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Synthetic method of di-tert-butyldichlorosilane

A technology of di-tert-butyldichlorosilane and a synthesis method, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc. It can reduce the production cost, reduce the cost and reduce the energy consumption.

Inactive Publication Date: 2017-01-25
ANQING FENGYUAN CHEM
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Problems solved by technology

[0004] Problems and shortcomings of existing technical solutions: the raw material is dichlorohydrosilane, which is a gas at room temperature, and has risks in transportation and storage; the dichlorohydrosilane in the Grignard reaction is gas, and the reaction is exothermic, requiring huge Energy consumption is used to cool down, and the production cost is high; chlorination is catalyzed by precious metal palladium, and at the same time, toxic carbon tetrachloride is used as a chlorine source
Among them, the recycling rate of palladium is low, and the production cost is high; at the same time, the pressure on environmental protection is high.

Method used

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  • Synthetic method of di-tert-butyldichlorosilane

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Embodiment Construction

[0014] Di-tert-butyldichlorosilane synthetic method, said reaction chemical reaction formula is

[0015] ;

[0016] In the first step, under the protection of nitrogen, add 2.1 equivalents of magnesium chips and a certain amount of tetrahydrofuran into the reaction kettle, and drop a small amount of chloro-tert-butane to initiate the reaction. After the above reaction is initiated, control the temperature in the reaction kettle at 50°C Add a total of 1 equivalent of chloro-tert-butane dropwise. After the dropwise addition, keep warm at 50-52°C for 2 hours, and tetrahydrofuran is a Grignard reagent with a concentration of 3-5 moles per liter;

[0017] In the second step, a certain amount of tetrahydrofuran and 1.0 equivalent of trichlorohydrosilane are added to a dry reaction kettle to form a solution, and the ice salt water is lowered to -5°C in the kettle, and the Grignard reagent prepared above is added dropwise to control During the dropwise addition, the temperature in ...

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Abstract

The invention discloses a synthesis method of ditertbutyldichlorosilane. The chemical equation of the reaction is shown in the specification. The synthesis method disclosed by the invention overcomes the shortcomings in the prior art; great modification is made based on format substitution and catalytic chlorination; the production risk is reduced; the energy consumption is reduced; the solvent with low toxicity is used; simultaneously, the chlorination utilization rate is improved; and the cost is reduced.

Description

technical field [0001] The invention relates to the technical field of organic synthesis methods suitable for large-scale industrial production, and specifically belongs to the synthesis method of di-tert-butyldichlorosilane. Background technique [0002] As a common organosilicon material, di-tert-butyldichlorosilane has attracted much attention in its synthesis research and amplification technology. The prior art mainly adopts two-step synthesis of Grignard substitution and palladium-catalyzed chlorination, and the product cost is high, which is not suitable for industrialization. The technical solutions generally adopted for this product in China are: [0003] [0004] Problems and shortcomings of existing technical solutions: the raw material is dichlorohydrosilane, which is a gas at room temperature, and has risks in transportation and storage; the dichlorohydrosilane in the Grignard reaction is gas, and the reaction is exothermic, requiring huge Energy consumption...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
Inventor 毛晓宇
Owner ANQING FENGYUAN CHEM
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