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Method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by continuous catalysis of solid phase catalyst

A technology for heptamethyltrisiloxane and hexamethyldisiloxane, which is used in the continuous catalytic synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane using a solid-phase catalyst It can solve the problems of long reaction time, low yield and difficult separation, and achieve the effects of long reaction time, efficient and stable reaction, and simple process

Active Publication Date: 2012-10-10
JIANGXI HITO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods have problems such as long reaction time or difficult separation, chlorine-containing raw materials pollute the environment, and the yield is not too high

Method used

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  • Method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by continuous catalysis of solid phase catalyst
  • Method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by continuous catalysis of solid phase catalyst
  • Method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by continuous catalysis of solid phase catalyst

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Effect test

Embodiment 1

[0025] Example 1. A method for continuously catalyzing and synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by using a solid phase catalyst, in which: hexamethyldisiloxane and linear The raw materials of methyl hydrogen polysiloxane are continuously added to the fixed bed reactor with constant temperature jacket and strong acid type ion exchange resin at a molar ratio of 2.5:1 and a flow rate of 50mL / h. The reaction temperature is constant 60℃, catalyzed and balanced by the solid phase catalyst of the macroporous strong acid styrene-based cation exchange resin, the residence time is 6h, the reaction is continuous in the reactor, and the flow rate of the reaction product is controlled to flow directly from the fixed reactor, and the product from the reactor is used Gas chromatograph for quantitative analysis, the gas chromatogram is as figure 1 As shown, the content of MDHM is 32.3%. After high-reduction and low-reduction rectification, the fractions in the range of 141-2℃ are...

Embodiment 2

[0028] Example 2. A method for continuously catalyzing the synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane using a solid-phase catalyst, wherein: hexamethyldisiloxane and linear methyl The molar ratio of the base hydrogen polysiloxane (MDHnM) raw materials is 3:1, the rest is the same as in Example 1, and the content of MDHM is 29.2%.

Embodiment 3

[0029] Example 3. A method for continuously catalyzing the synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane using a solid phase catalyst, wherein: hexamethyldisiloxane and linear methyl The molar ratio of the base hydrogen polysiloxane (MDHnM) raw materials is 2:1, the rest is the same as in Example 1, and the content of MDHM is 30.1%.

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Abstract

The invention relates to a method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by continuous catalysis of a solid phase catalyst. Hexamethyldisiloxane and straight chain methyl hydrogen polysiloxane in a molar ratio of 3:1-2:1 are taken as raw materials, strongly acidic ion exchange resin is taken as the solid phase catalyst, the reaction temperature is 40 to 80 DEG C, a fixed bed reactor is adopted, the raw materials pass through the reactor filled with the ion exchange resin at a certain flow rate, the retention period is 5 to 10 hours, the conversion rate of the raw materials is ensured by the retention period of the reaction through controlling the flow rate of the reaction product, the continuous reaction production is realized, and the reaction product is subjected to low fraction and high fraction removal rectification to form the 1,1,1,3,5,5,5-heptamethyltrisiloxane product with the purity of over 99 percent. The method has the advantages of readily available raw materials, no three-waste emission, simple process, continuous production, high-efficiency and stable reaction, simple separation, recyclable catalyst, conversion per pass of the raw material straight chain methyl hydrogen polysiloxane of over 32 percent, good product quality and low production cost.

Description

Technical field [0001] The invention relates to a method and process for continuously catalyzing and synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by using a solid phase catalyst. Background technique [0002] 1,1,1,3,5,5,5-Heptamethyltrisiloxane (MDHM) is an important organosilicon intermediate. Because it contains active silicon-hydrogen bonds, it is used to synthesize polyether and alkyl Modified trisiloxane is the basic raw material and can be widely used in pesticide additives, coating additives and daily chemicals, etc. However, the existing synthetic processes generally have disadvantages such as low yield and complex by-products. Therefore, The improvement of the synthesis process of MDHM and the increase of yield are of great significance. [0003] Patent GB0632954 mentions the use of hexamethyldisiloxane (MM) and methylhydrodichlorosilane (MeSiHC12) hydrolysate through concentrated sulfuric acid for catalytic equilibrium of MDHM method, and the trimethylchlorosilane ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08
CPCY02P20/584
Inventor 廖洪流彭任远卢荣美肖书琴
Owner JIANGXI HITO CHEM
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