Mercaptopropyl polysiloxane with photoreaction activity and preparation method thereof

A technology of mercaptopropylene polysiloxane and photoreactivity, which is applied in the field of mercaptopropylene polysiloxane and its preparation, can solve the problems of poor compatibility of acrylates, achieve fast reaction speed and improve mechanical properties

Inactive Publication Date: 2017-01-11
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome defects and deficiencies such as photocuring of polysiloxane and poor compatibility between photocuring polysiloxane and epoxy resin and acrylate in the prior art, and provide a photoreactive polysiloxane Mercaptopropylene polysiloxane

Method used

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  • Mercaptopropyl polysiloxane with photoreaction activity and preparation method thereof
  • Mercaptopropyl polysiloxane with photoreaction activity and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] First add 70g of water, 35g of ethanol, and 4g of concentrated brine into the flask, then add 30g of hexamethyldisiloxane into the above solution, then add 150g of mercaptopropyltriethoxysilane, 100g of phenylmethyldimethoxy Diethyldiethoxysilane and 75g of diethyldiethoxysilane were added dropwise to the above-mentioned prehydrolysis solution, and then co-hydrolysis-polycondensation reaction was carried out at 60°C for 4.5h, and the reaction system was separated to obtain mercaptopropylene polysiloxane, which was used Wash with 70% ethanol aqueous solution for 3 times, and finally vacuumize at 120° C. to remove residual solvent and low boilers to obtain mercaptopropylene polysiloxane with a yield of 85.35%.

[0032] After testing, the molar ratio of the mercaptopropyl segment, the phenyl segment and the dialkyl segment in the obtained mercaptopropyl polysiloxane molecule is 0.63:0.55:0.43.

Embodiment 2

[0034] First add 90g of water, 50g of ethanol, and 5.5g of concentrated brine into the flask, then add 50g of hexamethyldisiloxane into the above solution, then add 100g of mercaptopropylmethyldimethoxysilane, 100g of diphenyldimethoxysilane Add methoxysilane and 50g dimethyldiethoxysilane dropwise to the above pre-hydrolysis solution, then co-hydrolyze-polycondense at 65°C for 4 hours, separate the reaction system to obtain mercaptopropylene polysiloxane, Wash with 70% ethanol aqueous solution for 3 times, and finally vacuumize at 110° C. to remove residual solvent and low boilers to obtain mercaptopropylene polysiloxane with a yield of 82.46%.

[0035] After testing, the molar ratio of the mercaptopropyl segment, the phenyl segment and the dialkyl segment in the obtained mercaptopropyl polysiloxane molecule is 0.55:0.41:0.34.

Embodiment 3

[0037] First add 45g of water, 20g of ethanol, and 2.5g of concentrated brine into the flask, then add 25g of hexamethyldisiloxane into the above solution, then add 94g of mercaptopropyltrimethoxysilane, 50g of tetramethyltetraphenylcyclo Tetrasiloxane and 60g of diisopropyldimethoxysilane are added dropwise to the above-mentioned pre-hydrolysis solution, and then co-hydrolysis-polycondensation reaction is carried out at 70°C for 3 hours, and the reaction system is separated to obtain mercaptopropylenepolysiloxane , washed 3 times with 70% ethanol aqueous solution, and finally vacuumed at 130° C. to remove residual solvent and low boilers to obtain mercaptopropylene polysiloxane with a yield of 83.64%.

[0038] After testing, the molar ratio of the mercaptopropyl segment, the phenyl segment and the dialkyl segment in the obtained mercaptopropyl polysiloxane molecule is 0.48:0.37:0.34.

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Abstract

The invention discloses mercaptopropyl polysiloxane with photoreaction activity and a preparation method thereof. Mercaptopropyl polysiloxane is polysiloxane molecules containing mercaptopropyl chain segments, phenyl chain segments and dialkyl chain segments. The preparation method of mercaptopropyl polysiloxane comprises the steps that hexamethyldisiloxane and silane with different substituent groups are subjected to a cohydrolysis-polycondensation reaction under the acidic condition to generate mercaptopropyl polysiloxane. Silane with different substituent groups is a mixture of mercaptopropyl silane, phenyl silane and dialkyl silane or tetramethoxysilane, prepared mercaptopropyl polysiloxane, silicone rubber, epoxy resin, acrylate resin and other materials can have good compatibility by controlling and adjusting the relative content of the mercaptopropyl chain segments, the phenyl chain segments and the dialkyl chain segments, mercaptopropyl polysiloxane can be used for cross-linking and curing of the materials, an optically transparent composite is prepared, the mechanical performance of the material can be improved, the photocuring reaction speed is high, and mercaptopropyl polysiloxane can be used for the fields of electronic packaging materials, optical materials, 3D printing consumables and the like.

Description

technical field [0001] The invention belongs to the technical field of functional polymer materials, and more specifically relates to a photoreactive mercaptopropylene polysiloxane and a preparation method thereof. Background technique [0002] Organopolysiloxane is a typical semi-inorganic and semi-organic polymer material. Its special valence bond structure makes it have many excellent physical and chemical properties different from carbon-based polymers, such as temperature resistance, weather resistance, insulation Properties, low surface energy, and chemical stability make it widely used in the fields of electronics, energy, chemical industry, national defense, and aerospace. However, traditional organopolysiloxanes, such as hydroxyl-terminated polysiloxanes and vinyl polysiloxanes, have the disadvantages of slow curing speed and high temperature curing during the curing and crosslinking process, which not only consumes time and energy , which also limits its wide rang...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/28C08G77/06C08L63/00C08L63/10C08L83/04C08L83/08
CPCC08G77/28C08G77/06C08L63/00C08L63/10C08L83/04C08L83/08C08L2201/10C08L2203/206C08L2205/02C08L2205/035
Inventor 向洪平刘晓暄董海辉尹敬锋谭启聪何佳泽
Owner GUANGDONG UNIV OF TECH
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