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Q-type high-refractive-index phenyl vinyl silicone oil as well as synthesis method and application thereof

A technology of phenylvinyl silicon and synthesis method, which is applied in the direction of adhesives, etc., can solve the problems of difficulty in synthesizing uniform high-refractive silicone oil, poor stability, unfavorable use, etc., and achieve moderate viscosity of the system, good anti-aging performance, suitable for The effect of industrial production

Active Publication Date: 2021-08-31
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Patent CN101885845A uses phenylpolysiloxane and methylcyclosiloxane with a low degree of polymerization to synthesize phenyl silicone oil, which is difficult to synthesize high-refractive silicone oil with uniform arrangement, and its stability is not as good as that of methylphenylsiloxane.
CN105295051A Utilizes the basic catalyst polymerization process to obtain phenyl silicone oil although the phenyl content is high, but the viscosity is also greatly increased at the same time, which is not conducive to downstream use in formulations
There are few reports in the existing literature about the synthesis method of phenyl vinyl silicone oil with high phenyl content and low viscosity

Method used

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  • Q-type high-refractive-index phenyl vinyl silicone oil as well as synthesis method and application thereof
  • Q-type high-refractive-index phenyl vinyl silicone oil as well as synthesis method and application thereof
  • Q-type high-refractive-index phenyl vinyl silicone oil as well as synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Take a 5000ml three-necked flask, condense and reflux, and protect it with nitrogen. Add 869.36g (2mol) of divinyltetraphenyldimethoxysilane, 208.33g (1mol) of tetraethyl orthosilicate, and 215g of ethanol into the reaction kettle. Slowly add 5.3g of concentrated sulfuric acid dropwise for 30min, raise the temperature to 60°C for equilibrium reaction for 1h, add 45g of deionized water to the reaction system for 30min, continue to react at 60°C for 3h, after the reaction is completed, heat up and steam out the ethanol and excess in the reaction system water until the liquid temperature is 105°C; cool down to 85°C, add 10.42g of acetic acid and 8.69g of divinyltetraphenyldimethoxysilane, continue the reaction for 3h, filter to remove the solid after the reaction, take the filtrate and wash it three times until neutral , and finally 120°C and 10mbar negative pressure to distill out excess water and low volatile matter in the system to obtain vinylmethylphenyl Q-type end-cap...

Embodiment 2

[0082] Take a 5000ml three-neck flask, condense and reflux, protect with nitrogen, add 1086.70g (2.5mol) divinyltetraphenyldimethoxysilane, 208.33g (1mol) tetraethyl orthosilicate, and 388g isopropanol into the reaction kettle, Slowly add 12.95g of concentrated sulfuric acid dropwise at room temperature for 30 minutes, raise the temperature to 70°C for equilibrium reaction for 2 hours, add 36g of deionized water to the reaction system for 30 minutes, and continue to react at 70°C for 5 hours. Ethanol, isopropanol and excess water until the liquid temperature is 105°C, then cool down to 85°C, add 6.2g of acetic acid and 16g of divinyltetraphenyldimethoxysilane, continue the reaction for 3h, filter to remove the solid after the reaction, and take The filtrate was washed three times with water until neutral, and finally excess water and low volatile matter in the system were distilled at 120°C and 10mbar negative pressure to obtain vinylmethylphenyl Q-type end-capping agent. The v...

Embodiment 3

[0084] Take a 5000ml three-necked flask, condense and reflux, and protect it with nitrogen. Add 869.36g (2mol) of divinyltetraphenyldimethoxysilane, 208.33g (1mol) of tetraethyl orthosilicate, and 215g of ethanol into the reaction kettle. Slowly add 5.3g of phosphoric acid for 30 minutes, raise the temperature to 75°C for equilibrium reaction for 1.5h, add 45g of deionized water to the reaction system for 1h, continue to react at 75°C for 4h, after the reaction is completed, heat up and steam out the ethanol and excess in the reaction system water, until the liquid temperature is 105°C, cool down to 80°C, add 14.5g of acetic acid and 8.69g of divinyltetraphenyldimethoxysilane, continue the reaction for 3h, filter to remove the solid after the reaction, take the filtrate and wash it three times until neutral , and finally 120°C and 10mbar negative pressure to distill out excess water and low volatile matter in the system to obtain vinylmethylphenyl Q-type end-capping agent. The ...

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Abstract

The invention discloses Q-type high-refractive-index phenyl vinyl silicone oil as well as a synthesis method and application thereof. The silicone oil has a chemical structural expression as shown in a formula described in the specification. The Q-type high-refractive-index phenyl vinyl silicone oil prepared by the invention is used for preparing an LED packaging adhesive, and the cured LED packaging adhesive has relatively high refractive index and light transmittance; and the cross-linking density is higher than that of a common packaging adhesive, and the packaging adhesive has relatively good anti-aging performance and is suitable for being used in a high-power LED (light-emitting diode) lamp.

Description

technical field [0001] The invention relates to a phenyl vinyl silicone oil, in particular to a Q-type high refraction phenyl vinyl silicone oil, a synthesis method thereof and an application in LED packaging materials. Background technique [0002] High-refractive phenyl vinyl silicone oil is the main ingredient of current high-power LED packaging formulation materials. The phenyl content in the silicone oil determines the refractive index after encapsulation and curing. The higher the phenyl content, the greater the increase in the refractive index of the material. In addition, the silicone oil must also take into account the adjustment of the hardness and toughness of the encapsulation material. In order to increase the phenyl content, a larger molecular weight of linear phenyl silicone oil is often required, which will reduce the crosslink density after encapsulation and curing, and reduce its toughness. The greater the degree of polymerization, the greater the hardness ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/08C09J183/07
CPCC08G77/20C08G77/08C09J183/04C08L2205/035C08L2203/206C08L2205/025C08L83/04
Inventor 宋远超封玲珑刘志锋高源杨继朋杨慧雅
Owner WANHUA CHEM GRP CO LTD
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