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A kind of method of one-step catalytic synthesis ethylene glycol ethyl ether acetate

A technology of ethylene glycol ethyl ether acetate and ethyl acetate, which is applied in the field of fine chemicals, can solve the problems of complex process, difficult product treatment, easy environmental pollution, etc., achieve high reactivity, avoid difficult product treatment, and protect the environment The effect of little pollution

Active Publication Date: 2015-10-14
吉林怡达化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of method of synthesizing ethylene glycol ethyl ether acetate in one step, and this method avoids complex process in traditional two-step reaction, easy environmental pollution, the problems such as difficult product treatment, technique is simple, energy consumption is low, And the catalyst is easy to separate, reusable, energy saving and environmental protection

Method used

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  • A kind of method of one-step catalytic synthesis ethylene glycol ethyl ether acetate
  • A kind of method of one-step catalytic synthesis ethylene glycol ethyl ether acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 176.2g ethyl acetate and 3.3g catalyst (magnesium aluminum zirconium salt cation molar ratio is Mg:Al:Zr=1:1:0.06) into a reaction kettle with a volume of 2L, and stir in a closed state with N 2 Replace the air in the kettle, heat up, and when the temperature reaches 120°C, continue to feed 44.0g of ethylene oxide into the reactor, the pressure in the reactor is 0.30~0.50MPa, and the reaction temperature is constant at 120°C. The molar ratio of the reaction raw materials is ethyl acetate: ethylene oxide = 2:1. The conversion rate of ethylene oxide was 76.99%, the yield of ethylene glycol ether acetate was 28.80%, and the yield of diethylene glycol ether acetate was 24.63%.

Embodiment 2

[0022] Add 211.4g ethyl acetate and 3.6g catalyst (magnesium aluminum zirconium salt cation molar ratio is Mg:Al:Zr=1:1:0.06) into a reaction kettle with a volume of 2L, close the stirring, and use N 2 Replace the air in the kettle, heat up, and when the temperature reaches 120°C, continue to feed 26.4g of ethylene oxide into the reactor, the pressure in the reactor is 0.30~0.50MPa, and the reaction temperature is constant at 120°C. The molar ratio of the reaction raw materials is ethyl acetate: ethylene oxide = 4:1. The conversion rate of ethylene oxide was 81.13%, the yield of ethylene glycol ether acetate was 41.37%, and the yield of diethylene glycol ether acetate was 25.16%.

Embodiment 3

[0024] Add 220.3g ethyl acetate and 3.7g catalyst (magnesium aluminum zirconium salt cation molar ratio is Mg:Al:Zr=1:1:0.06) into a reaction kettle with a volume of 2L, close the stirring, and use N 2 Replace the air in the kettle, heat up, and when the temperature reaches 120°C, continuously feed 22.0g of ethylene oxide into the reactor, the pressure inside the reactor is 0.30~0.50MPa, and the reaction temperature is constant at 120°C. The molar ratio of the reaction raw materials is ethyl acetate: ethylene oxide = 5:1. The conversion rate of ethylene oxide was 74.05%, the yield of ethylene glycol ether acetate was 41.74%, and the yield of diethylene glycol ether acetate was 21.26%.

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Abstract

The invention relates to a method for one-step catalytic synthesis of ethylene glycol ethyl ether acetate. The method comprises the steps of stirring ethyl acetate and oxirane as raw materials and magnesium-aluminum-zirconium composite oxide as a solid catalyst in a reaction kettle in a closed manner, replacing air in the kettle with N2, heating to a set temperature, performing ring opening on oxirane and embedding oxirane into ester bond of ethyl acetate, and reacting to synthesize ethylene glycol ethyl ether acetate, wherein the reaction process conditions are as follows: the molar ratio of ethyl acetate to oxirane is (1-9) : 1, the reaction temperature is 80-160 DEG C, and the mass percent of the catalyst accounts for 0.1%-5% the total mass; magnesium-aluminum-zirconium composite oxide is prepared by adopting a coprecipitation method through ageing, drying and high-temperature roasting. The method has the advantages that ethylene glycol ethyl ether acetate can be obtained in one step, the problems of high requirements for equipment caused by a conventional esterification reaction and relative difficulty in treatment of ethylene glycol ethyl ether acetate are solved, the catalyst is easy to separate and is recyclable, and the effects of energy conservation and environmental protection are achieved.

Description

technical field [0001] The invention relates to the synthesis of ethylene glycol ethyl ether acetate, specifically, ethyl acetate and ethylene oxide are used as raw materials, and under the action of a solid catalyst magnesium-aluminum-zirconium composite oxide, ethylene oxide ring-opens and embeds ethyl acetate in one step The reaction synthesizes ethylene glycol ethyl ether acetate. It belongs to the technical field of fine chemicals. Background technique [0002] The molecular structure of ethylene glycol ethyl ether acetate contains alkyl groups, ether bonds, and carbonyl groups. It has good solubility and excellent performance that ordinary solvents do not have. [0003] The raw materials based on ethylene oxide and propylene oxide are an important method for producing polyoxyalkylene fine chemicals. Glycol ether solvents are one of the important derivatives of epoxy compounds and have a wide range of industrial applications. Applications. Glycol ether ester compound...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/16C07C67/26
CPCC07C67/29C07C69/16Y02P20/10
Inventor 郭登峰赵会晶刘准曹惠庆朱煜张静
Owner 吉林怡达化工有限公司
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