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Preparation method of vinyl phenyl silicone oil

A technology of vinyl phenyl silicon and vinyl double head, which is applied in the field of preparation of vinyl phenyl silicone oil, and can solve the problems of high viscosity of vinyl phenyl silicone oil, low refractive index and light transmittance, single preparation method, etc. , to achieve the effects of low viscosity, light transmittance reduction and refractive index improvement

Active Publication Date: 2020-06-16
新纳奇材料科技江苏有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of existing vinyl phenyl silicone oil is comparatively simple, mostly first hydrolyzes phenylalkoxysilane, then reacts with vinyl cyclosiloxane, methyl cyclosiloxane or end-capping agent, and then Product oil-water separation, removal of low-boiling substances, the existing method has the problems of more by-products, low yield, high viscosity of vinyl phenyl silicone oil, low refractive index and light transmittance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Follow the steps below to prepare vinylphenyl silicone oil:

[0023] (1) Add porous ceramics to tetrabutylammonium chloride aqueous solution with a mass concentration of 10%, the mass ratio of porous ceramics to tetrabutylammonium chloride aqueous solution is 1:25, heat to 120°C and stir for 4 hours to obtain a mixture Solution 1, filter the mixed solution 1 to obtain a filter cake 1, wash the filter cake 3 times with deionized water and then dry it at 100°C to obtain a pretreated porous ceramic, add trifluoroform with a mass concentration of 10% to the pretreated porous ceramic In the sulfonic acid aqueous solution, the mass ratio of the pretreated porous ceramics to the trifluoromethanesulfonic acid aqueous solution is 1:18, heated to 120°C and stirred for 4 hours to obtain the mixed solution 2, and filtered the mixed solution 2 to obtain the filter cake 2, and the filter cake 2. After washing 3 times with deionized water, dry at 100°C to obtain solid acid;

[0024] ...

Embodiment 2

[0028] Follow the steps below to prepare vinylphenyl silicone oil:

[0029] (1) Add porous ceramics to tetrabutylammonium chloride aqueous solution with a mass concentration of 10%, the mass ratio of porous ceramics to tetrabutylammonium chloride aqueous solution is 1:25, heat to 120°C and stir for 4 hours to obtain a mixture Solution 1, filter the mixed solution 1 to obtain a filter cake 1, wash the filter cake 3 times with deionized water and then dry it at 100°C to obtain a pretreated porous ceramic, add trifluoroform with a mass concentration of 10% to the pretreated porous ceramic In the sulfonic acid aqueous solution, the mass ratio of the pretreated porous ceramics to the trifluoromethanesulfonic acid aqueous solution is 1:18, heated to 120°C and stirred for 4 hours to obtain the mixed solution 2, and filtered the mixed solution 2 to obtain the filter cake 2, and the filter cake 2. After washing 3 times with deionized water, dry at 100°C to obtain solid acid;

[0030] ...

Embodiment 3

[0034] Follow the steps below to prepare vinylphenyl silicone oil:

[0035] (1) Add porous ceramics to tetrabutylammonium chloride aqueous solution with a mass concentration of 10%, the mass ratio of porous ceramics to tetrabutylammonium chloride aqueous solution is 1:25, heat to 120°C and stir for 4 hours to obtain a mixture Solution 1, filter the mixed solution 1 to obtain a filter cake 1, wash the filter cake 3 times with deionized water and then dry it at 100°C to obtain a pretreated porous ceramic, add trifluoroform with a mass concentration of 10% to the pretreated porous ceramic In the sulfonic acid aqueous solution, the mass ratio of the pretreated porous ceramics to the trifluoromethanesulfonic acid aqueous solution is 1:18, heated to 120°C and stirred for 4 hours to obtain the mixed solution 2, and filtered the mixed solution 2 to obtain the filter cake 2, and the filter cake 2. After washing 3 times with deionized water, dry at 100°C to obtain solid acid;

[0036] ...

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Abstract

The invention provides a preparation method of vinyl phenyl silicone oil, which comprises the following steps: (1) sequentially adding deionized water, solid acid and divinyl tetramethyl disiloxane into a reaction kettle, stirring, mixing, heating to 40-100 DEG C, and dropwisely adding phenyltriethoxysilane into the reaction kettle after the temperature of the reaction kettle is stable; (2) afterdropwise addition of the phenyltriethoxysilane is finished, stirring and reacting for 1-3 hours at 40-100 DEG C, cooling to room temperature, discharging to obtain a reaction solution, and filtering the reaction solution to obtain a filtrate; and (3) washing the filtrate obtained in the step (2) with water until the filtrate is neutral, putting the filtrate into another clean reaction kettle, introducing nitrogen, continuously heating to 60-100 DEG C while stirring, vacuumizing, and carrying out reduced pressure distillation to remove low-boiling-point substances, thereby obtaining the vinyl phenyl silicone oil. The vinyl phenyl silicone oil prepared by the preparation method disclosed by the invention has relatively high refractive index and light transmittance and relatively low viscosity.

Description

technical field [0001] The invention relates to a preparation method of vinyl phenyl silicone oil. Background technique [0002] Vinyl phenyl silicone oil is a basic raw material for LED silicone packaging materials, its quality and technical indicators directly affect the quality of LED lights. The preparation method of existing vinyl phenyl silicone oil is comparatively simple, mostly first hydrolyzes phenylalkoxysilane, then reacts with vinyl cyclosiloxane, methyl cyclosiloxane or end-capping agent, and then Product oil-water separation, removal of low-boiling point substances, the problems of the existing method are that there are many by-products, the yield is not high, the viscosity of the obtained vinylphenyl silicone oil is relatively high, and the refractive index and light transmittance are relatively low. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a preparation method of vinyl phenyl silicone oil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/08C08G77/20
CPCC08G77/08C08G77/20C08G77/80
Inventor 徐守彬余跃
Owner 新纳奇材料科技江苏有限公司
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