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A method for adsorption and purification of 1,1,1,3,5,5,5-heptamethyltrisiloxane

A technology of heptamethyltrisiloxane and adsorption resin, which is applied in the direction of silicon organic compounds, can solve the problems of large equipment investment, unfavorable industrial production, and high energy consumption, and achieve the effects of less equipment investment, increased strength, and short process

Active Publication Date: 2018-07-13
江苏科幸新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purification process used in existing patents and literature technologies all adopts distillation or evaporation process, which has high energy consumption and large investment in equipment, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1. Amination reaction

[0025] Add 100Kg of chloromethylated spheres, 80Kg of hexamethylenetetramine, and 80Kg of pure water into a 500L reactor, and react at 80°C for 12 hours. After the reaction, filter, discharge, and dry to obtain a primary amine-based resin.

[0026] Step 2. Carboxylation reaction

[0027] Add 100Kg primary amino resin, 300Kg 3-oxocyclobutane carboxylic acid, 20Kg cis-15-tetradecanemonoic acid, 0.05Kg 1-carboxyethyl-3-methylimidazolium chloride salt in 1000L reactor , 300Kg of water, reacted at 60°C for 50h to obtain an adsorption resin.

[0028] Step 3. Purification of 1,1,1,3,5,5,5-heptamethyltrisiloxane

[0029] In the 500L exchange column, add the adsorption resin product that 100Kg step 2 obtains, add crude product 1,1,1,3,5,5,5-heptamethyltrisiloxane from the top of the exchange column, flow rate 100L / h, The effluent is purified 1,1,1,3,5,5,5-heptamethyltrisiloxane. The adsorption rate is shown in Table 1.

Embodiment 2

[0031] Step 1. Amination reaction

[0032] Add 100Kg of chloromethylated spheres, 50Kg of hexamethylenetetramine, and 80Kg of pure water into a 500L reactor, and react at 80°C for 10 hours. After the reaction, filter, discharge, and dry to obtain a primary amine-based resin.

[0033] Step 2. Carboxylation reaction

[0034] Add 100Kg primary amino resin, 200Kg 3-oxocyclobutane carboxylic acid, 10Kg cis-15-tetradecanemonoic acid, 0.01Kg 1-carboxyethyl-3-methylimidazolium chloride salt in 1000L reactor , 300Kg of water, reacted at 60°C for 30h to obtain an adsorption resin.

[0035] Step 3. Purification of 1,1,1,3,5,5,5-heptamethyltrisiloxane

[0036] In the 500L exchange column, add the adsorption resin product that 100Kg step 2 obtains, add crude product 1,1,1,3,5,5,5-heptamethyltrisiloxane from the top of the exchange column, flow rate 50L / h, The effluent is purified 1,1,1,3,5,5,5-heptamethyltrisiloxane. The adsorption rate is shown in Table 1.

Embodiment 3

[0038] Step 1. Amination reaction

[0039] Add 100Kg of chloromethylated spheres, 100Kg of hexamethylenetetramine, and 80Kg of pure water into a 500L reactor, and react at 80°C for 10 hours. After the reaction, filter, discharge, and dry to obtain a primary amine-based resin.

[0040] Step 2. Carboxylation reaction

[0041] Add 100Kg primary amino resin, 400Kg3-oxocyclobutane carboxylic acid, 50Kg cis-15-tetradecanemonoic acid, 0.1Kg1-carboxyethyl-3-methylimidazolium chloride salt in 1000L reactor , 300Kg of water, reacted at 60°C for 60h to obtain an adsorption resin.

[0042] Step 3. Purification of 1,1,1,3,5,5,5-heptamethyltrisiloxane

[0043] In the 500L exchange column, add the adsorption resin product that 100Kg step 2 obtains, add crude product 1,1,1,3,5,5,5-heptamethyltrisiloxane from the top of the exchange column, flow rate 150L / h, The effluent is purified 1,1,1,3,5,5,5-heptamethyltrisiloxane. The adsorption rate is shown in Table 1.

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Abstract

The invention discloses a method for adsorbing and purifying 1, 1, 1, 3, 5, 5, 5-heptamethyltrisiloxane.The method includes preparing adsorbent resin with oxo-cyclobutane; adding the adsorbent resin into an exchange column to obtain adsorbent resin products; adding a crude product 1, 1, 1, 3, 5, 5, 5-heptamethyltrisiloxane into the exchange column from the upper side of the exchange column to obtain effluent which is the purified 1, 1, 1, 3, 5, 5, 5-heptamethyltrisiloxane.

Description

technical field [0001] The invention relates to a method for preparing organosilicon products, in particular to a method for adsorbing and purifying 1,1,1,3,5,5,5-heptamethyltrisiloxane. Background technique [0002] Trisiloxane surfactants have excellent spreadability, wettability and penetrability. In recent years, they have been widely used as agricultural adjuvants in agriculture and have very broad application prospects. With the development of trisilane surfactants With the continuous expansion of the application field of active agents, 1,1,1,3,5,5,5-heptamethyltrisiloxane is used as an intermediate for the synthesis of trisiloxane surfactants, and its synthesis and purification also appear more and more important. [0003] CN101020691 discloses the method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane, the steps are as follows: will have ME 3 The trimethylsilane of the general formula SIX is hydrolyzed with an inorganic weak base solution, and then slowly add...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/20C08F8/32C08F8/00
CPCC07F7/20C08F8/00C08F8/32C08F12/08
Inventor 张玲董建国
Owner 江苏科幸新材料有限公司