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A kind of preparation method of mtq type phenyl hydrogen-containing silicone resin reinforced with mq silicone resin

A technology of phenyl hydrogen-containing silicone and MQ silicone resin, which is applied in the field of preparation of phenyl hydrogen-containing silicone resin, can solve the problems of reducing the content of T chain segments, no reinforcing effect, and reduced reinforcing effect, and achieves good compatibility , Solve the problem of compatibility and good resilience

Active Publication Date: 2016-09-14
INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] If you want to obtain polysiloxane with medium and low phenyl content, that is, phenylpolysiloxane with low refractive index in the range of 1.43~1.48, you must reduce the content of T chain segments, which results in a decrease in the reinforcing effect or even no reinforcement. strong effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 33.5g of tetramethyldihydrodisiloxane, 99g of phenyltrimethoxysilane and 100g of methylcyclohexane into the flask, and stir evenly. 5g of p-toluenesulfonic acid was added as a catalyst, and then 100g of deionized water was added dropwise for hydrolysis. After the dropwise addition was completed, the temperature was raised to 70° C. for constant temperature aging for 3 hours, then cooled to room temperature, liquid separation was carried out, and 197 g of the organic layer was taken and weighed. Transfer to a clean beaker, which is the hydroxyl-containing MT-type phenyl hydrogen-containing silicone resin prepolymer solution (component A).

[0025] Add 100 g of deionized water and 5 g of p-toluenesulfonic acid to another flask, stir evenly, and then slowly add 88.6 g of ethyl orthosilicate dropwise for hydrolysis. After the dropwise addition, 100 g of methylcyclohexane and 34.5 g of hexamethyldisiloxane were added, and the temperature was raised to 70°C for constant ...

Embodiment 2

[0028] The preparation method of the hydroxyl-containing MT type phenyl hydrogen-containing silicone resin prepolymer solution (component A) is the same as in Example 1.

[0029] Add 100 g of deionized water and 5 g of p-toluenesulfonic acid to another flask, stir evenly, and then slowly add 98.4 g of ethyl orthosilicate dropwise for hydrolysis. After the dropwise addition, 100 g of methylcyclohexane and 34.5 g of hexamethyldisiloxane were added, and the temperature was raised to 70°C for constant temperature aging for 3 hours, then cooled to room temperature, separated, and the organic layer was taken to weigh 162 g. Transfer to a clean beaker, which is the hydroxyl-containing MQ silicone resin prepolymer solution (component B).

[0030] Mix the above component A and component B according to the mass ratio of 1.216:1, stir evenly, then add 10g of p-toluenesulfonic acid, heat up to reflux, and distill the water produced by the condensation with a water separator at the same ti...

Embodiment 3

[0032] The preparation method of the hydroxyl-containing MT type phenyl hydrogen-containing silicone resin prepolymer solution (component A) is the same as in Example 1.

[0033] Add 100 g of deionized water and 5 g of p-toluenesulfonic acid to another flask, stir evenly, and then slowly add 110 g of ethyl orthosilicate dropwise for hydrolysis. After the dropwise addition, 100 g of methylcyclohexane and 27.9 g of hexamethyldisiloxane were added, and the temperature was raised to 70° C. for constant temperature aging for 3 hours, then cooled to room temperature, separated, and the organic layer was taken to weigh 158 g. Transfer to a clean beaker, which is the hydroxyl-containing MQ silicone resin prepolymer solution (component B).

[0034]Mix the above-mentioned component A and component B according to the mass ratio of 1.247:1, stir evenly, then add 10g of p-toluenesulfonic acid, heat up to reflux, and distill the water produced by the condensation with a water separator at t...

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Abstract

A preparation method of MTQ type phenyl hydrogen-containing silicone resin reinforced with MQ silicone resin, which is characterized in that the hydroxyl-containing MT type phenyl hydrogen-containing silicone resin prepolymer solution and the hydroxyl-containing MQ silicone resin prepolymer solution Mix, heat to reflux, distill the water produced by condensation; stir the reaction, stop heating, cool to room temperature; then wash with water until neutral, dry, decolorize, remove the solvent and low-molecular compounds in vacuum, and obtain a colorless and transparent MQ silicone resin reinforcement MTQ type phenyl hydrogen silicone resin. The MTQ type phenyl hydrogen-containing silicone resin prepared by the present invention has high light transmittance, clarity and transparency, and good compatibility with phenyl vinyl silicone resin, and can be used as a crosslinking agent for phenyl silicone rubber, which can make the silicone rubber have good resilience, Tear resistance, thermal shock resistance, heat resistance, radiation resistance, aging resistance.

Description

technical field [0001] The invention relates to a preparation method of phenyl hydrogen-containing silicone resin, in particular to a preparation method of MTQ type phenyl hydrogen-containing silicone resin reinforced with MQ silicone resin. Background technique [0002] The phenyl hydrogen-containing silicone resin of the present invention is an important raw material for the preparation of addition-type phenyl silicone rubber. Silica, carbon black, calcium carbonate, etc. must be added to the formula of silicone rubber as reinforcing fillers, or MQ silicone resin must be added Reinforcement, otherwise it will not have mechanical properties and strength after vulcanization and cannot be used. [0003] Due to the addition of white carbon black with a refractive index of 1.46 as reinforcement, the traditional methyl silicone rubber with a refractive index of 1.41 and the high phenyl silicone rubber with a refractive index of 1.50 have too much refractive index deviation and b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/44
Inventor 朱淮军戴子林涂伟萍
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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