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Safe separation method for increasing yield of methyl phenyl dialkoxy silicane

A technology of methylphenyldialkoxysilane and methylphenyldichlorosilane, which is applied in the field of organosilicon chemistry, can solve the problems of heavy separation load, high separation cost, and difficult separation and purification, so as to increase yield, The effect of high yield, safe and efficient separation

Active Publication Date: 2007-10-24
ZHEJIANG KAIHUA SYNTHETIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The object of the present invention is to provide a kind of method that improves the yield of methylphenyldialkoxysilane in the conversion material of methylphenylalkoxysilane, safe and efficient separation of methylphenyldialkoxysilane, to solve In the prior art, the use of methyltrichlorosilane to neutralize the dissolved sodium alkoxide and solid sodium alkoxide residue in the methylphenyl alkoxy conversion material requires heavy separation load, high separation cost and separation and purification of various substances in the neutralization reaction product. Difficult problem while increasing the yield of methylphenyldialkoxysilane

Method used

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  • Safe separation method for increasing yield of methyl phenyl dialkoxy silicane
  • Safe separation method for increasing yield of methyl phenyl dialkoxy silicane
  • Safe separation method for increasing yield of methyl phenyl dialkoxy silicane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The 1000mL three-necked flask equipped with a constant-pressure pressurized funnel, a stirrer and a pH meter was placed in a cold water bath with a temperature of 10.4° C. Under nitrogen protection, the solid content of 564.5g of sodium condensation synthesis was added to the three-necked flask and was 30 %, the methylphenylethoxysilane conversion material with a methylphenyldiethoxysilane content of 13.54%, start stirring, and pass 103.2g of methylphenyldichlorosilane with a concentration of 98.2% within 0.5h. The constant pressure feeding funnel was slowly added dropwise into the three-necked flask. After the dropwise addition of methylphenyldichlorosilane, the temperature of the mixed solution in the three-necked flask was 17.1°C, and the pH value of the mixed solution was 6.9. The mixture obtained by titration was filtered under reduced pressure to obtain 383.9 g of clear filtrate. After GC analysis, its mass composition was 40.92% of toluene, 2.78% of chlorobenzene,...

Embodiment 2

[0031]A 1000mL three-necked flask equipped with a constant-pressure pressurized funnel, a stirrer and a pH meter is placed in a cold water bath with a temperature of 8.6°C, and under a dry air atmosphere, the solid content of adding 560.6g of sodium condensation to the three-necked flask is: 30% methylphenylethoxysilane conversion material with a methylphenyldiethoxysilane content of 13.54%, start stirring, and pass 101.9 g of methylphenyldichlorosilane with a concentration of 90.7% through it within 1 hour. The constant pressure feeding funnel was slowly added dropwise into the three-necked flask. After the dropwise addition of methylphenyldichlorosilane was completed, the temperature of the mixed solution in the three-necked flask was 18.7°C, and the pH value of the mixed solution was 6.6. The mixture obtained by titration was filtered under reduced pressure to obtain 289.7g of clear filtrate. After GC analysis, its mass composition was toluene 41.66%, chlorobenzene 2.84%, me...

Embodiment 3

[0034] The 1000mL three-necked flask equipped with a constant-pressure pressurized funnel, a stirrer and a pH meter was placed in a cold water bath with a temperature of 6.4° C. Under a nitrogen atmosphere, the solid content of adding 570.2g of sodium condensation to the three-necked flask was 32. %, methylphenyldimethoxysilane conversion material with a methylphenyldimethoxysilane content of 17.3%, start stirring, and pass 108.0 g of methylphenyldichlorosilane with a concentration of 95.3% through it within 1.5h. The constant pressure feeding funnel was slowly added dropwise into the three-necked flask. After the dropwise addition of methylphenyldichlorosilane, the temperature of the mixed solution in the three-necked flask was 18.9°C, and the pH value of the mixed solution was 7.0. The mixture obtained by titration was filtered under reduced pressure to obtain 303.5 g of clear filtrate. After GC analysis, its mass composition was 40.32% of toluene, 2.76% of chlorobenzene, 39....

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Abstract

The invention discloses a receiving rate improving method of methylbenzene dialkoxy silicane and safe separating method of methylbenzene alkoxy silicane, which comprises the following steps: adopting methylbenzene dichloro-silicane as neutralizing agent; adding the methylbenzene dichloro-silicane into the transmitting material of methylbenzene alkoxy silicane slowly protected by dried air or nitrogen to neutralize under normal temperature or cooling bath; controlling the pH value of composite material to 2-9; filtering slag after reacting; rectifying the filtrate; separating to recycling the solvent and non-reacted raw material; separating the high-purity methylbenzene dialkoxy silicane under certain reflux rate; increasing the receiving rate of methylbenzene dialkoxy silicane in the transmitting material of methylbenzene alkoxy silicane greatly; fitting for preparing the product of national defence, space aviation, architecture and rubber widely.

Description

technical field [0001] The invention relates to the field of organosilicon chemistry, in particular to a method for improving the yield of methylphenyldialkoxysilane in a methylphenylalkoxysilane conversion material and safely separating the methylphenylalkoxysilane. Background technique [0002] Methylphenyl dialkoxysilane is an important specialty silicone monomer, which is widely used in defense, aerospace, construction and rubber fields. Through Grignard method, sodium condensation method, redistribution method, etc., alkoxysilanes with a higher degree of hydrocarbylation and mixed hydrocarbon groups can be further prepared from methylphenyl dialkoxysilane. Methylphenyl dialkoxysilane can also be directly used as a weather-resistant and waterproof additive for coatings to reduce the hygroscopicity, anti-adhesion and electromagnetic properties of coatings; it can also be used as an anti-crosslinking agent for silicone rubber to improve the performance of silicone rubber. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 伍川蒋剑雄邱化玉袁志伟丁列华西林
Owner ZHEJIANG KAIHUA SYNTHETIC MATERIAL
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