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Purification method and application of diethoxytetramethyldisilane

A technology of tetramethyldisilane and diethoxy, which is applied in the field of purification of diethoxytetramethyldisilane, can solve the problems such as the influence of post-treatment vacuum distillation

Active Publication Date: 2016-01-20
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, the presence of a slight excess of ethanol in the reaction system will also have an impact on post-treatment vacuum distillation

Method used

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  • Purification method and application of diethoxytetramethyldisilane
  • Purification method and application of diethoxytetramethyldisilane

Examples

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Embodiment 1

[0034] 1. Preparation method

[0035] (1) Under nitrogen protection, add solvent dichloromethane 100ml and raw material 1,2-dichloro-1,1,2,2-tetramethyldisilane (20g) into a dry 250ml three-necked bottle, stir mechanically, and the system Cool to an internal temperature of 0°C with an ice-salt bath.

[0036] (2) Keeping the internal temperature of the system at 5° C., add absolute ethanol (10 g) dropwise rapidly, and after the dropwise addition is completed, keep the temperature and stir for 10 minutes.

[0037] (3) Keep the internal temperature of the system at 0-5°C, slowly add triethylamine (22g) dropwise, and the dropwise addition is completed in about 30 minutes, and the system is kept at 0-10°C for 30 minutes.

[0038] (4) The reaction system is filtered through the diatomaceous earth layer, and the filter cake is rinsed with cold n-pentane.

[0039] (5) Combine the filtrates, and use a rotary evaporator to steam the low boiling point at a vacuum of -0.09~-0.1MPa and a...

Embodiment 2

[0043] 1. Preparation method

[0044] (1) Under the protection of nitrogen, add 100ml of solvent dichloromethane and raw material 1,2-dichloro-1,1,2,2-tetramethyldisilane (28g) into a dry 250ml three-necked bottle, stir mechanically, and the system Cool with an ice-salt bath to an internal temperature of 5°C.

[0045] (2) Keeping the internal temperature of the system at 5° C., add absolute ethanol (14 g) dropwise quickly, and after the dropwise addition is completed, keep stirring for 10 minutes.

[0046] (3) Keep the internal temperature of the system at 0-5°C, slowly add triethylamine (30.8g) dropwise, and the dropwise addition is completed in about 30 minutes, and the system is kept at 0-10°C for 30 minutes.

[0047] (4) The reaction system is filtered through the diatomaceous earth layer, and the filter cake is rinsed with cold n-pentane.

[0048] (5) Combine the filtrates, and use a rotary evaporator to evaporate the low boiling point; then the concentrated product is ...

Embodiment 3

[0052] 1. Preparation method

[0053] (1) Under nitrogen protection, add solvent dichloromethane 100ml and raw material 1,2-dichloro-1,1,2,2-tetramethyldisilane (20g) into a dry 250ml three-necked bottle, stir mechanically, and the system Cool to an internal temperature of 3°C with an ice-salt bath.

[0054] (2) Keeping the internal temperature of the system at 5° C., add absolute ethanol (10 g) dropwise rapidly, and after the dropwise addition is completed, keep the temperature and stir for 10 minutes.

[0055](3) Keep the internal temperature of the system at 0-5°C, slowly add triethylamine (22g) dropwise, and the dropwise addition is completed in about 30 minutes, and the system is kept at 0-10°C for 30 minutes.

[0056] (4) The reaction system is filtered through the diatomaceous earth layer, and the filter cake is rinsed with cold n-pentane.

[0057] (5) The combined filtrates were distilled under reduced pressure. Distillation conditions: use a rectification column wi...

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Abstract

The invention relates to the technical field of chemical industry, in particular to a purification method and an application of dioxethyl-tetramethyl-disilane. A reduced pressure distillation method is utilized for purifying 1, 2-dioxethyl-1, 1, 2, 2-tetramethyl-disilane, and in the reduced pressure distillation process, fillers of a rectifying column for the reduced pressure distillation include magnesium chips, calcium chloride or mixture of the magnesium chips and the calcium chloride. In purification steps of the 1, 2-dioxethyl-1, 1, 2, 2-tetramethyl-disilane, the magnesium chips and / or calcium chloride are / is used as the fillers in the reduced pressure distillation, so that removal of residual hydrogen chloride and ethanol in a reaction system is facilitated, and the 1, 2-dioxethyl-1, 1, 2, 2-tetramethyl-disilane with high purity can be obtained.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a purification method and application of diethoxytetramethyldisilane. Background technique [0002] 1,2-diethoxy-1,1,2,2-tetramethyldisilane is an organic liquid that can be used to prepare oligomeric silicon compounds, or as a coupling reactant to introduce dimethylethyldisilane into the molecule Oxysilyl fragments. [0003] Diethoxytetramethyldisilane can be prepared by reacting dichlorotetramethyldisilane with ethanol. The raw material 1,2-dichloro-1,1,2,2-tetramethyldisilane is easy to absorb moisture and produce hydrogen chloride , and hydrogen chloride will promote the decomposition of the reaction product 1,2-diethoxy-1,1,2,2-tetramethyldisilane. On the other hand, the presence of a slight excess of ethanol in the reaction system will also have an impact on post-treatment vacuum distillation. Contents of the invention [0004] The purpose of the present inve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/20C07F7/18
Inventor 王万军李金华黄祚刚姜标
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI