A kind of preparation method of silicon hydrogen compound

A technology for silicon hydride compounds and chlorosilanes, applied in the direction of silicon organic compounds, etc., can solve problems such as hindering the use of such compounds, high price of silicon hydride compounds, harsh preparation methods, etc., which is beneficial to laboratory preparation and industrial production. High temperature and high pressure reaction, simple operation effect

Active Publication Date: 2018-02-13
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In a word, silicon hydrogen compounds have a wide range of uses in the fields of organosilicon chemistry, organosilicon polymers and organic synthesis, but due to the limitation of the existing preparation methods, the price is expensive.
[0003] In the prior art, the synthesis methods of silicon hydrogen compounds mainly include: (1) direct synthesis method, the silicon hydrogen compound obtained by this method is a by-product of preparing chlorosilane, and the silicon hydrogen compound obtained is only methyl dichloro Monohydrosilane and dimethyl-chloro-hydrosilane, and the boiling points of the above two silicon hydrogen compounds are 40.4°C and 35.4°C respectively, making their use range relatively narrow
(2) Metal hydrides reduce chlorosilanes or alkoxysilanes, and the reducing agent metal hydrides used in this method are respectively LiAlH 4 , LiH, etc., expensive and dangerous to operate
The characteristics of the existing technology determine that the cost of raw materials for the preparation of silicon hydrogen compounds is relatively high, and the preparation method is harsh, so the obtained silicon hydrogen compounds are expensive, which hinders the use of such compounds

Method used

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  • A kind of preparation method of silicon hydrogen compound
  • A kind of preparation method of silicon hydrogen compound
  • A kind of preparation method of silicon hydrogen compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of preparation method of silicon hydrogen compound, comprises steps as follows:

[0028] (1) In a four-necked round-bottomed flask equipped with a spherical condenser, a thermometer, a constant pressure dropping funnel and a T-type three-way piston, put 1.33g of magnesium chips, and mix 7.85g of phenyldimethylsilyl chloride and 6.63 The mixed solution of g tetrahydrofuran (THF) was slowly added dropwise to magnesium chips, heated to 80°C under the protection of Ar gas atmosphere, and reacted at 80°C with a stirring speed of 10r / min for 24 hours. Cool naturally to room temperature under the protection of atmosphere to obtain an intermediate reaction product;

[0029] (2) At a stirring speed of 10r / min, slowly add H to the intermediate reaction product at a rate of 3 drops per second. 3 o + solution, dropwise added H 3 o + H in solution 3 o + The molar amount of phenyldimethylsilane is equal to that of phenyldimethylsilane, filtered, the filtrate is extracted...

Embodiment 2

[0031] A kind of preparation method of silicon hydrogen compound, comprises steps as follows:

[0032] (1) In a four-neck round bottom flask equipped with a spherical condenser, a thermometer, a constant pressure dropping funnel and a T-shaped three-way piston, put 1.18g of magnesium chips, and mix 9.52g of diphenylmethylchlorosilane and 14.66 The mixed solution of g hexamethylphosphoric triamide (HMPA) was slowly added dropwise to magnesium chips, heated to 90°C under the protection of Ar gas atmosphere, and reacted at 90°C with a stirring speed of 15r / min for 20 hours. After completion, naturally cool to room temperature under the protection of Ar gas atmosphere to obtain an intermediate reaction product;

[0033] (2) At a stirring speed of 15r / min, slowly add H to the intermediate reaction product at a rate of 4 drops per second. 3 o + solution, dropwise added H 3 o + H in solution 3 o + The molar amount of diphenylmethylsilane is equal to that of diphenylmethylchloro...

Embodiment 3

[0035] A kind of preparation method of silicon hydrogen compound, comprises steps as follows:

[0036] (1) In a four-neck round-bottom flask equipped with a spherical condenser, a thermometer, a constant pressure dropping funnel and a T-shaped three-way piston, put 0.45g of magnesium powder, add 4.60g of triphenylchlorosilane to 4.05g of tetrahydrofuran (THF) and hexamethylphosphoric triamide (HMPA) in the mixed solution, obtain mixture, the mass ratio of tetrahydrofuran (THF) and hexamethylphosphoric triamide (HMPA) in the mixed solution is: 2.5:1, will The mixture was slowly added dropwise to the heated magnesium powder, heated to 90°C under the protection of Ar gas atmosphere, and reacted at 90°C with a stirring speed of 16r / min for 20 hours. Cool to room temperature to obtain an intermediate reaction product;

[0037] (2) At a stirring speed of 16r / min, slowly add H to the intermediate reaction product at a rate of 5 drops per second. 3 o + solution, dropwise added H 3...

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Abstract

The present invention relates to a kind of preparation method of silicon hydrogen compound, and this method is under the protection of Ar gas, with tetrahydrofuran (THF) and/or hexamethylphosphoric triamide (HMPA) as solvent, with the derivatization of chlorosilane or chlorosilane react with metal magnesium to prepare silicon hydrogen compounds. The method has the characteristics of cheap and easy-to-obtain raw materials, simple operation, mild reaction conditions and low cost.

Description

technical field [0001] The invention relates to a preparation method of a silicon hydrogen compound, which belongs to the technical field of synthesis of organosilicon compounds. Background technique [0002] Silicon hydrogen compounds are an important class of monomers, through which many new organosilicon compounds and their polymers can be synthesized; silicon hydrogen compounds are also effective hydrosilation reagents, and many useful carbon-functional organic compounds can be synthesized through hydrosilation reactions. Silicon compounds, or modify organosilicon polymer compounds; silicon hydrogen compounds have strong reducing properties, and the reduced products are simple and easy to post-reaction, so they are very useful reducing agents in organic synthesis. In a word, silicon hydrides are widely used in the fields of organosilicon chemistry, organosilicon polymers and organic synthesis, but they are expensive due to the limitation of the existing preparation metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08
Inventor 张洁张林冯圣玉
Owner SHANDONG UNIV
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