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Method for preparing organic silicon end-capping reagent containing phenyl vinyl by using grignard method

A technology of phenylvinyl and silicone, which is applied in the field of silicone end-capping agents, can solve the problems of many side reactions, high equipment requirements, and easy pollution of the environment, and achieve the effect of mild reaction conditions and suppression of side reactions

Active Publication Date: 2014-12-10
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

[0008] CN101693720B discloses the method that utilizes phenyl Grignard reagent to prepare phenyl trichlorosilane or diphenyl dichlorosilane, during concrete operation, under the protection of nitrogen, drop in magnesium and lithium chloride and chlorobenzene and initiator, synthesize phenyl lattice Then add silicon tetrachloride to react to synthesize phenyltrichlorosilane or diphenyldichlorosilane. This method uses chlorosilane as a raw material. Chlorosilane is easily hydrolyzed and condensed to generate hydrochloric acid when it sees water vapor, which corrodes equipment and causes relatively large pollution. , and more side effects
This method also uses chlorosilane as a raw material, which is easy to pollute the environment, requires high equipment, and has many side reactions.

Method used

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  • Method for preparing organic silicon end-capping reagent containing phenyl vinyl by using grignard method
  • Method for preparing organic silicon end-capping reagent containing phenyl vinyl by using grignard method
  • Method for preparing organic silicon end-capping reagent containing phenyl vinyl by using grignard method

Examples

Experimental program
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Embodiment 1

[0024] A 500ml four-necked flask equipped with a constant pressure dropping funnel, a thermometer, a stirrer, a condenser and a nitrogen gas introduction system, purging the flask with nitrogen, replacing the air in the bottle; 60% ether and 24g magnesium chips and 6.28g Put a mixture of 40% methyl ether and 47.1g of bromobenzene in a flask, stir and heat up to about 140°C; smoke appears in the bottle, indicating that the reaction has started, keep the temperature at about 150°C, and add the remaining 25.12g of 60% ether And the mixture of 40% methyl ether and 188.4g of bromobenzene, continue to react for 5h, obtain the reaction product Grignard reagent containing phenyl; keep the temperature of Grignard reagent containing phenyl at 50°C, then slowly add 132g of methyl vinyl Dimethoxysilane, the dropping time is 135min. After the dropping is completed, stir at a constant temperature of 60°C for 4 hours, cool to room temperature, filter out the suspended matter, and distill the ...

Embodiment 2

[0026] A 500ml four-necked flask equipped with a constant pressure dropping funnel, a thermometer, a stirrer, a condenser and a nitrogen gas introduction system, purging the flask with nitrogen to replace the air in the bottle; Put chlorobenzene in the flask, stir and raise the temperature to about 140°C; smoke appears in the bottle, indicating that the reaction has started, keep the temperature at about 150°C, add the remaining 12.58g of ether and 191.25g of chlorobenzene, continue the reaction for 5h, Obtain the phenyl-containing Grignard reagent of the reaction product; keep the phenyl-containing Grignard reagent temperature at 50° C., then slowly add 132 g of methylvinyldimethoxysilane dropwise for 150 min. Stir at a constant temperature of 60°C for 4 hours, cool to room temperature, filter out the suspended matter, distill the filtrate at atmospheric pressure, distill off ether, excess chlorobenzene and methylvinyldimethoxysilane, cut off the fraction at 181-183°C to obtai...

Embodiment 3

[0028] A 500ml four-necked flask equipped with a constant pressure dropping funnel, a thermometer, a stirrer, a condenser and a nitrogen gas introduction system, purging the flask with nitrogen, replacing the air in the bottle; Put a mixture of 20% methyl ether and 78.5g of bromobenzene in a flask, stir and heat up to about 140°C; smoke appears in the bottle, indicating that the reaction has started, keep the temperature at about 150°C, and add the remaining 27.36g of 80% ether and 20% methyl ether mixture and 314g of bromobenzene, and continue to react for 5h to obtain a phenyl-containing Grignard reagent; keep the phenyl-containing Grignard reagent temperature at 45°C, and then slowly add 160g of methyl vinyl di Ethoxysilane, the dropping time is 135min. After the dropping is completed, stir at 60°C for 4 hours, cool to room temperature, filter out the suspended matter, and distill the filtrate under atmospheric pressure to distill off ether, excess bromobenzene and methyl V...

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Abstract

The invention discloses a method for preparing an organic silicon end-capping reagent containing phenyl vinyl by using a grignard method. The method is characterized by comprising the following steps: (1) reacting chlorobenzene or bromobenzene with magnesium metal in an ether solvent so as to form a grignard reagent; (2) reacting the grignard reagent with silane with vinyl in an ether solvent so as to form a required organic silicon end-capping reagent; and (3) filtering and distilling, thereby obtaining the organic silicon end-capping reagent containing phenyl vinyl. The method for preparing the organic silicon end-capping reagent containing phenyl vinyl is gentle in reaction conditions, and the yield is greater than 90%.

Description

technical field [0001] The invention relates to a method for preparing a phenylvinyl-containing organosilicon end-capping agent by using a coupling reaction of a phenyl-containing Grignard reagent and a vinyl-containing silane. Background technique [0002] In polymer chemistry and organic synthesis, end groups have a great influence on the properties of polymers. Many polymers need to be end-capped, so end-capping agents are used. The monofunctional end-blocking agent added in the polycondensation reaction can change the two end groups of the polycondensate into the same functional group, thereby terminating the polymerization reaction. In addition to being used as a molecular weight regulator, the end-capping agent sometimes has the function of deactivating the end group or bringing active groups, increasing the thermal stability of the polymer or improving its reactivity. [0003] Silicone end-capping agent is an indispensable raw material in silicone chemistry, and play...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C07F7/12
Inventor 朱淮军戴子林涂伟萍
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI