Nucleophilic method used for preparing phenylmethyldialkoxysilanes

A technology of methyl phenyl dialkoxy silane and methyl trialkoxy silane is applied in the synthesis field of organosilicon compounds, which can solve the problem of difficult separation of by-products and target monomers, extremely high requirements for drying of instruments and equipment, and metal Problems such as troublesome handling of halogen salts, to achieve the effect of enhancing rapid progress and offensive capabilities, eliminating unsafe hidden dangers, and mild and controllable production conditions

Inactive Publication Date: 2016-01-20
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is a Grignard method, and its disadvantages are also very obvious, namely: a large number of flammable and explosive organic solvents such as ether, toxic such as tetrahydrofuran, etc., are very harmful to the environment and people; it is difficult to separate by-products from target monomers ; Grignard reagent is very active, and has extremely high requirements on the drying of instruments and equipment. It is easy to explode when encountering active hydrogen, and the risk is high; the treatment of a large amount of metal halide salts is also troublesome.

Method used

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  • Nucleophilic method used for preparing phenylmethyldialkoxysilanes

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Effect test

Embodiment 1

[0043] A nucleophilic method for preparing methylphenyldialkoxysilane includes the following steps:

[0044] (1) Under the protection of nitrogen, add 23g of sodium block to 69g of toluene, then add 0.33g of paraffin, and heat to 99°C to prepare a metal sodium particle suspension;

[0045] (2) Add the metal sodium particle suspension to the mixture of 62.5g chlorobenzene and 227g methyltrimethoxysilane, then add 0.32g 15-crown-5, and react for 2h at 38°C to stop the reaction. The reaction mixture was filtered and rectified under reduced pressure to obtain methylphenyldimethoxysilane with a yield of 87%.

Embodiment 2

[0047] A nucleophilic method for preparing methylphenyldialkoxysilane includes the following steps:

[0048] (1) Under the protection of nitrogen, add 23 g of sodium block to 115 g of toluene, then add 0.35 g of oleic acid, and heat to 102° C. to prepare a metal sodium particle suspension;

[0049] (2) Add the metal sodium particle suspension to the mixture of 59.2g chlorobenzene and 358.5g methyltrimethoxysilane, then add 0.45g 15-crown-5, and react for 7h at 44℃, stop the reaction After the reaction mixture is filtered, it is rectified under reduced pressure to obtain methylphenyldimethoxysilane with a yield of 67%.

Embodiment 3

[0051] A nucleophilic method for preparing methylphenyldialkoxysilane includes the following steps:

[0052] (1) Under the protection of nitrogen, add 23g of sodium block to 138g of toluene, then add 0.31g of oleic acid, and heat to 104°C to prepare a metal sodium particle suspension;

[0053] (2) Add the metal sodium particle suspension to the mixture of 56.25g of chlorobenzene and 408.66g of methyltrimethoxysilane, then add 0.45g of 15-crown-5, and react for 5h at 52°C to stop the reaction After the reaction mixture is filtered, it is rectified under reduced pressure to obtain methylphenyldimethoxysilane with a yield of 67%.

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Abstract

The invention relates to a nucleophilic method used for preparing phenylmethyldialkoxysilanes. The nucleophilic method comprises following steps: 1) under protection of insert gas, metallic sodium is cut into small pieces and is added into an organic solvent, a dispersing agent is added, and an obtained solution is heated so as to obtain a brightly silvery sodium particle suspension; and 2) the brightly silvery sodium particle suspension is added into a mixed solution of halogeno benzene and methyl trialkoxysilane, and a reaction accelerator is added so as to obtain a phenylmethyldialkoxysilane product, or halogeno benzene is added into the brightly silvery sodium particle suspension so as to obtain a phenyl alkali metal sodium suspension, and the phenyl alkali metal sodium suspension is added into a mixed solution of methyl trialkoxysilane and the reaction accelerator so as to obtain the phenylmethyldialkoxysilane product. Operation of the nucleophilic method is carried out under normal pressure; the nucleophilic method is mild and controllable; phenylmethyldialkoxysilane can be obtained with high yield; and the nucleophilic method is suitable for industrialized and large-scale production.

Description

Technical field [0001] The invention belongs to the synthetic field of organosilicon compounds and relates to a method for preparing methylphenyldialkoxysilane by a nucleophilic method. Background technique [0002] Methyl phenyl dialkoxy silane is a very important organosilicon functional compound and an important raw material for the production of phenyl silicone oil and high-end liquid silicone rubber. In particular, the introduction of phenyl groups into silicon atoms can greatly improve and enhance the performance of silicone materials, such as the heat resistance, radiation resistance, chemical stability, and excellent optical properties of silicone products, making silicone materials useful in national defense, Aviation, chemical, medical and other fields have great application value. [0003] At present, the methods for synthesizing methyl phenyl silane monomer mainly include direct method, Grignard method, sodium condensation method and so on. The direct method has a hig...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 宋超伊港周磊周玲朱永和
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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