Method for preparing dichlorodimethylsilane by virtue of disproportionation

A technology of dimethyldichlorosilane and monomethyltrichlorosilane, which is applied in the field of disproportionation to prepare dimethyldichlorosilane, can solve the problems of inability to carry out catalytic reaction, high temperature and high pressure required for the reaction, and high requirements for process equipment, and achieves excellent performance. Low temperature reaction activity, improved compatibility, good catalyst activity

Active Publication Date: 2014-09-24
诸暨市蔚莱科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The catalysts used in existing patents and literature technologies, amines are used as catalysts, and the reaction conditions are mild and the process is mature, but the selectivity of dimethyl is not good; when phosphate is used as a catalyst, the selectivity of dimethyl is not good; AlCl 3 As a catalyst, the selectivity of dimethylformamide is good, but the reaction needs high temperature and high pressure, which

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step (1) in 500L reactor, add 3-chloropropylethoxysilane 100Kg and 1-methylimidazole 30Kg respectively in N 2 Reflux at 80°C for 24 hours under atmosphere, then cool, wash and dry to obtain 1-propyl-triethoxysilyl-imidazolium chloride ionic liquid.

[0022] Step (2) Add aluminum trichloride 100Kg, 3Kg1-propyl group-triethoxysilyl-imidazolium chloride ionic liquid, 80Kg fluorine intercalation hydrotalcite, 800Kg methyl alcohol to react respectively in i000L reactor, reaction temperature is 70°C, and the reaction time is 30 hours. After the reaction, a composite catalyst of aluminum trichloride and ionic liquid supported by fluorine-intercalated hydrotalcite is obtained.

[0023] Step (3) Add 100Kg of monomethyltrichlorosilane and 60Kg of trimethylchlorosilane into a 500L high-pressure reactor, and 5Kg of the composite catalyst prepared in step (1), raise the temperature to 250°C, and stop heating after 4 hours of constant temperature , cooled to normal temperature to ob...

Embodiment 2

[0025] (1) Add 3-chloropropylethoxysilane 100Kg and 1-methylimidazole 30Kg respectively in 500L reactor, in N 2 Reflux at 60° C. for 48 h under atmosphere, then cool, wash and dry to obtain 1-propyl-triethoxysilyl-imidazolium chloride ionic liquid.

[0026] (2) Add aluminum trichloride 100Kg, 1-propyl-triethoxysilyl-imidazolium chloride ionic liquid 1Kg, fluorine intercalation hydrotalcite 40Kg, ethanol 500Kg respectively in i000L reactor and react, and the reaction temperature is 50°C, and the reaction time is 40 hours. After the reaction, a composite catalyst of aluminum trichloride and ionic liquid supported by fluorine-intercalated hydrotalcite is obtained.

[0027] (3) Add 100Kg of monomethyltrichlorosilane and 50Kg of trimethylchlorosilane in a 500L autoclave, and 5Kg of the composite catalyst prepared in step (1), heat up to 150°C, and stop heating after 8 hours at a constant temperature. Cool to normal temperature to obtain dimethyldichlorosilane. The conversion rate i...

Embodiment 3

[0029] (1) Add 3-chloropropylethoxysilane 100Kg and 1-methylimidazole 30Kg respectively in 500L reactor, in N 2 Reflux at 120° C. for 12 h under atmosphere, then cool, wash, and dry to obtain 1-propyl-triethoxysilyl-imidazolium chloride ionic liquid.

[0030] (2) In a 2000L reactor, add aluminum trichloride 100Kg, 1-propyl-triethoxysilyl-imidazolium chloride ionic liquid 10Kg, fluorine intercalation hydrotalcite 100Kg, butanol 1000Kg to react respectively, and the reaction temperature The temperature is 80°C, and the reaction time is 20 hours. After the reaction, a composite catalyst of aluminum trichloride and ionic liquid supported by fluorine-intercalated hydrotalcite is obtained.

[0031] (3) Add 100Kg of monomethyl trichlorosilane, 100Kg of trimethyl monochlorosilane, and 5Kg of composite catalyst into a 500L high-pressure reactor, heat up to 350°C, keep the temperature for 2 hours, stop heating, and cool to normal temperature to obtain di Methyldichlorosilane. The conv...

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PUM

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Abstract

The invention discloses a method for preparing dichlorodimethylsilane by virtue of disproportionation. The method comprises the following steps: enabling aluminum trichloride, a 1-propyl-triethoxysilyl-imidazole chloride ionic liquid, fluorine intercalated hydrotalcite, aluminum trichloride and alcohol to react; obtaining a composite catalyst of fluorine intercalated hydrotalcite loaded aluminum trichloride and an ionic liquid after completing reaction; and adding methyltrichlorosilane, trimethylsilyl chloride and the composite catalyst into a high-pressure reaction kettle, and reacting to obtain dichlorodimethylsilane. The method disclosed by the invention has the advantages of good catalyst activity, cyclic utilization, small three wastes (waste gas, waste water and waste residues) and environment-friendly.

Description

technical field [0001] The invention relates to a method for preparing organosilicon, in particular to a method for preparing dimethyldichlorosilane by disproportionation. Background technique [0002] The strength of organosilicon monomer production technology directly affects the development of the entire organosilicon industry. Dimethyldichlorosilane ((CH 3 ) 2 SiCl 2 , referred to as dimethyl) is one of the most important monomers, and its consumption accounts for about 80% of the whole monomer production. Most factories will produce more by-products such as monomethyltrichlorosilane (abbreviated as monomethyl, accounting for 10-15%) and trimethylchlorosilane (abbreviated as trimethyl, accounting for 1%) when preparing dimethyl by direct method, but they The use of hydrogen chloride is limited, and direct discharge is easy to react with moisture in the air to form hydrogen chloride, polluting the environment, and there are many inconveniences in long-term storage. It...

Claims

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Application Information

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IPC IPC(8): C07F7/12B01J31/28
Inventor 张玲王新
Owner 诸暨市蔚莱科技有限公司
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