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Preparation method of trimethylsilanol

A technology of trimethylsilanol and hexamethyldisilazane, which is applied in the field of preparation of trimethylsilanol, can solve problems such as complex use of raw materials, insufficient environmental protection, and complicated processes, and achieve single raw materials and easy expansion The effect of less production and consumption

Pending Publication Date: 2020-10-23
苏州矽索新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above-mentioned preparation method of this trimethylsilanol has the advantage of few by-products, but there are still some shortcomings in the above-mentioned preparation method of this trimethylsilanol, such as: one, poor controllability during the reaction; two, The use of raw materials is relatively complicated and the amount used is large; 3. There are still some by-products, and the environmental protection is not good enough; 4. The process is relatively complicated and requires post-processing steps

Method used

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  • Preparation method of trimethylsilanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] refer to figure 1 , a preparation method of trimethylsilanol, specifically comprising the following steps:

[0029] S1. Select raw materials: select the following components by weight for use: 450 parts of hexamethyldisilazane, 45 parts of glacial acetic acid, and 90 parts of water;

[0030] S2. Mixing: Add water and glacial acetic acid into a 1000ml four-necked bottle, stir it evenly after mixing, and then heat the mixture to 60°C;

[0031] S3, reaction: add hexamethyldisilazane dropwise to the mixed solution obtained in S2, and react for 2 hours;

[0032] S4. Rectification: distill the solution obtained in S3 to obtain trimethylsilanol with a purity of more than 98%.

[0033] Among them, the ammonia gas produced during the S3 reaction is absorbed and treated by the tail gas recovery device.

[0034] Wherein, when S3 reacts, use HNMR detection means to confirm that the reaction generates trimethylsilanol.

[0035] Wherein, during S4 distillation, the distillation t...

Embodiment 2

[0039] refer to figure 1 , a preparation method of trimethylsilanol, specifically comprising the following steps:

[0040] S1. Select raw materials: select the following components by weight for use: 480 parts of hexamethyldisilazane, 45 parts of glacial acetic acid, and 100 parts of water;

[0041] S2. Mixing: Add water and glacial acetic acid into a 1000ml four-necked bottle, stir it evenly after mixing, and then heat the mixture to 65°C;

[0042] S3. Reaction: add hexamethyldisilazane dropwise to the mixed solution obtained in S2, and react for 2.4 hours;

[0043] S4. Rectification: distill the solution obtained in S3 to obtain trimethylsilanol with a purity of more than 98%.

[0044] Among them, the ammonia gas produced during the S3 reaction is absorbed and treated by the tail gas recovery device.

[0045] Wherein, when S3 reacts, use HNMR detection means to confirm that the reaction generates trimethylsilanol.

[0046] Wherein, during S4 distillation, the distillatio...

Embodiment 3

[0049] refer to figure 1 , a preparation method of trimethylsilanol, specifically comprising the following steps:

[0050] S1. Select raw materials: select the following components by weight for use: 520 parts of hexamethyldisilazane, 45 parts of glacial acetic acid, and 100 parts of water;

[0051] S2. Mixing: Add water and glacial acetic acid into a 1000ml four-necked bottle, stir it evenly after mixing, and then heat the mixture to 68°C;

[0052] S3. Reaction: add hexamethyldisilazane dropwise to the mixed solution obtained in S2, and react for 3 hours;

[0053] S4. Rectification: distill the solution obtained in S3 to obtain trimethylsilanol with a purity of more than 98%.

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Abstract

The invention discloses a preparation method of trimethylsilanol. The preparation method is characterized by specifically comprising the following steps: S1, selecting raw materials: selecting, by weight for later use: 450-550 parts of hexamethyldisilazane, 45-55 parts of glacial acetic acid and 90-110 parts of water; S2, mixing: adding water and glacial acetic acid into a 1000 ml four-necked bottle, mixing, uniformly stirring, and then heating the mixed solution to 60-70 DEG C; S3, reacting: dropwise adding hexamethyldisilazane into the mixed solution obtained in step S2, and reacting for 2-3hours; and S4, rectifying: distilling a solution obtained in step S3 to obtain trimethylsilanol with the purity of 98% or above. The preparation method of the trimethylsilanol has the advantages of simple raw materials, short manufacturing process, less production waste and the like.

Description

technical field [0001] The invention relates to the field of trimethylsilanol preparation, in particular to a preparation method of trimethylsilanol. Background technique [0002] The CAS number of trimethylsilanol is 1066-40-6, also known as trimethylsilanol, trimethylhydroxysilane, trimethylsilanol 25G. [0003] The boiling point of trimethylsilanol is 100°C, the autoignition point is 395°C, the relative density is 0.8112 (20 / 4°C, and the refractive index is 1.3880 (20°C). It is easy to dehydrate and condenses into hexamethyldisiloxane. And it can be obtained by It is obtained by hydrolysis of trimethylchlorosilane. In the preparation of silicone oil and silicone rubber, its condensate - hexamethyldisiloxane can be used as a capping group. The hydroxyl group in the Si-O bond of trimethylsilanol is not Stable, under the action of acid or alkali, or under the condition of heat, it will condense and dehydrate to generate hexamethyldisiloxane. [0004] Can refer to the Chine...

Claims

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Application Information

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IPC IPC(8): C07F7/08
CPCC07F7/0836
Inventor 李杰张彩云刘巨文
Owner 苏州矽索新材料有限公司
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