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Process for preparing tetramethyldivinyldisilazane by conversion of divinyl tetramethyl disiloxane

A technology of tetramethyldivinyldisilazane and tetramethyldivinyldisilazane is applied in the field of preparation of tetramethyldivinyldisilazane and can solve the problem of tetramethyldivinyldisilazane. The problems of small disilazane output and high production cost can achieve the effect of avoiding ammonia waste, thorough reaction and solving pollution

Inactive Publication Date: 2012-10-17
XINYAQIANG SILICON CHEM JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aiming at the shortcomings in the background technology, the present invention develops a preparation process for converting tetramethyldivinyldisilazane from tetramethyldivinyldisiloxane to solve the problem of tetramethyldivinyldisilazane caused by the shortage of raw materials. The output of divinyldisilazane is so small that the cost of subsequent production is too high

Method used

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  • Process for preparing tetramethyldivinyldisilazane by conversion of divinyl tetramethyl disiloxane
  • Process for preparing tetramethyldivinyldisilazane by conversion of divinyl tetramethyl disiloxane

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Embodiment 1

[0021] As shown in the figure, the preparation process steps of converting tetramethyldivinyldisiloxane into tetramethyldivinyldisilazane are:

[0022] 1. Esterification reaction: first put 1200 kg of concentrated sulfuric acid into the dripping tank, then put 800 kg of tetramethyldivinyldisiloxane and 2000 kg of petroleum benzene into the stirring tank, mix and stir for one hour; then pour into the stirring tank Concentrated sulfuric acid was added dropwise, and the dropwise addition was completed within two hours. During the reaction, a gas phase balance device was used to prevent volatilization of benzene and tetramethyldivinyldisiloxane, which not only reduced material loss, but also prevented environmental pollution. The temperature was controlled at 60 Below ℃; stop stirring after the reaction is over, keep the layers static for 60 minutes, release the dilute sulfuric acid at the bottom, and import the crude product of the upper layer into the ammoniation kettle;

[0023...

Embodiment 2

[0027] As shown in the figure, the preparation process steps of converting tetramethyldivinyldisiloxane into tetramethyldivinyldisilazane are:

[0028] 1. Esterification reaction: first put 1000 kg of concentrated sulfuric acid into the dripping tank, then put 600 kg of tetramethyldivinyldisiloxane and 1800 kg of petroleum benzene into the stirring tank, mix and stir for one hour; then pour into the stirring tank Concentrated sulfuric acid was added dropwise, and the dropwise addition was completed within two hours. During the reaction, a gas phase balance device was used to prevent volatilization of benzene and tetramethyldivinyldisiloxane, which not only reduced material loss, but also prevented environmental pollution. The temperature was controlled at 60 Below ℃; stop stirring after the reaction is over, keep the layers static for 60 minutes, release the dilute sulfuric acid at the bottom, and import the crude product of the upper layer into the ammoniation kettle;

[0029...

Embodiment 3

[0033] As shown in the figure, the preparation process steps of converting tetramethyldivinyldisiloxane into tetramethyldivinyldisilazane are:

[0034] 1. Esterification reaction: first put 1400 kg of concentrated sulfuric acid into the dripping tank, then put 1000 kg of tetramethyldivinyldisiloxane and 2200 kg of petroleum benzene into the stirring tank, mix and stir for one hour; then pour into the stirring tank Concentrated sulfuric acid was added dropwise, and the dropwise addition was completed within two hours. During the reaction, a gas phase balance device was used to prevent volatilization of benzene and tetramethyldivinyldisiloxane, which not only reduced material loss, but also prevented environmental pollution. The temperature was controlled at 60 Below ℃; stop stirring after the reaction is over, keep the layers static for 60 minutes, release the dilute sulfuric acid at the bottom, and import the crude product of the upper layer into the ammoniation kettle;

[003...

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Abstract

The invention discloses a process for preparing tetramethyldivinyldisilazane by conversion of divinyl tetramethyl disiloxane. The process comprises steps of: (1) esterification reaction: first adding concentrated sulfuric acid into a dropping tank, and then adding thedivinyl tetramethyl disiloxane and petroleum benzene into a stirring kettle; then dropwise adding concentrated sulfuric acid into the stirring kettle, stopping stirring after reaction, releasing dilute sulfuric acid at the bottom upper, and introducing upper crude product into an ammoniation reactor; (2) ammoniation: opening a circulating water pump and mixing, opening an ammonia inlet valve, and introducing ammonia slowly; and (3) distillation: adding clear liquid into a rectification tower kettle, recovering petroleum benzene and intermediate distillate intermittently for recycling, and then recovering tetramethyldivinyldisilazane, so as to finally leave the target product of tetramethyldivinyldisilazane in the tower kettle. The process of the invention adopts a compressor recovery unit to carry out secondary amination synthesis and usage of ammonia, and avoids ammonia waste caused by the reaction pressure requirement.

Description

technical field [0001] The invention relates to a preparation process of tetramethyldivinyldisilazane, in particular to a preparation process of converting tetramethyldivinyldisilazane from tetramethyldivinyldisilazane. Background technique [0002] At present, there is no preparation process for the synthesis of tetramethyldivinyldisilazane in China except the direct synthesis method of raw material dimethylvinyl chlorosilane. The biggest problem of this method is that the raw material dimethyl vinyl chlorosilane is domestically produced. There is no manufacturer, and the import is more difficult and the quantity is small. Contents of the invention [0003] Aiming at the shortcomings in the background technology, the present invention develops a preparation process for converting tetramethyldivinyldisilazane from tetramethyldivinyldisiloxane to solve the problem of tetramethyldivinyldisilazane caused by the shortage of raw materials. The output of divinyldisilazane is so...

Claims

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Application Information

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IPC IPC(8): C07F7/10
Inventor 初亚军
Owner XINYAQIANG SILICON CHEM JIANGSU
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