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A kind of synthetic method of phenyl block silicone resin

A synthesis method and technology of silicone resin, applied in the field of chemical production, can solve the problems of low crosslinking degree, low hardness, easy to scratch, etc., and achieve the effect of excellent anti-adhesive performance, low surface energy, and good flexibility

Active Publication Date: 2021-07-13
HUBEI XINGRUI SILICON MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Ordinary silicone resin has a highly cross-linked network structure, high hardness and strength, but poor toughness; while silicone rubber has a helical long-chain structure, good elasticity, but low cross-linking degree, low hardness, and easy to scratch hurt

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add 54.2g of phenyltrichlorosilane, 28g of dimethyldichlorosilane, 23.4g of diphenyldichlorosilane, 24.8g of methylphenyldichlorosilane, 100g of toluene, 15g of 1500mPa.s into a 500ml three-necked flask Stir and mix the hydroxypolytrifluoropropylmethylsiloxane evenly, add the above mixed solution into the water with a constant pressure dropping funnel, and the titration time is about 30 minutes. Poly 3h.

[0025] (2) Stand for stratification, separate the lower layer of acid water, and wash the upper layer of hydrolyzate with hot distilled water until neutral to obtain a silicone resin prepolymer, then dewater the silicone resin prepolymer at 110°C for 1 hour After the end, add 2g of tetramethylammonium hydroxide to carry out the condensation reaction for 4 hours. After the reaction, wash with hot distilled water to neutrality, and then remove the water to obtain a phenyl silicone resin product. The resin can be cured to form a film, and it is transparent after curi...

Embodiment 2

[0028] (1) Add 74.5 phenyltrichlorosilane, 21.02 dimethyldichlorosilane, 17.5 diphenyldichlorosilane, 18.5 methylphenyldichlorosilane, 100g toluene, 15g700gmPa.s dihydroxy poly Stir trifluoropropylmethylsiloxane for 10 minutes, add the above mixed solution to the water with a constant pressure dropping funnel, and the titration time is about 30 minutes. After the drop is completed, react at room temperature for 1 hour, the hydrolysis is completed, and then pre-polymerize at 80°C 3h.

[0029] (2) Wash with water until neutral to obtain a silicone resin prepolymer, add sodium sulfate to remove water, add 3g of sodium hydroxide for dehydration condensation reaction for 3 hours, wash with water until neutral, then remove water at high temperature, and desolventize to obtain phenyl intercalated section of silicone. The resin can be cured to form a film, which is transparent and elastic after curing

[0030] (3) The elongation at break of the coating glue prepared by using this si...

Embodiment 3

[0033] (1) Add 54.2g of phenyltrichlorosilane, 28g of dimethyldichlorosilane, 23.4g of diphenyldichlorosilane, 24.8g of methylphenyldichlorosilane, and 100g of toluene into a 500ml three-necked flask with constant pressure drops Add the above mixed solution into the water through the funnel, and the titration time is about 30 minutes. After the dropping, react at room temperature for 1 hour, the hydrolysis is completed, and then pre-polymerize at 80°C for 3 hours.

[0034] (2) Stand for stratification, separate the lower layer of acid water, and wash the upper layer of hydrolyzate with hot distilled water until neutral to obtain a silicone resin prepolymer, then dewater the silicone resin prepolymer at 110°C for 1 hour After the end, add 2g of tetramethylammonium hydroxide to carry out the condensation reaction for 4 hours. After the reaction, wash with hot distilled water until neutral, and then remove the water to obtain the phenyl silicone resin product. The resin is brittl...

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Abstract

The invention provides a phenyl block silicone resin, which is composed of phenyltrichlorosilane, dimethyldichlorosilane, diphenyldichlorosilane, methylphenyldichlorosilane, solvent, dihydroxypolytrifluoropropylene phenyl methyl siloxane as raw material, after hydrolysis, prepolymerization, water washing, water removal, condensation, precipitation to obtain phenyl block silicone resin. The fluorine group is introduced, so that the phenyl silicone resin has lower surface energy, oil resistance, anti-fouling, and excellent anti-sticking properties. The synthetic silicone resin of the present invention can be cured into a transparent film at room temperature, and the prepared coating glue has a tensile strength of more than 2.5Mpa and a Shore hardness of 75Å. The combination of branched silicone resin and linear siloxane makes the silicone resin have better flexibility and flexibility, and provides the possibility of application materials that require a certain degree of toughness in some high-temperature applications.

Description

technical field [0001] The invention relates to a method for synthesizing phenyl block silicone resin, which belongs to the technical field of chemical production. Background technique [0002] Silicone resin has many excellent physical and chemical properties, such as high and low temperature resistance, radiation resistance, oxidation resistance, high air permeability, weather resistance, mold release, water resistance and physiological inertia. Now it has been widely used in many fields such as electronic and electrical chemical industry, metallurgy, construction, aerospace, aviation, medical materials and so on. Silicone resin is a necessary raw material for some high-end silicone products. Although the amount of silicone resin used is not large, it is indispensable. At present, the domestic production of silicone resin is relatively small, and foreign products block our technology. In this international environment, it is necessary to develop silicone resin independentl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/44C08G77/06
CPCC08G77/06C08G77/44C08G77/80
Inventor 李海娟李书兵陈海平
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD