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Method for synthesizing phenyl methyl dialkoxyl silane with high selectivity

A technology of phenylmethyldialkoxysilane and methyltrialkoxysilane, which is applied in the field of organosilicon chemical industry, can solve problems affecting heat and mass transfer, side reactions, and high reaction temperature, so as to improve selectivity and yield, make up for costs, and increase yield

Inactive Publication Date: 2013-05-22
天津楷美肽生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Although this method solves the shortcomings of high reaction temperature in the synthesis of phenylmethyldialkoxysilane by the one-step Grignard reagent method, but because the reaction must use tetrahydrofuran as a solvent, the magnesium salt generated by the reaction in this solvent Filtration of by-product alkoxymagnesium chloride is very difficult
Although it is possible to remove part of THF by distillation, and then add xylene and continue distillation to remove the remaining THF, but due to the strong coordination between these magnesium salts and THF, it is difficult to completely remove THF by distillation.
Moreover, heating a mixture containing a large amount of magnesium salt residue and reaction products can seriously affect the heat and mass transfer during heating
In this case, overheating is easy to occur, and other side reactions occur, affecting the yield and purity of the target product
As a result, the yield of the phenylmethyldialkoxysilane obtained by this method is low, and a large amount of diphenyl substituted by-products are generated, that is, the reaction selectivity is very poor

Method used

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  • Method for synthesizing phenyl methyl dialkoxyl silane with high selectivity
  • Method for synthesizing phenyl methyl dialkoxyl silane with high selectivity

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Embodiment 1

[0048] Embodiment 1 (this embodiment is not included in the scope of the present invention as a comparative example. In a 5L four-necked flask, add 241g methyltrimethoxysilane and 1000mL tetrahydrofuran. Start stirring, add dropwise 1030mL concentration of 1.72mol / L The solution of chlorophenyl Grignard reagent in tetrahydrofuran.After reacting for 1 hour, most of tetrahydrofuran was evaporated by heating.Add 1000mL dimethylbenzene, continue to distill remaining tetrahydrofuran.Filter after being down to room temperature, filtrate obtains 99g phenylmethyl dihydrofuran through fractional distillation Methoxysilane (31% yield) and 69 g of diphenylmethylmethoxysilane (17% yield).

Embodiment 2

[0050] Add 377g of methyltriethoxysilane and 1000mL of ether into a 5L four-neck flask, and add dropwise 1080mL of bromophenyl Grignard reagent ether solution with a concentration of 1.63mol / L under stirring; Filtration; the filtrate is fractionated, reclaimed ether and excess methyltriethoxysilane, then distilled under reduced pressure to obtain phenylmethyldiethoxysilane 316g (yield 86%) and diphenylmethylethoxysilane 11 g (yield 3%) of silane.

Embodiment 3

[0052] Add 240g of methyltrimethoxysilane and 1000mL of ether into a 5L four-neck flask, and add dropwise 1080mL of bromophenyl Grignard reagent ether solution with a concentration of 1.63mol / L under stirring; 1000 mL of n-hexane was added to the system, and then filtered; the filtrate was fractionated to obtain 305 g of phenylmethyldimethoxysilane (yield 95%) and 4 g of diphenylmethylmethoxysilane (yield 1%).

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Abstract

The invention relates to a method for synthesizing phenyl methyl dialkoxyl silane with high selectivity. The structural formula of phenyl methyl dialkoxyl silane is PhMeSi(OR)2, in which R is alkyl with 1-6 carbons. The method is characterized by comprising the following steps of: performing reaction with methyl trialkoxyl silane based on non-cyclic ether compounds such as ethyl ether as a reaction liquor and a bromobenzene Grignard reagent as a raw material; and then, obtaining the target compound, i.e., phenyl methyl dialkoxyl silane with high selectivity and high yield through simple filtering and fractional purification, and meanwhile, greatly inhibiting the generation of a byproduct diphenyl methyl alkoxyl silane.

Description

technical field [0001] The invention belongs to the field of organosilicon chemical industry, and in particular relates to a synthesis method of polysiloxane industrial monomer, that is, phenylmethyldialkoxysilane. This monomer has a particularly important application in the synthesis of high-performance polymethylphenylsiloxane. Background technique [0002] Phenylsilane is an important monomer in the organosilicon chemical industry. Its consumption is second only to methylsilane monomer. It is one of the basic raw materials for the synthesis of phenyl silicone oil, phenyl silicone rubber and phenyl silicone resin. For polysiloxane obtained from methylsilane monomer, after introducing a certain proportion of phenyl monomer into its main chain, it can endow it with excellent high and low temperature resistance, radiation resistance and physical and mechanical properties, and can also improve Its compatibility with organic compounds and inorganic fillers increases the refrac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 孙怀林王国伟高成强
Owner 天津楷美肽生物科技有限公司
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