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A kind of preparation method of siloxane

A technology of siloxane and silane, which is applied in the field of preparation of high-branched vinylphenyl silsesquioxane, can solve the problem of reducing the light transmittance of LED packaging materials, the difficulty of mixing gas phase white carbon black, and the refractive index. Large difference and other problems, to achieve superior anti-ultraviolet performance, improve stability and light transmittance, no gel effect

Inactive Publication Date: 2018-08-24
马凤国
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the addition of fumed silica can significantly improve the mechanical properties of silicone rubber, the mixing of fumed silica is difficult, the dust is large, and it is easy to agglomerate, which makes processing difficult.
The key point is that due to the large difference in refractive index between fumed silica and silicone packaging materials, the addition of fumed silica will reduce the light transmittance of LED packaging materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 20 parts of phenyltrimethoxysilane, 20 parts of xylene, 20 parts of ethanol, 40 parts of deionized water, and 3 parts of divinyltetramethyldisiloxane into a 250ml four-necked flask, and under nitrogen atmosphere, At 30°C, stir rapidly, perform hydrolysis reaction for 1 hour, then raise the temperature to 85°C, add 4 parts of concentrated hydrochloric acid (37wt%), and conduct polycondensation reaction for 6 hours. Wash with water until neutral, distill the product-dissolved solution in nitrogen atmosphere at 100°C for 2 hours, pour the product obtained from the distillation into a petri dish, and remove the low boiling point at 80°C / -0.085MPa The obtained colorless and transparent product vinyl phenyl silsesquioxane. The resulting product nD 25 =1.5575, the vinyl mass percentage content is 2.2% as measured by chemical titration, and the 29 Si NMR measurements show that the product has a uniform structure and a high degree of branching.

Embodiment 2

[0031]18 parts of phenyltrimethoxysilane, 2 parts of methyltrimethoxysilane, 30 parts of toluene, 20 parts of ethanol, 35 parts of deionized water, 2 parts of divinyltetramethyldisiloxane, dimethylethylene Add 1 part of ethoxysilane to a 250ml four-necked flask, stir rapidly under nitrogen atmosphere at 10°C, hydrolyze for 6 hours, then heat up to 75°C, add 6 parts of concentrated hydrochloric acid (37wt%), polycondensate for 8 hours , after the reaction is over, let stand to separate layers, wash the organic phase with resin dissolved in deionized water until neutral, wash the solution with product dissolved in water until neutral, and distill at 60°C for 6h under nitrogen atmosphere, distill the distilled The resulting product was poured into a petri dish, and low boilers were removed at 80°C / -0.085MPa to obtain a colorless and transparent product, vinylphenyl silsesquioxane. The resulting product nD 25 =1.5551, through chemical titration, the vinyl mass percentage content ...

Embodiment 3

[0033] 10 parts of phenyltrimethoxysilane, 5 parts of phenyltriethoxysilane, 5 parts of methyltrimethoxysilane, 40 parts of xylene, 40 parts of isopropanol, 200 parts of deionized water, divinyl tetra Add 2.5 parts of methyldisiloxane into a 250ml four-neck flask, stir rapidly under nitrogen atmosphere at 100°C, and perform hydrolysis reaction for 1 hour, then raise the temperature to 60°C, add 6 parts of concentrated sulfuric acid (96wt%), polycondensation reaction 9h, after the reaction is over, let stand to separate layers, wash the organic phase with resin dissolved in deionized water until neutral, wash the solution with product dissolved in water until neutral, and distill at 20°C for 24h under a nitrogen atmosphere. The distilled product was poured into a petri dish, and the low boilers were removed at 80°C / -0.085MPa to obtain a colorless and transparent product, vinylphenyl silsesquioxane. The resulting product nD 25 =1.5568, the vinyl mass percentage content is 2.14%...

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Abstract

The present invention discloses a preparation method for siloxane, particularly a cross-linking agent applied to reinforcement of an organosilicon material. An acid catalyst is added to a mixed solution of aryl trifunctional silane, alkyl trifunctional silane, an organic solvent, water and a blocking agent for producing a catalytic reaction, resin is washed with water to be neutral after the reaction is finished, and distillation and vacuum drying are carried out to prepare colorless transparent and highly-branched vinyl phenyl silicone resin. The preparation method has the advantages that raw materials are easily available, the operation is simple and easy to control, industrialization is facilitated and the product performance is superior. The product is particularly suitable for use as across-linking agent for micro-lenses, optical coatings and LED packaging materials, further has high potential for use as the cross-linking agent for other organosilicon materials, and is used in aspects of a surface treating agent, a release agent, a defoaming agent, an anti-sticking agent, a brightener, a release force regulator of an addition-type anti-sticking agent, other additives and the like.

Description

technical field [0001] The invention relates to a method for preparing siloxane, in particular to a method for preparing vinylphenyl silsesquioxane with a high degree of branching. technical background [0002] Silicone resin is an organosiloxane with a highly cross-linked network structure, which has the dual characteristics of organic resin and inorganic material, and has unique physical and chemical properties. The introduction of phenyl functional groups into the silicone resin can improve the heat resistance and adhesion of the silicone resin, especially effectively improve the refractive index of the resin. The introduction of vinyl groups endows silicone resin with certain reaction characteristics, especially for the addition reaction with hydrogen silicon groups, which provides a good reaction basis for its use in addition-type silicone rubber. Vinyl phenyl silsesquioxane with a high degree of branching will play a key role in transparent addition silicone rubber, e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/08
Inventor 马凤国刘涛
Owner 马凤国
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