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Synthesis method of ditertbutyldichlorosilane

A technology of di-tert-butyldichlorosilane and a synthesis method, which is applied in chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, organic chemistry, etc. The problem of low production cost and high production cost can achieve the effect of reducing production cost, low cost and convenient operation.

Inactive Publication Date: 2013-11-27
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 grid reaction is gas, and the reaction is exothermic, requiring huge energy Consumption to cool down, high production cost; chlorination is catalyzed by precious metal palladium, and at the same time, toxic carbon tetrachloride is used as 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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  • Synthesis method of ditertbutyldichlorosilane
  • Synthesis method of ditertbutyldichlorosilane
  • Synthesis method of ditertbutyldichlorosilane

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Embodiment Construction

[0017] Di-tert-butyldichlorosilane synthetic method, said reaction chemical reaction formula is

[0018]

[0019] In the first step, under the protection of nitrogen, 2.1 equivalents of magnesium chips and a certain amount of tetrahydrofuran are added to the reaction kettle, and tetrahydrofuran is the Grignard reagent. , after the above reaction is initiated, control the temperature in the reactor below 50°C and add a total of 1 equivalent of tert-chlorobutane dropwise, and after the dropwise addition, keep the temperature at 50-52°C for 2 hours;

[0020] 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 the kettle was between -8°C and -5°C, and after the dropwise addition was completed, the temperat...

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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 existing technology is mainly synthesized by two steps of grid substitution and palladium-catalyzed chlorination, the product cost is high, and it 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 grid reaction is gas, and the reaction is exothermic, requiring huge energy Consumptio...

Claims

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Application Information

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