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Method for preparing tert-butyldimethyl chlorosilane

A technology of tert-butyldimethylchlorosilane and cyclohexane, which is applied in the field of preparation of tert-butyldimethylchlorosilane, can solve the problems of solvent loss, incomplete dehydration of filter cake, decomposition and disproportionation of chlorosilane, etc. Achieve the effects of easy control, stable product yield and simple production operation

Inactive Publication Date: 2010-09-01
HAIMEN BEST FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the fine-particle magnesium salt is easy to pass through the filter bag and enter the filtrate. When heating and rectifying, it is easy to cause the decomposition and disproportionation of chlorosilane.
The deliquification in the filter cake is not complete, the solvent loss is serious, and part of the product dissolved in the solvent is also taken away

Method used

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  • Method for preparing tert-butyldimethyl chlorosilane
  • Method for preparing tert-butyldimethyl chlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] like figure 1 Shown, a kind of preparation method of tert-butyldimethylsilyl chloride,

[0022] a. In the synthesis kettle, put 10g of magnesium into a mixed solvent of 160ml of ether and cyclohexane, the volume ratio of ether and cyclohexane in the mixed solvent is 6.5:3.5, drop Add a mixed solution composed of 35g tert-butyl chloride and 50g dimethyldichlorosilane, and keep it warm for 2.5 hours after dropping to obtain the synthesized material;

[0023] b. Transfer the synthesized material into the dissolution tank, drop the temperature to 10°C and add 400ml of hydrochloric acid with a volume concentration of 25%, static layering, remove the waste water at the bottom, and obtain the upper layer of material liquid;

[0024] c. Transfer the upper layer material liquid in the dissolving tank to the rectifying tank for purification, remove the solvent, and obtain the product tert-butyldimethylchlorosilane.

Embodiment 2

[0026] like figure 1 Shown, a kind of preparation method of tert-butyldimethylsilyl chloride,

[0027] a. In the synthesis kettle, put 12g of magnesium into a mixed solvent composed of 200ml of ether and cyclohexane. The volume ratio of ether and cyclohexane in the mixed solvent is 7:3. At 50°C, add dropwise A mixed solution composed of 45g tert-butyl chloride and 65g dimethyldichlorosilane was incubated for 3 hours after dropping to obtain the synthesized material;

[0028] b. Transfer the synthesized material into the dissolution tank, drop the temperature to 12.5°C and add 500ml of hydrochloric acid with a volume concentration of 28%, static layering, remove the waste water at the bottom, and obtain the upper layer of feed liquid;

[0029] c. Transfer the upper layer material liquid in the dissolving tank to the rectifying tank for purification, remove the solvent, and obtain the product tert-butyldimethylchlorosilane.

Embodiment 3

[0031] like figure 1 Shown, a kind of preparation method of tert-butyldimethylsilyl chloride,

[0032] a. In the synthesis kettle, put 15g of magnesium into a mixed solvent of 240ml of ether and cyclohexane. The volume ratio of ether and cyclohexane in the mixed solvent is 7.5:2.5. At 55°C, add dropwise A mixed solution composed of 55g tert-butyl chloride and 78g dimethyldichlorosilane was incubated for 3.5 hours after dropping to obtain the synthesized material;

[0033] b. Transfer the synthesized material into the dissolution tank, drop the temperature to 15°C, add 600ml of hydrochloric acid with a volume concentration of 30%, static layering, remove the waste water at the bottom, and obtain the upper layer of material liquid;

[0034] c. Transfer the upper layer material liquid in the dissolving tank to the rectifying tank for purification, remove the solvent, and obtain the product tert-butyldimethylchlorosilane.

[0035] The invention has the advantages that the produc...

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Abstract

The invention relates to a method for preparing tert-butyldimethyl chlorosilane, which is characterized by comprising the following steps of: a, in a synthesis kettle, putting 10 to 15 weight parts of magnesium into 160 to 240 volume parts of mixed solvent consisting of ether and cyclohexane, dripping mixed solution consisting of 35 to 55 weight parts of tertiary butyl chloride and 50 to 78 weight parts of dimethyl dichlorosilane into the mixed solvent at the temperature of between 40 and 55 DEG C, a preserving heat for 2.5 to 3.5 hours after the dripping is finished to obtain a synthesized material; b, transferring the synthesized material to a dissolution kettle, cooling the synthesized material to between 10 and 15 DEG C, then dripping 400 to 600 volume parts of 25 to 30 percent hydrochloric acid into the dissolution kettle, standing and demixing the solution, and removing wastewater at the bottom to obtain upper liquor; and c, transferring the upper liquor in the dissolution kettle to a rectification kettle to perform purification, and removing the solvent to obtain a tert-butyldimethyl chlorosilane product. The method has the advantages of simple synthesis process, high safety and stable product yield.

Description

technical field [0001] The invention relates to a preparation method of tert-butyldimethylchlorosilane, which belongs to the field of chemical industry. Background technique [0002] Tert-butyl dimethyl chlorosilane, English name: Tert-butyl dimethyl chlorosilane, molecular formula: t-C 4 h 9 (CH 3 ) 2 SiCl, the appearance is: white transparent crystal, boiling point: 124°C-126°C, melting point: 87°C-90°C. [0003] At present, the most widely used method is to make Grignard reagent (tert-butyl magnesium chloride) with tert-butyl chloride and magnesium, and then react with dimethyldichlorosilane. [0004] Since the Grignard reagent is very sensitive to moisture, the raw materials used and the equipment flow must be kept dry. During the reaction process, a dry inert gas is usually used for protection to prevent moisture from entering the reaction system, so as to ensure the safe and smooth progress of the reaction. [0005] Metal magnesium is mostly used in the state of m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12
Inventor 杨鹤炉徐斌蔡斌
Owner HAIMEN BEST FINE CHEM
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