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 high production cost, complex process, and inability to meet the requirements of purity. Separation, simple process, less by-products

Inactive Publication Date: 2019-03-08
湖北新蓝天新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, the prior art has the following disadvantages: 1. The yield of the product is low, generally 70%-80%; 2. The purity of the product is low. At present, the purity can reach 98% at most, which cannot meet the requirements for purity in special fields; 3. The process of product synthesis is complicated, the production cost is high, and the energy consumption is large, which wastes energy

Method used

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Examples

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preparation example Construction

[0023] The embodiment of the present invention provides a preparation method of trimethylsilanol, comprising the following steps:

[0024] S1: Under stirring conditions, add hexamethyldisilazane and phosphoric acid into the reaction kettle, the molar ratio of hexamethyldisilazane and phosphoric acid is 1:1~3;

[0025] S2: After a period of heat preservation and reaction, stir and rinse with a solvent;

[0026] S3: Separation after static layering to obtain trimethylsilanol. The separation method can be to use a pear-shaped separatory funnel to statically layer. The lower layer is the solvent, released from the lower port, and the upper layer is trimethylsilanol. Mouth poured out.

[0027] In step S1, phosphoric acid with a purity of not less than 60% is used.

[0028] In step S1, the stirring speed is 200-400 r / min.

[0029] In step S1, hexamethyldisilazane is added dropwise to phosphoric acid at a rate of 0.7 g / min to 1.0 g / min.

[0030] In step S2, the reaction temperatu...

Embodiment 1

[0040] Hexamethyldisilazane and phosphoric acid are reacted according to the molar ratio of 1:1, the purity of phosphoric acid is 85%, and hexamethyldisilazane is added dropwise at a rate of 0.7g / min into the reactor containing phosphoric acid , dripping while continuing to stir, the stirring speed is 200r / min, the reaction temperature is controlled at 60°C-65°C during the dropwise addition, and the reaction is kept at 60°C-65°C for 2 hours after the dropwise addition. The crude product obtained after the reaction was rinsed with distilled water in a pear-shaped separatory funnel, the mass ratio of the crude product to distilled water was 1:6, and separated after static layering to obtain a product with a purity of 99.5% and a yield of 92.4%.

Embodiment 2

[0042] Hexamethyldisilazane and phosphoric acid are fed and reacted at a molar ratio of 1:1.5, the purity of phosphoric acid is 70%, and hexamethyldisilazane is added dropwise to the reaction kettle containing phosphoric acid at a rate of 0.8g / min , dripping while continuing to stir, the stirring speed is 300r / min, the reaction temperature is controlled at 60°C-65°C during the dropwise addition, and the reaction is kept at 60°C-65°C for 3h after the dropwise addition is completed. The crude product obtained after the reaction was rinsed in a pear-shaped separatory funnel with ultrapure water, the mass ratio of the crude product to distilled water was 1:8, and separated after static layering to obtain a product with a purity of 99.6% and a yield of 92.8%.

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Abstract

The invention discloses a preparation method of trimethylsilanol. The preparation method includes the following steps of: S1, adding hexamethyldisilazane and phosphoric acid into a reaction kettle while stirring, wherein the molar ratio of the hexamethyldisilazane to the phosphoric acid is 1:(1 to 3); S2, after a period of heat-insulated reaction, performing stirring and rinsing by a solvent; S3,after standing and layering, performing separation to obtain the trimethylsilanol. The preparation method has the advantages that the method is used for preparing the trimethylsilanol, the process issimple in the production process, the process of a rectification stage is omitted in the washing procedure, the energy consumption is reduced, and the problem that the solvent is difficult to completely separate in the system is solved, so that the purity of a washed product can reach 99.6%, and the yield thereof can reach 92.8%; the subsequent separation is simple, reaction by-products, namely phosphoric acid aqueous solutions in which salt is dissolved, are few and can be recycled and reused, and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of trimethylsilanol. Background technique [0002] Trimethylsilanol, also known as trimethylhydroxysilane, has a boiling point of 100°C, a relative density of 0.8112, and a refractive index of 1.3880. The hydroxyl group in the Si-OH bond is unstable. It can be condensed and dehydrated under the action of acid or alkali, or under heat. This produces hexamethyldisiloxane. Compared with the corresponding carbon alcohol, trimethylsilanol has stronger acidity, can react with lithium aluminum tetrahydrogen, Si-OH bond can be reduced to Si-H bond, and can be used as a sealant for linear polysiloxane. Terminal agent, with hydrophobicity, is the most important intermediate for the preparation of organosilicon alkoxide and various polysiloxane products, including silicone oil, silicone rubber and silicone resin, etc. It has a wide range of uses, huge econom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
CPCC07F7/0836
Inventor 王昆李胜杰邹泓肖俊平
Owner 湖北新蓝天新材料股份有限公司
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