Synthesis method of phenyl hydrogen-containing silicone oil

A technology of phenyl hydrogen-containing silicone oil and synthesis method, which is applied in the field of synthesis of organic polymer compounds, can solve problems such as difficult process control, high cost, and serious pollution, and achieve simple and easy process operation, good transparency, and high refraction rate effect

Active Publication Date: 2011-02-16
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing relevant patents mainly include: one is the early preparation by hydrolysis of chlorosilane, but the process is difficult to control,

Method used

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  • Synthesis method of phenyl hydrogen-containing silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 432g of diphenyldihydroxysilane into a 3000ml three-necked flask containing 1500g of toluene and 320g of pyridine, and slowly drop into a mixed solution of 230g of methylhydrogendichlorosilane and 300g of toluene under vigorous stirring, and the dropping temperature is controlled at 25°C the following. After the dropwise addition was completed, stirring was maintained at room temperature for 60 min. Then add 40°C deionized water, and wash the organic layer repeatedly until neutral. The organic layer was taken, and 201 g of D4, 39 g of hexamethyldisiloxane and 37.8 g of concentrated sulfuric acid were added to react at room temperature for 4 hours. Then stand for stratification, remove sulfuric acid, then add 1000g of 3% sodium bicarbonate solution and stir for 15min, remove the water layer, and then repeatedly wash the organic layer with 40°C deionized water until neutral. After the organic layer was filtered, the solvent was removed by heating, and the low molecu...

Embodiment 2

[0027] Add 432g of diphenyldihydroxysilane into a 3000ml three-necked flask containing 1500g of toluene and 320g of pyridine, and slowly drop into a mixed solution of 230g of methylhydrogendichlorosilane and 300g of toluene under vigorous stirring, and the dropping temperature is controlled at 25°C the following. After the dropwise addition was completed, stirring was maintained at room temperature for 60 min. Then add deionized water at 50°C, and wash the organic layer repeatedly until neutral. The organic layer was taken, and 148g of DMC (dimethylsiloxane mixed ring, D3-D5), 35.9g of hexamethyldisiloxane and 35g of concentrated sulfuric acid were added to react at room temperature for 4 hours. Then stand for stratification, remove sulfuric acid, add 1000g of 3% sodium bicarbonate solution and stir for 15min, remove the water layer, and then repeatedly wash the organic layer with deionized water at 50°C until neutral. After the organic layer was filtered, the solvent was re...

Embodiment 3

[0029] Add 432g of diphenyldihydroxysilane into a 3000ml three-necked flask containing 1500g of toluene and 320g of pyridine, and slowly drop into the mixed solution of 460g of methylhydrogendichlorosilane and 300g of toluene under vigorous stirring, and the dropping temperature is controlled at 25°C the following. After the dropwise addition was completed, stirring was maintained at room temperature for 60 min. Then add deionized water at 60°C, and wash the organic layer repeatedly until neutral. The organic layer was taken, and 33g of D4, 36.1g of hexamethyldisiloxane and 48g of concentrated sulfuric acid were added to react at room temperature for 4 hours. Then stand for stratification, remove sulfuric acid, then add 1000g of 3% sodium bicarbonate solution and stir for 15min, remove the water layer, and then repeatedly wash the organic layer with deionized water at 60°C until neutral. After the organic layer was filtered, the solvent was removed by heating, and the low mo...

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Abstract

The invention provides a synthesis method of phenyl hydrogen-containing silicone oil. The synthesis method comprises the following steps of: removing hydrogen chloride from diphenylsilanediol and methyl hydrogen dichlorosilane serving as raw materials under the action of an acid receiving agent; performing a balanced reaction under a strong-acid condition; and decoloring, filtering, and removing a solvent and a low-boiling-point substance so as to obtain the phenyl hydrogen-containing silicone oil. The synthesis method has the advantages of readily available raw materials, mild reaction condition and simple and practical process. The viscosity of the phenyl hydrogen-containing silicone oil obtained by the method of the invention is between 200 and 500 mm<2>/s, the refractive index is between 1.50 and 1.53 and the hydrogen content is between 0.2 and 0.6 percent. The phenyl hydrogen-containing silicone oil can be used in crosslinking curing reactions of a light-emitting diode (LED) potting compound and other addition polysiloxanes with high refractive indexes and has the characteristics of quick curing, attractive appearance and high refractive index.

Description

technical field [0001] The invention relates to a method for synthesizing organic polymer compounds, in particular to a method for synthesizing phenyl hydrogen-containing silicone oil. Background technique [0002] With the development of human society, energy problems and environmental problems are becoming more and more serious. How to save energy more economically and environmentally friendly has become an urgent problem to be solved. According to statistics, lighting currently accounts for about 20% of the world's total energy consumption. Replacing traditional light sources with low efficiency and high power consumption with light sources with low energy consumption, long life, and environmental protection and safety is undoubtedly an important breakthrough to solve this problem. [0003] Light-emitting diode, referred to as LED, is a kind of electroluminescent solid-state device, and its structure is mainly composed of PN junction chip, electrode and optical system. C...

Claims

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Application Information

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IPC IPC(8): C08G77/06C08G77/12
Inventor 吴国相龚蓉
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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