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Preparation method of vinyl phenyl silicone oil with high phenyl content

A vinyl phenyl silicon, high phenyl technology, applied in the field of preparation of vinyl phenyl silicone oil, can solve the problems of low refractive index and light transmittance of phenyl silicone oil, and achieve high phenyl content and good light transmittance , the effect of high refractive index

Pending Publication Date: 2020-06-30
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 traditional phenyl silicone oil is made by the method of hydrolysis and condensation of diphenyldialkoxysilane and dimethyldialkoxysilane, and the refractive index and light transmittance of the obtained phenyl silicone oil are not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Follow the steps below to prepare vinylphenyl silicone oil with high phenyl content:

[0021] (1) DMC and tetramethylammonium hydroxide pentahydrate with a mass ratio of 70:30 are heated to 75° C., stirred and mixed for 5 hours at a speed of 400 r / min, and vacuumized to reflux to remove water to obtain an alkali gel catalyst;

[0022] (2) Heat octamethylcyclotetrasiloxane and octaphenylcyclotetrasiloxane with a mass ratio of 75:25 to 75°C, stir and mix for 75 minutes, and vacuum dehydrate for 1 hour to obtain methylphenylcyclotetrasiloxane oxane mixture;

[0023] (3) Add divinyltetraphenyldisiloxane to the methylphenylcyclosiloxane mixture obtained in step (2) and mix evenly, then add the alkali gel catalyst obtained in step (1) and heat it to 100°C for 400r Stirring and mixing at a speed of 1 / min for 5 hours obtained the mixture, and the mass ratio of divinyltetraphenyldisiloxane, methylphenylcyclosiloxane mixture and alkali gel catalyst was 2:100:1;

[0024] (4) Con...

Embodiment 2

[0026] Follow the steps below to prepare vinylphenyl silicone oil with high phenyl content:

[0027] (1) DMC and tetramethylammonium hydroxide pentahydrate with a mass ratio of 60:20 are heated to 70° C., stirred and mixed for 4 hours at a speed of 600 r / min, and vacuumized to reflux to remove water to obtain an alkali gel catalyst;

[0028] (2) Heat octamethylcyclotetrasiloxane and octaphenylcyclotetrasiloxane with a mass ratio of 65:15 to 70°C, stir and mix for 90 minutes, and vacuum dehydrate for 1 hour to obtain methylphenylcyclotetrasiloxane oxane mixture;

[0029] (3) Add divinyltetraphenyldisiloxane to the methylphenylcyclosiloxane mixture obtained in step (2) and mix evenly, then add the alkali gel catalyst obtained in step (1), heat to 90°C and then 600r Stirring and mixing at a speed of 1 / min for 4 hours to obtain the mixture, the mass ratio of divinyltetraphenyldisiloxane, methylphenylcyclosiloxane mixture, alkali gel catalyst is 1:100:1;

[0030] (4) Continue to ...

Embodiment 3

[0032] Follow the steps below to prepare vinylphenyl silicone oil with high phenyl content:

[0033] (1) DMC and tetramethylammonium hydroxide pentahydrate having a mass ratio of 80:40 are heated up to 80° C., stirred and mixed for 6 hours at a speed of 300 r / min, and vacuumized to reflux to remove water to obtain an alkali gel catalyst;

[0034] (2) Heat octamethylcyclotetrasiloxane and octaphenylcyclotetrasiloxane with a mass ratio of 85:30 to 80°C, stir and mix for 60 minutes, and vacuum dehydrate for 1 hour to obtain methylphenylcyclotetrasiloxane oxane mixture;

[0035] (3) Add divinyltetraphenyldisiloxane to the methylphenylcyclosiloxane mixture obtained in step (2) and mix evenly, then add the alkali gel catalyst obtained in step (1), heat to 110°C and then 300r Stirring and mixing at a speed of 1 / min obtained the mixture for 6 hours, and the mass ratio of divinyltetraphenyldisiloxane, methylphenylcyclosiloxane mixture and alkali gel catalyst was 3:100:1;

[0036] (4)...

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PUM

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Abstract

The invention provides a preparation method of vinyl phenyl silicone oil with high phenyl content, wherein the preparation method comprises the following steps: (1) heating DMC and a tetramethylammonium hydroxide pentahydrate to 70-80 DEG C, stirring and mixing for 4-6 h, and vacuumizing, refluxing and dewatering to obtain an alkali gel catalyst; (2) heating octamethylcyclotetrasiloxane and octaphenylcyclotetrasiloxane to 70-80 DEG C, stirring and mixing for 60-90 min, and vacuumizing and dehydrating for 1 h to obtain a methylphenylcyclosiloxane mixture; (3) adding divinyl tetraphenyl disiloxane into the methyl phenyl cyclosiloxane mixture, uniformly mixing, adding an alkali gel catalyst, heating to 90-110 DEG C, and stirring and mixing for 4-6 h to obtain a mixture; and (4) continuously heating the mixture to 150-165 DEG C, decomposing the alkali gel catalyst for 0.5-1.5 h under a stirring condition, vacuumizing, carrying out reduced pressure distillation to remove low-boiling-point substances, and thus obtaining the vinyl phenyl silicone oil with high phenyl content. The vinyl phenyl silicone oil prepared by the preparation method disclosed by the invention has relatively high refractive index, light transmittance and relatively good heat resistance.

Description

technical field [0001] The invention relates to a preparation method of vinyl phenyl silicone oil with high phenyl content. Background technique [0002] There are many kinds of silicone oil in silicone products, among which phenyl silicone oil is one of the main varieties. Phenyl silicone oil has insulation, ozone resistance, water-repellent and moisture-proof, high and low temperature resistance and radiation resistance, and is widely used in the fields of electronics, machinery and daily chemical products. High-refractive index LED (light-emitting diode) encapsulant is a high-end product among LED encapsulation materials. Its function is to maximize the output of the luminous flux of the LED chip, and at the same time control the spatial distribution of the output light, and play the role of an optical lens. Vinyl phenyl silicone oil is an important raw material for the preparation of LED silicone encapsulants. The higher the refractive index and light transmittance, the...

Claims

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Application Information

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