Method for preparing phenyl trialkyl alkoxy silane by nucleophilic method

A technology of phenyltrialkoxysilane and tetraalkoxysilane, which is applied in the field of synthesis of organosilicon compounds, can solve the problems of extremely high requirements for equipment drying, unfavorable large-scale production, and high risk of reaction, and achieve the elimination of unnecessary Potential safety hazards, moderate and controllable production conditions, and the effect of less dosage

Inactive Publication Date: 2015-09-23
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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Problems solved by technology

However, the alcoholysis method will produce acid gas in the production process, seriously corrode the production equipment, pollute the environment, and is not conducive to large-scale industrial production; while the Grignard method is more dangerous because of the high activity of the Grignard reagent. The requirements are extremely high, and the problems such as difficult separation of products are not conducive to industrialization

Method used

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  • Method for preparing phenyl trialkyl alkoxy silane by nucleophilic method

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Experimental program
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Effect test

Embodiment 1

[0030] Under the protection of nitrogen, add 23g of sodium block into 92g of toluene, then add 0.46g of palmitic acid, and heat to 102°C to prepare metal sodium particle suspension. Add the metal sodium particle suspension to the mixed solution of 63.75g chlorobenzene and 345g tetramethoxysilane, then add 0.43g cyclodextrin, react at 40°C for 5h, stop the reaction, and filter the reaction mixture, Distillation under reduced pressure gave phenyltrimethoxysilane with a yield of 86.5%.

Embodiment 2

[0032] Under nitrogen protection, add 46g of sodium block to 230g of toluene, then add 0.77g of paraffin, heat to 107°C to prepare a suspension of metallic sodium particles, lower the temperature to 40°C, add 120.79g of chlorobenzene dropwise to metallic sodium In the particle suspension, after 3 hours of reaction, a phenyl sodium suspension is generated, and then the phenyl sodium suspension is added dropwise to a mixture of 1230.2g tetraethoxysilane and 1.37g 15-C-5, at 40°C , reacted for 4h, stopped the reaction, filtered the reaction mixture, and rectified under reduced pressure to obtain phenyltriethoxysilane with a yield of 78%.

Embodiment 3

[0034] Under the protection of nitrogen, add 72g of sodium block to 504g of toluene, then add 1.26g of oleic acid, heat to 112°C to prepare metal sodium particle suspension, lower the temperature to 45°C, add 172.13g of chlorobenzene dropwise to the metal In the sodium particle suspension, react for 2 hours to form a phenyl sodium suspension, and then add the phenyl sodium suspension dropwise to a mixture of 1630.3g tetramethoxysilane and 1.63g 18-C-6, at 45°C , reacted for 2.5 hours, stopped the reaction, filtered the reaction mixture, and rectified under reduced pressure to obtain phenyltrimethoxysilane with a yield of 70%.

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Abstract

The invention belongs to the technical field of synthesis of organosilicon compound and particularly relates to a method for preparing phenyl trialkyl alkoxy silane by a nucleophilic method. Under inertia gas protection, the method includes adding sodium into methylbenzene and dispersant, heating and preparing metal sodium metallic particle suspension; adding metal sodium metallic particle suspension into mixed liquid of halogeno benzene and tetraalkoxy silane, then adding reaction accelerant, rectifying to obtain phenyl trialkyl alkoxy silane products after reaction mixture is subjected to solid-liquid separation; or adding halogeno benzene into the metal sodium metallic particle suspension to react to prepare phenyl alkali metal sodium salt suspension, adding the phenyl alkali metal sodium salt suspension into mixed liquid of tetraalkoxy silane and reaction accelerant, and rectifying to obtain phenyl trialkyl alkoxy silane products after reaction mixture is subjected to solid-liquid separation. The preparation conditions of normal pressure, low temperature, simple operation, mildness and controllability are achieved and industrialization is facilitated.

Description

technical field [0001] The invention belongs to the technical field of synthesis of organosilicon compounds, and in particular relates to a method for preparing phenyltrialkoxysilane by a nucleophilic method. Background technique [0002] Phenyltrialkoxysilane is a very important organosilicon functional compound and an important raw material for the production of phenylsilicone resin and high-end liquid silicone rubber. In particular, the introduction of phenyl groups into silicon atoms can greatly improve the performance of organic silicon materials, such as improving the heat resistance, radiation resistance, chemical stability, and excellent optical properties of organic silicon products, making organic silicon materials widely used in national defense, aviation, etc. , chemical, medical and other fields have great application value. [0003] Nowadays, the methods of synthesizing phenylalkoxysilane often use methods such as alcoholysis method and Grignard method. Howev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 胡庆超宋超徐晓光刘海龙王安营刘殿忠李云杰张振玉许栋沈惟龙张停毛宁张学迪朱永和周磊周玲
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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