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 cumbersome preparation process, generation of large acid waste water, difficult control, etc., and achieve simple reaction process conditions, reaction Short, easily controlled effects

Active Publication Date: 2015-01-28
NICHE TECH KAISER SHANTOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

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

[0024] The polycondensation reaction was carried out under 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, the solid catalyst in the obtained reaction solution is filtered off, and then...

Embodiment 2

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

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

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

[0035] The polycondensation reaction was carried out under 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, the solid catalyst in the obtained reaction solution is filtered off, and then the low b...

Embodiment 3

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

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

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

[0046] The polycondensation reaction was carried out under 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, the solid catalyst in the obtained reaction solution is filtered off, and then...

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Abstract

A method for preparing phenyl silicone resin with high-refractive index orderly comprises the following steps: (1) carrying out polycondensation in the presence of a solid catalyst, with phenyl silanol and alkoxy silane as monomers; (2) after the polycondensation ends, filtering out the solid catalyst in the obtained reaction liquid, and then removing low-boiling-point substances in the reaction liquid to obtain the phenyl silicone resin with high refractive index. Compared to the prior art, the present invention has the following advantages: 1. the reaction process condition being simple, easy to control and convenient to industrialize; 2. no solvent needing to be added in the preparation process and environment-friendly; 3. no hydrolysis reaction being required in the reaction process and the reaction time being short; 4. after the reaction ends, the catalyst could being removed by filtration, needless to neutralize and washing to remove the catalyst; simplifying the process and reducing the wastewater discharge; and 5. the prepared phenyl silicone resin having a refractive index between 1.56 and 1.60, and having excellent performances such as high refractive index, high light transmittance, radiation resistance and high and low temperature resistance etc.

Description

Technical field [0001] The invention relates to an organic polymer compound, in particular to a method for preparing a high refractive index phenyl silicone resin. Background technique [0002] Phenyl silicone resin has excellent electrical insulation, water repellency, 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) and is suitable for light-emitting diodes (LED ) Package. However, most of the existing phenyl silicone resins have the following problems during the preparation process: a large amount of acidic waste water is generated during the preparation process, or a large amount of solvents are required as the reaction medium, which is severely polluted; the preparation process is complicated and cumbersome and difficult to control. Moreover, with the development of high-power and high-efficiency LEDs, phenyl silicone resins for LED packaging a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06
CPCC08G77/06C08G77/14C08G77/18C08G77/08C08G77/80
Inventor 周振基周博轩
Owner NICHE TECH KAISER SHANTOU
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