used method of adding rubber particles to improve toughness often reduces the transparency of silicone resins.

Method used

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  • Modified silicone resin and preparation method thereof
  • Modified silicone resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 20g of methyltriethoxysilane into a reaction bottle with a stirrer, add 6g of dilute hydrochloric acid containing 153uL / L of HCl, reflux at 80°C for 12h, and age at room temperature for 12h to settle the resin at the bottom of the bottle. Wash off the HCl with distilled water until pH=7 is neutral, pour off the upper layer of water, add 12g of ethanol after drying, and prepare a 20g concentration of 30% (mass fraction) polymethylorganosilsesquioxane solution, and analyze it by mass spectrometry The number average molecular weight was measured to be 900.

[0027] Hydroxymethyl silicone oil (viscosity at 20°C is 15-50mm 2 the s -1 ) is a product of Beijing Dingye Industry and Trade Co., Ltd., and the brand number is 203. Add 4 g of hydroxymethyl silicone oil into the 20 g of polymethylorganosilsesquioxane solution prepared above, and mix evenly to obtain a clear and uniform mixed solution. Among them, the weight ratio of hydroxymethyl silicone oil to polymethylorga...

Embodiment 2

[0033] Add 24g of phenyltrimethoxysilane into a reaction bottle with a stirrer, add 10g of dilute hydrochloric acid containing 153uL / L of HCl, reflux at 80°C for 24h, and age at room temperature for 48h to settle the resin at the bottom of the bottle. Wash off HCl with distilled water until the pH=7 is neutral, pour off the upper layer of water, add 12g of acetone after drying, and prepare a 20g concentration of 30% (mass fraction) polyphenylorganosilsesquioxane solution, and use mass spectrometry Its number average molecular weight was measured to be 1500. Hydroxymethyl silicone oil (viscosity at 20°C is 15-50mm 2 the s -1) is a product of Beijing Dingye Industry and Trade Co., Ltd., the brand name is 203, 2g of hydroxymethyl silicone oil is added to the 20g of polyphenylorganosilsesquioxane solution prepared above, and mixed evenly to obtain a clear and uniform mixed solution. Among them, the weight ratio of hydroxymethyl silicone oil to polyphenylorganosilsesquioxane is 0...

Embodiment 3

[0039] Add 26g of vinyltriethoxysilane into a reaction bottle with a stirrer, add 12g of dilute hydrochloric acid containing 153uL / L of HCl, reflux at 80°C for 24h, and age at room temperature for 48h to settle the resin at the bottom of the bottle. Wash off the HCl with distilled water until the pH=7 is neutral, pour off the upper layer of water, add 12g of tetrahydrofuran after drying, and prepare a 20g concentration of 30% (mass fraction) polyvinylorganosilsesquioxane solution, and analyze it by mass spectrometry The number average molecular weight was measured to be 2000. Hydroxymethyl silicone oil (viscosity at 20°C is 15-50mm 2 the s -1 ) is a product of Beijing Dingye Industry and Trade Co., Ltd., and the brand name is 203. Add 5 g of hydroxymethyl silicone oil to the 20 g of polyvinylorganosilsesquioxane solution prepared above, and mix well to obtain a clear and uniform mixed solution. Among them, the weight ratio of hydroxymethyl silicone oil to polyvinylorganosils...

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Abstract

The invention discloses a modified silicone resin and a preparation method thereof. The modified silicone resin provided by the invention is a compound consisting of silicon oil and polysilsesquioxane, the flexural modulus of the modified silicon resin is 160 to 280 MPa, the transmittance in visible light (400 to 800 nm) range is 88 to 93 percent, and the insulativity of the modified silicon resin is the same as that of air. The preparation method for the modified silicone resin comprises the following steps: 1) dissolving the silicon oil and the polysilsesquioxane into a solvent to obtain a mixed solution; 2) placing the mixed solution in the environment of the temperature of between 0 and 40 DEG C and the relative humidity of 10 to 40 percent, and volatilizing the solvent to make that the percentage composition of gross mass of the polysilsesquioxane and the silicon oil in the mixed solution is 50 to 80 percent; and 3) placing the solution obtained in the step 2) in the acid environment with the relative humidity of more than 80 percent and pH of 0 to 3 to obtain the modified silicone resin.

Description

technical field [0001] The invention relates to a modified silicone resin and a preparation method thereof. Background technique [0002] Polyorganosilsesquioxane (PSQ) is a class of empirical formula (RSiO 3 / 2 ) n The organosilicon polymer, the ratio of oxygen atoms to silicon atoms is 1.5, where R can be hydrogen, alkyl, alkylene, aryl, arylene and their organic functional group derivatives. Under normal hydrolysis and condensation conditions, the trifunctional monomer RSiX 3 (X=Cl, OR) reaction often gives the hydrolysis product PSQ with non-specific regular structure. Due to the special structure of polyorganosilsesquioxane, its unique properties and uses are determined. [0003] Polyorganosilsesquioxane contains Si-O-Si chemical bonds with high bond energy in the molecular structure, while the configuration is a ladder or cage structure, and the cured resin forms a cross-linked network structure, so The material has excellent heat resistance. Polyorganosilsesquiox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08L83/04
Inventor 李燕芳刘海云杨曙光李晓峰戴珍张小莉徐坚
Owner INST OF CHEM CHINESE ACAD OF SCI
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