Phenyl-containing MT type resin and preparation method thereof

A resin and phenyl technology, applied in the field of phenyl-containing MT-type resin and its preparation, can solve the problems of different refractive index, white turbidity of compound liquid silicone rubber, etc. Effect

Active Publication Date: 2013-01-16
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the control of the molecular weight of synthetic MT-type resins is mainly controlled by different M / T ratios. Because MT resins with different M / T ratios have different phenyl content, there are differences in refractive index when compounding with different molecular weights. , and the difference in refractive index will cause white turbidity in the compound liquid silicone rubber

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 72g of deionized water, 250ml of toluene, 0.01g of concentrated sulfuric acid (concentration 98%) into a four-neck flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, raise the temperature to 60°C and add 42.3g of 1,3 - divinyl 1,1,3,3-tetramethyldisiloxane with 524.7 g of phenyltrimethoxysilane. After the dropwise addition, react at reflux temperature for 5 hours, cool, add 400 ml of toluene, neutralize to neutral with sodium bicarbonate, then add 1 ml of 30% acetic acid aqueous solution to acid, wash with water until neutral, and remove the solvent in vacuo , maintain a low boiling point at 190°C for 2 hours to remove small molecular impurities, and obtain a colorless and transparent vinyl phenyl MT resin with a weight-average molecular weight of 823 and a refractive index of 1.536 as measured by GPC.

Embodiment 2

[0025] Add 72g of deionized water, 250ml of toluene, 0.01g of concentrated sulfuric acid (concentration 98%) into a four-neck flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, raise the temperature to 80°C and add 37.4g of Hexamethasone dropwise phenyl disiloxane and 524.7g phenyltrimethoxysilane. After the dropwise addition, react at reflux temperature for 5 hours, cool, add 400 milliliters of toluene, neutralize to neutrality with sodium bicarbonate, then add 1 milliliter of 30% acetic acid aqueous solution to acidity, wash with water to neutrality, and remove the solvent in vacuo. Maintain low boiling at 190°C for 2 hours to remove small molecule impurities to obtain a colorless and transparent trimethylphenyl MT resin with a weight average molecular weight of 785 and a refractive index of 1.534 as measured by GPC.

Embodiment 3

[0027] Add 72g of deionized water, 250ml of toluene, and 0.13g of trifluoromethanesulfonic acid into a four-necked flask with mechanical stirring, reflux condenser, thermometer and dropping funnel, and add 22.9g of trimethylmethane dropwise at 90°C. Oxysilane and 52.88 g of phenyltriethoxysilane. After the dropwise addition, react at reflux temperature for 3 hours, cool, add 400 milliliters of toluene, neutralize to neutral with sodium bicarbonate, then add 1 milliliter of 30% acetic acid aqueous solution to acid, wash with water until neutral, vacuum desolventization, Maintain low boiling at 190°C for 2 hours to remove small molecule impurities to obtain a colorless and transparent vinyl phenyl MT resin with a weight-average molecular weight of 1300 and a refractive index of 1.536 as measured by GPC.

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Abstract

The invention relates to phenyl-containing MT type resin and a preparation method thereof. The weight-average molecular weight of the phenyl-containing MT type resin is 800-8000. The preparation method of the phenyl-containing MT type resin includes the steps: (1) dissolving acid catalysts into solvent, increasing the temperature to 50-90 DEG C, dropwise adding a mixture of phenyl tri-alkoxy silane and monofunctional alkoxy silane and reacting for 3-8 hours; (2) decreasing the temperature of a reaction mixture to the room temperature, neutralizing the reaction mixture to neutrality, filtering and washing; and (3) removing the solvent so that the phenyl-containing MT type resin is obtained. The phenyl-containing MT type resin prepared by the method has the weight-average molecular weight of 800-8000 and can be applied to high-refraction liquid silicone rubber.

Description

technical field [0001] The invention relates to the field of silicone resins, in particular to a phenyl-containing MT-type resin and a preparation method thereof. Background technique [0002] MT-type resins refer to resins including trifunctional monomers (T units) and monofunctional monomers (M units). Phenyl-containing silicone liquid silica gel has excellent high and low temperature resistance, radiation resistance, wide operating temperature range, and high refractive index performance. It has a wide range of applications in various industries, especially aerospace, national defense, electronic and optical device packaging application. The phenyl-containing MT resin has an irreplaceable role as a reinforcing agent in transparent high-refractive liquid silicone rubber, and the combination of MT resins with different molecular weights has a better reinforcing effect on the mechanical properties of liquid silicone rubber. [0003] At present, the synthesis method of phen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/20C08G77/06
Inventor 涂世俭宋振虎李新莹张建新屈均
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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