Preparation method of tetramethyldivinyldisilazane

A technology of tetramethyldivinyldisilazane and dimethylvinylchlorosilane, which is applied in the field of synthetic silicone resin raw material preparation, can solve the problems of a large number of solvents, complicated processes, and reduced yields of similar substances, and achieve simplification The effect of production process, avoiding complicated process and avoiding side reactions

Active Publication Date: 2012-11-07
XINYAQIANG SILICON CHEM JIANGSU
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

However, the production route of the solvent method has the following disadvantages: a, due to the use of a large amount of solvent, two moles of ammonium chloride salts are generated while one mole of congeners are generated in the reaction, resulting in a significant decline in production capacity; b, the separation process of congeners and solvents requires A lot of energy consumption; c, the purity of similar substances is poor
In addition, in the preparation process of the congeners of tetramethyldivinyldisilazane, salt compounds are generated while the congeners are obtained. Therefore, the prior art uses a filtration desalination method to separate the congeners from the generated salts. Separation of compounds, resulting in complex process, greater loss of solvent and congeners, resulting in lower yield of congeners
[0004] Aiming at the shortcomings of the preparation method of the above-mentioned congeners of tetramethyldivinyldisilazane that need to use a large amount of solvent, complex process, high energy consumption and low yield, the inventor considers to provide a tetramethyldivinyldisilazane The preparation method of vinyldisilazane is to prepare tetramethyldivinyldisilazane without using a solvent, and has the characteristics of simple process, low energy consumption and high yield

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  • Preparation method of tetramethyldivinyldisilazane
  • Preparation method of tetramethyldivinyldisilazane

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preparation example Construction

[0020] The invention provides a preparation method of tetramethyldivinyldisilazane, which comprises the following steps: step a) adding dimethylvinylchlorosilane into a reaction kettle, and feeding ammonia gas under stirring conditions for reaction, the resulting The mass ratio of dimethylvinylchlorosilane to ammonia is 4.30~4.40:1, the reaction temperature is 110~115°C, and the reaction pressure is 0.15~0.18MPa; step b) add sodium hydroxide solution into the reaction kettle, and after stirring Tetramethyldivinyldisilazane is obtained.

[0021] In the above preparation process, the present invention reacts dimethylvinylchlorosilane and ammonia under solvent-free conditions, which simplifies the production process, reduces energy consumption, and increases the yield. The ammonia gas is preferably stored in the form of liquid ammonia, and the liquid ammonia is converted into ammonia gas during the process of passing the liquid ammonia into the reactor. The reaction formula of d...

Embodiment 1~4

[0034] Pump dimethyl vinyl chlorosilane into 1m 3 In the enamel reaction kettle, stir at a speed of 120 rpm, and at the same time slowly add liquid ammonia raw materials for reaction. The reaction time is 12 hours, and the ammonia flow rate reaches 99% within 2 hours. Control the reaction temperature and reaction pressure. The temperature of the water close to the jacket does not change within one hour, and the pressure remains unchanged for 180 minutes after the pressure approaches the upper limit of the operation;

[0035] Add 200Kg of concentrated 25% sodium hydroxide solution to the reaction kettle, stir for 30min, and obtain the crude product of tetramethyldivinyldisilazane;

[0036] The crude product of tetramethyldivinyldisilazane is subjected to batch rectification to obtain the finished product of tetramethyldivinyldisilazane.

[0037] Raw material ratio and reaction conditions of table 1 embodiment 1~4

[0038]

[0039] It can be seen from the above examples tha...

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Abstract

The invention discloses a preparation method of tetramethyldivinyldisilazane. The preparation method includes the following steps: dimethylvinylchlorosilane is added in a reaction kettle, ammonia is led in to perform reaction under the stirring condition, mass ratio of the dimethylvinylchlorosilane and the ammonia is 4.30-4.40:1, reaction temperature is 110-115 DEG C, and reaction pressure is 0.15-0.18 MPa; and sodium hydroxide solution is added in the reaction kettle, and the tetramethyldivinyldisilazane is obtained after stirring. Compared with the prior art, the dimethylvinylchlorosilane and the ammonia are reacted under the solvent-free condition, production process is simplified, energy consumption is reduced, and yield is improved. The preparation method of the tetramethyldivinyldisilazane uses the sodium hydroxide solution as salt dissolving agent, adopts alkaline water desalination technology, and avoids the problems of complicated process, severe loss, environment hazards and the like caused by filtration desalination in the prior art.

Description

technical field [0001] The invention relates to the technical field of preparation of synthetic silicone resin raw materials, in particular to a preparation method of tetramethyldivinyldisilazane. Background technique [0002] Tetramethyldivinyldisilazane is a colorless transparent liquid with the molecular formula C 8 h 19 NSi 2 , with a molecular weight of 185.42, is used in the preparation of silicone rubber, silicone colloid and vinyl silicone resin, and is also a commonly used adhesion promoter in the field of negative photoresists. However, there are few reports on the industrial production process of tetramethyldivinyldisilazane at home and abroad. [0003] At present, the congeners of tetramethyldivinyldisilazane (hereinafter referred to as congeners) are all prepared by solvent method by taking advantage of the feature that chlorides are easily soluble in water. However, the production route of the solvent method has the following disadvantages: a, due to the us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10
Inventor 初亚军
Owner XINYAQIANG SILICON CHEM JIANGSU
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