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Preparation method of hexamethyl disiloxane

A technology of hexamethyldisiloxane and trimethylmonochlorosilane, which is applied in the field of preparation of hexamethyldisiloxane, can solve problems such as low production efficiency, difficult product separation, and low product yield, and achieve The effect of low production cost, simple process operation and high product yield

Inactive Publication Date: 2009-02-11
JIANGSU HONGDA NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, hexamethyldisiloxane is mainly produced by hydrolysis method, that is, trimethylmonochlorosilane is hydrolyzed under acidic conditions to generate hexamethyldisiloxane and dilute hydrochloric acid. This method has low production efficiency and low product quality. The yield is low and the quality is poor. At the same time, the acid concentration generated in the production process is low and contains a small amount of organic waste water. Therefore, it is difficult to separate the products and cause serious environmental pollution, which limits the further development of production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] raw material

[0026] Trimethylchlorosilane mass ratio 100 parts, weight 217g,

[0027] Sodium carbonate mass ratio 50 parts, weight 106g,

[0028] Hexamethyldisiloxane mass ratio 20 parts, weight 43.4g.

[0029] First add the measured 43g of hexamethyldisiloxane and 106g of sodium carbonate into the reactor, start stirring, and at the same time, drop the measured 217g of trimethylmonochlorosilane into the reactor, and the reaction temperature is normal temperature. Adjust and control the addition rate according to the change of reaction temperature. There will be gas released during the reaction. When the dropwise addition is completed and continue to stir until no gas is produced, stop stirring and test the pH value of the material. When the pH value is 6.0-8.0, the reaction is complete and the reaction is stopped. ; cooling, centrifugal filtration (solid-liquid separation), centrifugal speed 1200 rpm, the resulting liquid is the hexamethyldisiloxane finished produc...

Embodiment 2

[0032] raw material

[0033] Trimethylchlorosilane mass ratio 100 parts, weight 217g,

[0034] Potassium carbonate mass ratio 100 parts, weight 217g,

[0035] Hexamethyldisiloxane mass ratio 200 parts, weight 434g.

[0036] Centrifugal filtration Centrifugal speed 1200 rpm,

[0037] Drying and drying Control the temperature at 150°C.

[0038] When producing, first add the metered 434g hexamethyldisiloxane and 217g potassium carbonate to the reactor, start stirring, and simultaneously drop the metered 217g trimethylmonochlorosilane into the reactor, The reaction temperature is normal temperature, adjust and control the addition rate according to the reaction temperature change, there will be gas released during the reaction, when the dropwise addition is completed, continue to stir until no gas is produced, stop stirring and test the pH value of the material, when the pH value is 6.0-8.0, it is The reaction is complete; stop the reaction, then centrifuge and filter, and the...

Embodiment 3

[0041] raw material

[0042] Trimethylchlorosilane mass ratio 100 parts, weight 217g,

[0043] Potassium carbonate mass ratio 75 parts, weight 162.8g,

[0044] Hexamethyldisiloxane mass ratio 100 parts, weight 217g.

[0045] Centrifugal filtration Centrifugal speed 1200 rpm,

[0046] Drying and drying Control the temperature at 150°C.

[0047] When in production, first add the measured 217g of hexamethyldisiloxane and 162.8g of potassium carbonate into the reactor, start stirring, and at the same time, drop the measured 217g of trimethyl-chlorosilane into the reactor , the reaction temperature is normal temperature, adjust and control the addition rate according to the change of the reaction temperature, there will be gas released during the reaction, when the dropwise addition is completed, continue to stir until no gas is produced, stop stirring and test the pH value of the material, when the pH value is 6.0-8.0 The reaction is complete; stop the reaction, then centrifug...

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Abstract

The invention relates to the field of organic chemistry, in particular to a preparation method for hexamethyldisiloxane, which is characterized in that: non-toxic and harmless carbonate is taken as a solid state reactant, trimethyl chloro silicane is taken as a liquid state reactant and hexamethyldisiloxane is taken as a reaction solvent; and the hexamethyldisiloxane is synthesized by liquid-solid reaction. The preparation method is simple and can react under mild conditions that only require normal temperature and normal pressure; reaction products can be obtained by simple solid-liquid separation.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a preparation method of hexamethyldisiloxane. Background technique [0002] Hexamethyldisiloxane is mainly used in the production of organic chemical industry and pharmaceutical chemical industry. At present, hexamethyldisiloxane is mainly produced by hydrolysis method, that is, trimethylmonochlorosilane is hydrolyzed under acidic conditions to generate hexamethyldisiloxane and dilute hydrochloric acid. This method has low production efficiency and low product quality. The yield is low, the quality is poor, and the acid concentration produced during the production process is low and contains a small amount of organic waste water, so the product separation is relatively difficult, and the environmental pollution is also relatively serious, thus limiting the further development of production. Contents of the invention [0003] The invention discloses a new preparation method of ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 祝纪才朱德洪朱恩俊
Owner JIANGSU HONGDA NEW MATERIAL
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