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A kind of dual-curable polysiloxane and its preparation method and use

A technology of polysiloxane and hydroxyl-terminated polysiloxane, which is applied in the field of silicon materials, can solve the problems of high photocuring energy requirements, high photocuring energy of products, human body and environmental damage, etc., and achieves excellent moisture and heat aging resistance. , the effect of reducing energy and improving end capping efficiency

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The disclosed technology for preparing dual-curing silicone materials mostly uses an end-capping agent containing an acrylate group to carry out a capping reaction on hydroxyl silicone oil. The ester decomposition reaction under catalysis leads to the production of acrylate, and acrylate has a strong pungent smell, which will cause great harm to human body and environment
The photocuring energy requirements of the resulting product are relatively high, which limits its application in LED-based light sources
[0005] CN102408569A discloses a dual-curable polysiloxane acrylate resin and a preparation method thereof. The method uses dibutyltin dilaurate as a catalyst and uses toluene or n-hexane as a solvent to prepare a silicone polymer with dual-curability , but the photocuring energy of the obtained product is higher

Method used

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  • A kind of dual-curable polysiloxane and its preparation method and use
  • A kind of dual-curable polysiloxane and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Take a 1000ml four-necked flask and fully dry it, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 70cP, start stirring for 300r / min, vacuumize and remove water at 80°C for 60min, cool down to 50°C, add 23g of dimethoxydicarbonate Chloropropylsilane, stir for 15min, add 0.7g acetic acid, react for 3h, add 46g chloropropyltrimethoxysilane, react for 2h, remove low boiling under the condition of 100℃, 5mbar, and add 0.015 p-hydroxyanisole to the obtained product g, 20 g of sodium acrylate, stir evenly, add 2.5 g of tetramethylammonium hydroxide and heat up to 80 °C for 3 hours, then heat up to 150 °C, extract low boiling under the condition of 5mbar, filter under positive pressure to obtain product I, and its silyl hydroxyl group is tested. The residue was 0.7% and methyl acrylate was not detected.

Embodiment 2

[0048]Take a 1000ml four-necked flask and fully dry it, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 200cP, turn on and stir for 300r / min, vacuumize and remove water at 100°C for 60min, cool down to 60°C, add 18g of dimethoxydicarbonate Chloropropylsilane, stir for 15min, add 0.5g phosphoric acid, react for 3h, add 38g chloropropyltrimethoxysilane, react for 2h, remove low boiling under the condition of 100℃, 5mbar, add N,N-diethyl ether to the obtained product Hydroxylamine 0.01g, sodium acrylate 16g, stir evenly, add 2.5g of tetramethylammonium hydroxide, heat up to 80 °C for 3 hours, then heat up to 145 °C, extract low boiling under 5mbar, filter under positive pressure to obtain product II, which has been tested Its silanol residue was 0.8%, and methyl acrylate was not detected.

Embodiment 3

[0050] Take a 1000ml four-necked flask and fully dry it, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 100cP, start stirring for 300r / min, vacuumize and remove water at 90°C for 60min, cool down to 70°C, add 20.5g dimethoxy Dichloropropylsilane, stirred for 15min, added 0.6g phosphoric acid, reacted for 4h, added 42g of chloropropyltrimethoxysilane, reacted for 3h, removed the low boiling point under the condition of 110℃, 6mbar, and added p-hydroxyanisole to the obtained product 0.015g, 18g sodium acrylate, stir evenly, add 2.6g of tetramethylammonium hydroxide, heat up to 80°C for 4h, then heat up to 150°C, extract low boiling under 5mbar, filter under positive pressure to obtain product III, which is tested for its silicon Hydroxyl residue was 0.6%, methyl acrylate was not detected.

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Abstract

The invention discloses a dual-curable polysiloxane and a preparation method and application thereof. The polysiloxane molecular structure contains acrylate groups, which can be quickly cross-linked and cured under ultraviolet light conditions, and the end group structure contains moisture curing groups, so the polymer has both moisture curing and UV light curing. Ability. The synthesis route provided by the invention can avoid the formation of acrylate, and the residual silanol is less than 1%, meanwhile, the energy required for light curing of the polymer is reduced, and the ability of the cured product to resist moisture and heat aging is improved.

Description

technical field [0001] The invention relates to a dual-curable polysiloxane, a preparation method and application thereof, and belongs to the field of silicon materials. Background technique [0002] The unique molecular structure of silicone enables it to combine the properties of inorganic materials and organic materials. It has excellent properties such as oxidation resistance stability, weather resistance, flame retardancy, hydrophobicity, corrosion resistance, and physiological inertness. It is widely used in electronic circuits. Protection of boards and main components. [0003] Ultraviolet light curing technology has the characteristics of fast curing, energy saving, room temperature curing, less pollution and superior performance. It is a new generation of green chemical technology. A photosensitive group is introduced into the molecular chain of polysiloxane to make it photocurable polysiloxane to improve its curing efficiency, which not only saves energy but also ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/385C08G77/398C09D183/04C09J183/04
CPCC08G77/38C08G77/385C08G77/398C09D183/04C09J183/04Y02P20/10
Inventor 马伟张聪颖张雨刘志锋曹骏封玲珑高源杨继鹏
Owner WANHUA CHEM GRP CO LTD
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