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A kind of preparation method of tetramethyl divinyl diphenyl trisiloxane

A technology of tetramethyldivinyldiphenyltrisiloxane and divinylsilazane, which is applied in the field of synthesizing organosilicon compounds, can solve the problems of low yield and difficult scale-up, and achieve high yield Effect

Active Publication Date: 2020-08-07
INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Usually, diphenyldichlorosilane or diphenyldimethoxysilane, tetramethyldivinyldisiloxane, water are used as raw materials, and toluene is used as a solvent, and hydrolysis and condensation are carried out under the action of a catalyst to form different polymers. phenylvinylpolysiloxane mixture containing 2 to 4% tetramethyldivinyldiphenyltrisiloxane with a single degree of polymerization, and the yield is low
In the above-mentioned aqueous reaction system, the hydrolysis rate of diphenyldichlorosilane or diphenyldimethoxysilane and the end-capping rate of tetramethyldivinyldisiloxane have a large difference, inevitably Diphenyldichlorosilane or diphenyldimethoxysilane self-hydrolysis and condensation reaction will occur, and it is difficult to form a large amount of tetramethyldivinyldiphenyltrisiloxane with a single degree of polymerization with the end-capping agent. Therefore, in order to obtain a large amount of tetramethyldivinyldiphenyltrisiloxane, it is difficult to scale up by using aqueous phase hydrolysis and high temperature distillation

Method used

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  • A kind of preparation method of tetramethyl divinyl diphenyl trisiloxane
  • A kind of preparation method of tetramethyl divinyl diphenyl trisiloxane
  • A kind of preparation method of tetramethyl divinyl diphenyl trisiloxane

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Effect test

Embodiment 1

[0025] Add 216g of n-heptane to a 2L dry four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a stirrer, and a condenser, weigh 216g of diphenylsilanediol and add it to the flask to form a mixed dispersion. Slowly add 216g of 1,1,3,3-tetramethyl-1,3-divinylsilazane to the liquid funnel dropwise for 1 hour. After the dropwise addition, raise the temperature to 90°C and continue stirring for 2 hours. Pressure distillation, cut off the fraction at 140~144℃ / 1mmHg to obtain a colorless transparent liquid, which is tetramethyldivinyldiphenyltrisiloxane. Weighing 357g, the yield is 92.97%, and the chromatographic detection content is 99.46%.

Embodiment 2

[0027] Add 250g of n-heptane to a 2L dry four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a stirrer, and a condenser tube, weigh 216g of diphenylsilanediol and add it to the flask to form a mixed dispersion. Slowly add 222g of 1,1,3,3-tetramethyl-1,3-divinylsilazane dropwise into the liquid funnel for 1.5 hours. After the dropwise addition, raise the temperature to 100°C and continue stirring for 2 hours. The system becomes transparent. Distill under reduced pressure and cut off the fraction at 140-144°C / 1mmHg to obtain a colorless transparent liquid, which is tetramethyldivinyldiphenyltrisiloxane. Weighing 362g, the yield is 94.27%, and the chromatographic detection content is 99.51%.

Embodiment 3

[0029] Add 280g of n-heptane to a 2L dry four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a stirrer, and a condenser tube, weigh 216g of diphenylsilanediol and add it to the flask to form a mixed dispersion. Slowly add 250g of 1,1,3,3-tetramethyl-1,3-divinylsilazane dropwise into the liquid funnel for 1 hour. After the dropwise addition, raise the temperature to 120°C and continue stirring for 3 hours. Pressure distillation, cut off the fraction at 140~144℃ / 1mmHg to obtain a colorless transparent liquid, which is tetramethyldivinyldiphenyltrisiloxane. Weighing 368g, the yield is 95.58%, and the chromatographic detection content is 99.56%.

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Abstract

The invention belongs to the technical field of synthesis of organic silicon compounds, and discloses a preparation method of tetramethyl divinyl diphenyl trisiloxanae. The preparation method comprises the following steps: stirring at room temperature, dropwise adding 1,1,3,3-tetramethyl-1,3-divinyl silazane into a mixed dispersion solution of diphenyl silanediol and n-heptane, heating to 90 to 120 DEG C, continuously stirring for 2 to 4 hours, decompression rectifying, intercepting 1mmHg of fraction at 140 to 144 DEG C, and obtaining the tetramethyl divinyl diphenyl trisiloxane. By adopting an anhydrous system reaction, the situation that the diphenyl dichlorosilane or dimethoxydiphenylsilane serving as raw material is easy to have hydrolysis and condensate into a polymer in the water system can be avoided. The 1,1,3,3-tetramethyl-1,3-divinyl silazane has high alkality and can have self-catalytic reaction without additional catalyst. The invention provides the preparation method of the tetramethyl divinyl diphenyl trisiloxane which is simple in process, stable in quality and high in yield.

Description

technical field [0001] The invention belongs to the technical field of synthesizing organosilicon compounds, and in particular relates to a preparation method of tetramethyldivinyldiphenyltrisiloxane. Background technique [0002] Tetramethyldivinyldiphenyltrisiloxane belongs to the category of vinyl phenyl silicone oil, which is a vinyl-terminated phenyl silicone oil with a special structure and has the smallest degree of polymerization, that is, the degree of polymerization is 1. It also has the properties of vinyl phenyl silicone oil, and can be used as a chain extender, diluent and polymer modification intermediate in the preparation of silicone rubber. [0003] Described tetramethyl divinyl diphenyl trisiloxane structural formula is as follows: [0004] [0005] Appearance is colorless and transparent liquid, refractive index (25°C): 1.5057, boiling point: 140~144°C / 1mmHg. [0006] Tetramethyldivinyldiphenyltrisiloxane is an important organic silicon intermediate, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08
CPCC07F7/0874
Inventor 朱淮军戴子林
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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