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Method for preparing phenyl silicone resin with high-refractive index

A technology of phenyl silicone resin and high refractive index, which is applied in the field of preparation of high refractive index phenyl silicone resin, can solve the problems of complex and tedious preparation process, generation of large acidic waste water, difficult control and the like, and achieves simple reaction process conditions and high reaction efficiency. Short, easy-to-control effects

Active Publication Date: 2013-08-07
NICHE TECH KAISER SHANTOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the existing phenyl silicone resins have the following problems in the preparation process: a large amount of acidic waste water is generated during the preparation process, or a large amount of solvent is required as the reaction medium, causing serious pollution; the preparation process is complicated and cumbersome, and it is not easy to control

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In this embodiment, the preparation method of high refractive index phenyl silicone resin comprises the following steps in sequence:

[0022] (1) Using phenylsilanol and alkoxysilane as monomers, polycondensation reaction is carried out under the action of a solid catalyst;

[0023] Above-mentioned phenylsilanol is diphenylsilanediol (its structural formula is HO(Ph 2 SiO)H), the dosage is 19.872g (grams). The above-mentioned alkoxysilane is phenyltrimethoxysilane, and its dosage is 29.15 g. Above-mentioned solid catalyst is potassium hydroxide, and its consumption is 0.3g (the consumption of solid catalyst is about 0.6% of reaction monomer total weight).

[0024] The polycondensation reaction was carried out under the condition of stirring, the reaction time of the polycondensation reaction was 4 hours, and the reaction temperature was 70°C.

[0025] (2) After the polycondensation reaction is completed, filter the solid catalyst in the obtained reaction solution, an...

Embodiment 2

[0032] In this embodiment, the preparation method of high refractive index phenyl silicone resin comprises the following steps in sequence:

[0033] (1) Using phenylsilanol and alkoxysilane as monomers, polycondensation reaction is carried out under the action of a solid catalyst;

[0034] Above-mentioned phenylsilanol is diphenylsilanediol (its structural formula is HO(Ph 2 SiO)H), the dosage is 19.872g (grams). The above-mentioned alkoxysilane is vinyltrimethoxysilane, and its usage amount is 17.75 g. The solid catalyst is a cation exchange resin, and its consumption is 5.64g (the consumption of the solid catalyst is about 15% of the total weight of the reaction monomers).

[0035] The polycondensation reaction was carried out under the condition of stirring, the reaction time of the polycondensation reaction was 3 hours, and the reaction temperature was 90°C.

[0036] (2) After the polycondensation reaction is completed, filter the solid catalyst in the obtained reaction...

Embodiment 3

[0043] In this embodiment, the preparation method of high refractive index phenyl silicone resin comprises the following steps in sequence:

[0044] (1) Using phenylsilanol and alkoxysilane as monomers, polycondensation reaction is carried out under the action of a solid catalyst;

[0045] The structural formula of the above-mentioned phenylsilanol is HO(CH 3 ) 2 SiO(Ph 2 SiO) 3 Si(CH 3 ) 2OH, the amount used is 42.41g (grams). The above-mentioned alkoxysilane is phenyltrimethoxysilane, and its usage amount is 11.6 g. Above-mentioned solid catalyst is sodium hydroxide, and its consumption is 0.31g (the consumption of solid catalyst is about 0.57% of reaction monomer total weight).

[0046] The polycondensation reaction was carried out under the condition of stirring, the reaction time of the polycondensation reaction was 4 hours, and the reaction temperature was 100°C.

[0047] (2) After the polycondensation reaction is completed, filter the solid catalyst in the obtai...

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Abstract

The invention discloses a method for preparing phenyl silicone resin with high-refractive index. The method orderly comprises the following steps of (1) by taking silicone-alcohol and alkoxy silane as monomers, carrying out polycondensation under effect of a solid catalyst; (2) filtering out the solid catalyst in obtained reaction liquid after polycondensation is finished, and removing low-boiling-point substance to the reaction liquid to obtain the phenyl silicone resin with high refractive index. Compared with the prior art, the method has the advantages that 1, the method is simple in reaction process condition, easy to control and convenient to industrialize; 2, no solvent is added in the preparation process; and the method is environment-friendly and free of pollution; 3, the reaction process does not need hydrolysis reaction; and the reaction time is short; 4, the catalyst can be directly filtered after the reaction is finished; neutralization is not needed; the catalyst is removed by washing; the process is simplified; and wastewater discharge is also reduced; and 5, the refractive index of the prepared phenyl silicone resin is between 1.56 and 1.60; and the phenyl silicone resin has excellent performances such as high refractive index, high light transmittance, radiation resistance and high and low temperature resistance.

Description

technical field [0001] The invention relates to organic polymer compounds, in particular to a preparation method of high refractive index phenyl silicone resin. Background technique [0002] Phenyl silicone resin has excellent electrical insulation, hydrophobicity, weather resistance, high temperature and low temperature resistance, radiation resistance and physiological inertness. In addition, it also has a high refractive index (up to 1.53), suitable for use in light-emitting diodes (LED ) package. However, most of the existing phenyl silicone resins have the following problems in the preparation process: a large amount of acid waste water is generated during the preparation process, or a large amount of solvent is required as the reaction medium, causing serious pollution; the preparation process is complex and cumbersome, and is not easy to control. Moreover, with the development of high-power and high-efficiency LEDs, the phenyl silicone resin used for LED packaging is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06
CPCC08G77/08C08G77/80
Inventor 周振基周博轩
Owner NICHE TECH KAISER SHANTOU
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