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Method for synthesizing diethylene glycol ethyl ether acrylate

A technology of diethylene glycol ethyl ether and methacrylate, which is applied in the field of fine chemicals, can solve the problems of backward production technology and low output, and achieve the effects of low environmental pollution, high catalytic activity and mild reaction conditions

Inactive Publication Date: 2019-01-11
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For a long time, methacrylates have been a chemical product that has been in short supply in China. Although there is a small batch of domestic production, the production process is backward and the output is low. So far, it still cannot meet the needs of the domestic market and mainly relies on imports.

Method used

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  • Method for synthesizing diethylene glycol ethyl ether acrylate
  • Method for synthesizing diethylene glycol ethyl ether acrylate
  • Method for synthesizing diethylene glycol ethyl ether acrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 111.9g methacrylic acid, 134.17g diethylene glycol ether, 12.3g catalyst S 2 o 8 2- / ZrO 2 -SiO 2 , 36.9g toluene, and 1.23g phenothiazine were added to a four-necked flask, the vacuum degree was -0.04~-0.045MPa, the temperature was raised to reaction reflux, and the temperature was continuously raised to 140°C, and the water in the water separator was separated in time, and the reaction raw materials The molar ratio is methacrylic acid: diethylene glycol ether = 1.3:1; the amount of catalyst is 5% of the total mass of raw materials; the amount of water-carrying agent is 15% of the total mass of raw materials; the amount of polymerization inhibitor is 5% of the total mass of raw materials , wherein the reaction temperature is 140°C. The conversion rate of diethylene glycol ethyl ether was 69.04%, and the yield of diethylene glycol ethyl ether methacrylate was 68.15%.

Embodiment 2

[0023] 111.9g methacrylic acid, 134.17g diethylene glycol ether, 12.3g catalyst S 2 o 8 2- / ZrO 2 -SiO 2 , 36.9g toluene, and 1.23g phenothiazine were added to a four-neck flask, the vacuum degree was -0.04~-0.045MPa, the temperature was raised to reaction reflux, and the temperature was continuously raised to 145°C, and the water in the water separator was separated in time, and the reaction raw materials The molar ratio is methacrylic acid: diethylene glycol ether = 1.3:1; the amount of catalyst is 5% of the total mass of raw materials; the amount of water-carrying agent is 15% of the total mass of raw materials; the amount of polymerization inhibitor is 5% of the total mass of raw materials , wherein the reaction temperature is 145°C. The conversion rate of diethylene glycol ethyl ether was 81.88%, and the yield of diethylene glycol ethyl ether methacrylate was 80.19%.

Embodiment 3

[0025] 111.9g methacrylic acid, 134.17g diethylene glycol ether, 12.3g catalyst S 2 o 8 2- / ZrO 2 -SiO 2 , 36.9g toluene, and 1.23g phenothiazine were added to a four-neck flask, the vacuum degree was -0.04~-0.045MPa, the temperature was raised to reaction reflux, and the temperature was continuously raised to 150°C, and the water in the water separator was separated in time, and the reaction raw materials The molar ratio is methacrylic acid: diethylene glycol ether = 1.3:1; the amount of catalyst is 5% of the total mass of raw materials; the amount of water-carrying agent is 15% of the total mass of raw materials; the amount of polymerization inhibitor is 5% of the total mass of raw materials , wherein the reaction temperature is 150°C. The conversion rate of diethylene glycol ether was 90.57%, and the yield of diethylene glycol ether methacrylate was 86.62%.

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Abstract

The invention relates to a method for synthesizing diethylene glycol ethyl ether acrylate. The method takes methacrylic acid and diethylene glycol monoethyl ether as raw materials; diethylene glycol ethyl ether acrylate is subjected to synthesis by direct esterification under existence of a catalyst, a water-carrying agent, and a polymerization inhibitor. The method adopts a S2O8<2-> / ZrO2-SiO2 solid acid catalyst, phenothiazine is used as the polymerization inhibitor, the conversion rate of diethylene glycol monoethyl ether is 99.58%, and the yield of diethylene glycol ethyl ether acrylate is93.81%. The method has the advantages that the method adopts the S2O8<2-> / ZrO2-SiO2 solid acid catalyst for a catalysis reaction, the catalyst has high catalytic activity and is easy to be separated from the product and can be reused, the problems that the traditional esterification reaction is demanding on the equipment, the product separation is difficult, and the pollution problem is serious can be avoided. The method has great significance to promote industrial energy conservation, environmental protection and sustainable development.

Description

technical field [0001] The present invention relates to the synthesis of diethylene glycol ethyl ether methacrylate, specifically methacrylic acid and diethylene glycol ethyl ether are raw materials, toluene is a water-carrying agent, and phenothiazine is a polymerization inhibitor. 2 o 8 2- / ZrO 2 -SiO 2 Under the action of diethylene glycol ethyl ether methacrylate was synthesized. It belongs to the technical field of fine chemicals. Background technique [0002] The research and application of methacrylate photocuring monomer is relatively rapid, and it has become an important member in the field of polymer materials and coatings. The chemical structure of methacrylate photocurable monomers contains functional groups such as unsaturated carbon-carbon double bonds, ether bonds, and carbonyl groups. It has multifunctional characteristics such as copolymerization and miscibility, and has fast curing speed, low irritation, and strong dilution. It is widely used in the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54B01J27/02B01J37/03B01J37/08B01J37/02
CPCB01J27/02B01J37/0201B01J37/031B01J37/082C07C67/08C07C69/54Y02P20/584
Inventor 郭登峰钱婷婷刘准章泽洲张皓文黄飞龙李瑞萍
Owner CHANGZHOU UNIV
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