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1,1,1,3,3,5,5-heptamethyltrisiloxane preparation method

A technology of heptamethyltrisiloxane and pentamethyldisiloxane, which is applied in the field of preparing 1,1,1,3,3,5,5-heptamethyltrisiloxane, and can solve by-products Many, troublesome separation, high cost and other problems, to achieve the effect of less by-product content, convenient separation and low production cost

Inactive Publication Date: 2016-03-09
上海楚青新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing synthesis process is generally 1,1,1,3,3,3-hexamethyldisiloxane, 1,1,3,3-tetramethyldisiloxane and dimethyldimethoxy Silane co-hydrolysis, this method produces more by-products, and the separation is more troublesome, which increases the cost of production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 11

[0015] The preparation method of embodiment 11,1,1,3,3,5,5-heptamethyltrisiloxane, the method comprises the following operations:

[0016] First mix 1,1,1,3,3,3-hexamethyldisiloxane and 1,1,3,3-tetramethyldisiloxane at a molar ratio of 1:1, add concentrated sulfuric acid Co-hydrolyzed for 1h to obtain 1,1,1,3,3-pentamethyldisiloxane, and then 1,1,1,3,3-pentamethyldisiloxane and dimethyldimethoxy The base silane is mixed at a molar ratio of 1:1, and concentrated sulfuric acid is added for co-hydrolysis for 1 to 3 hours. After rectification, the fraction at 135°C is collected to obtain 1,1,1,3,3,5,5-heptamethyltrisilane Oxygen products.

Embodiment 21

[0017] Embodiment 21, the preparation method of 1,1,3,3,5,5-heptamethyltrisiloxane, the method comprises the following operations:

[0018] First mix 1,1,1,3,3,3-hexamethyldisiloxane and 1,1,3,3-tetramethyldisiloxane at a molar ratio of 1:3, add concentrated sulfuric acid Co-hydrolyzed for 2h to obtain 1,1,1,3,3-pentamethyldisiloxane, and then 1,1,1,3,3-pentamethyldisiloxane and dimethyldimethoxy The base silane is mixed at a molar ratio of 1:1.5, and concentrated sulfuric acid is added for co-hydrolysis for 1 to 3 hours. After rectification, the fraction at 135°C is collected to obtain 1,1,1,3,3,5,5-heptamethyltrisilane Oxygen products.

Embodiment 31

[0019] Embodiment 31, the preparation method of 1,1,3,3,5,5-heptamethyltrisiloxane, the method comprises the following operations:

[0020] First mix 1,1,1,3,3,3-hexamethyldisiloxane and 1,1,3,3-tetramethyldisiloxane at a molar ratio of 1:5, add concentrated sulfuric acid Co-hydrolyzed for 3h to obtain 1,1,1,3,3-pentamethyldisiloxane, and then 1,1,1,3,3-pentamethyldisiloxane and dimethyldimethoxy The base silane is mixed at a molar ratio of 1:2, and concentrated sulfuric acid is added for co-hydrolysis for 1 to 3 hours. After rectification, the fraction at 135°C is collected to obtain 1,1,1,3,3,5,5-heptamethyltrisilane Oxygen products.

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PUM

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Abstract

The present invention discloses a 1,1,1,3,3,5,5-heptamethyltrisiloxane preparation method, wherein 1,1,1,3,3,3-hexamethyldisiloxane and 1,1,3,3-tetramethyldisiloxane are subjected to co-hydrolysis for 1-4 h under catalysis of concentrated sulfuric acid to obtain 1,1,1,3,3-pentamethyldisiloxane, the 1,1,1,3,3-pentamethyldisiloxane and dimethyl dimethoxy silicane are subjected to co-hydrolysis for 1-3 h under catalysis of concentrated sulfuric acid, rectification is performed, and the distillate at a temperature of 135 DEG C is collected so as to obtain the 1,1,1,3,3,5,5-heptamethyltrisiloxane product. According to the present invention, the method has characteristics of strong target property, less by-product content in the product, and easy separation.

Description

technical field [0001] The invention belongs to the technical field of organosilicon, in particular to a method for preparing 1,1,1,3,3,5,5-heptamethyltrisiloxane. Background technique [0002] 1,1,1,3,3,5,5-heptamethyltrisiloxane is an important organosilicon intermediate, mainly used to pass through terminal allyl polyether due to its active silicon-hydrogen bond Synthesis of Si-C type trisiloxane hyperdispersant by hydrosilylation reaction. The existing synthesis process is generally 1,1,1,3,3,3-hexamethyldisiloxane, 1,1,3,3-tetramethyldisiloxane and dimethyldimethoxy Silane co-hydrolysis, this method produces more by-products, and the separation is more troublesome, which increases the production cost. Contents of the invention [0003] The object of the present invention is to provide a method for preparing 1,1,1,3,3,5,5-heptamethyltrisiloxane to solve the above-mentioned problems in the prior art. [0004] For realizing the above-mentioned purpose of the invention...

Claims

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Application Information

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IPC IPC(8): C07F7/08
Inventor 张斌
Owner 上海楚青新材料科技有限公司
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