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Method for synthesizing phenyl-containing organosilicon monomers

A synthesis method and organosilicon technology, applied in the direction of organic chemistry, chemical instruments and methods, compounds of group 4/14 elements of the periodic table, etc., can solve the problems of high production cost and low yield, achieve fast reaction speed, The effect of high activity and excellent application performance

Inactive Publication Date: 2014-09-03
SICHUAN KELIXIN NEW MATERIALS CO LTD
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Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a method for synthesizing phenyl-containing organosilicon monomers, which uses novel and cheap raw material methyl trimethoxy Base silane, magnesium and chlorobenzene (or bromobenzene) are used as raw materials, using a one-step Grignard method, using iodine as a catalytic initiator, activating and initiating the reaction at a certain temperature for a period of time, then heating up and continuing the reaction to finally obtain methyl Phenyldimethoxysilane and methyldiphenylmethoxysilane solve the problem that the one-step Grignard method has not yet been realized to prepare methylphenyldimethoxysilane, and the yield is low and the production cost is expensive. , to meet the needs of modern industrial production with high yield and low energy consumption

Method used

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  • Method for synthesizing phenyl-containing organosilicon monomers

Examples

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Effect test

Embodiment 1

[0032] Add 150 parts of toluene, 32 parts of methyltrimethoxysilane, 4 parts of magnesium, 5 parts of chlorobenzene, and 0.01 part of iodine into the reaction kettle in sequence, and heat to 80°C for activation and initiation reaction. After activation and initiation reaction for 1 hour, then Raise the temperature to 120°C, and gradually add 55 parts of chlorobenzene. The reaction is complete. Filter and distill to obtain the product methylphenyldimethoxysilane, methyldiphenylmethoxysilane.

[0033] The selectivity of methylphenyldimethoxysilane is 75%, and the selectivity of methyldiphenylmethoxysilane is 5%.

Embodiment 2

[0035] Add 245 parts of 2-methyltetrahydrofuran, 42 parts of methyltrimethoxysilane, 6 parts of magnesium, 8 parts of chlorobenzene, and 0.05 parts of iodine to the reaction kettle in sequence, and heat to 40°C to initiate the activation reaction. After hours, the temperature was raised to 60°C, and 42 parts of chlorobenzene were gradually added. The reaction is complete. Filter and distill to obtain the product methylphenyldimethoxysilane, methyldiphenylmethoxysilane.

[0036] The selectivity of methylphenyldimethoxysilane is 81%, and the selectivity of methyldiphenylmethoxysilane is 4%.

Embodiment 3

[0038] Add 250 parts of toluene, 100 parts of 2-methyltetrahydrofuran, 48 parts of methyltrimethoxysilane, 7 parts of magnesium, 8 parts of chlorobenzene, and 0.1 part of iodine to the reactor in sequence, and heat to 60°C for activation to initiate the reaction. After initiating the reaction for 1.5 hours, the temperature was raised to 110° C., and 40 parts of chlorobenzene were gradually added. The reaction is complete. Filter and distill to obtain the product methylphenyldimethoxysilane, methyldiphenylmethoxysilane.

[0039] The selectivity of methylphenyldimethoxysilane is 85%, and the selectivity of methyldiphenylmethoxysilane is 3%.

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Abstract

The invention discloses a method for synthesizing phenyl-containing organosilicon monomers. The method comprises the steps of performing one-step Grignard reaction on raw materials including methyltrimethoxy silane, magnesium and benzene halide: performing activation initiation reaction in the presence of a catalytic initiator under the condition that a solvent is added or not added, heating, continuously reacting, filtering and distilling to obtain methyl phenyl dimethoxy silane and methyl diphenyl methoxy silane. According to the method, the novel and cheap raw materials including methyltrimethoxy silane, magnesium and chlorobenzene (or bromobenzene) are used, and the raw materials react at a certain temperature by adopting the one-step Grignard method and using iodine as the catalytic initiator, are heated and then continuously react to obtain methyl phenyl dimethoxy silane and methyl diphenyl methoxy silane, thus solving the problem that the preparation of methyl phenyl dimethoxy silane with the one-step Grignard method is not realized at present and the problems of low yield, high production cost and the like when methyl triethoxysilane is used as a raw material, and meeting the requirements of modernized industrial production for high yield and low energy consumption.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing an environmentally friendly and new material of organosilicon phenyl monomer. Background technique [0002] Methylphenyl silicone monomer is usually synthesized by thermal condensation. Thermal condensation generally involves thermal condensation of methyldichlorosilane and chlorobenzene in a fixed bed to generate phenyl monomer methylphenyldichlorosilane and hydrogen chloride. The synthesis cost of this method is relatively low, but because the composition of the thermal condensation product is complex, and the boiling point of the raw material and the product are close, it is difficult to separate later, resulting in a low purity of the product, which makes it difficult to apply it in high-end silicone products; in addition, because the product synthesized by this method The production of carcinogenic polychlorinated biphenyls, etc., is increasingl...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 龚小伦牟浩斌孙建厅
Owner SICHUAN KELIXIN NEW MATERIALS CO LTD
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