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Method for synthesizing ethylene glycol diacetate by adopting transesterification method

A technology of ethylene glycol di-acetate, applied in the field of organic compound synthesis, can solve the problems of untimely removal, long reaction time, low reaction conversion rate, etc., and achieve mild reaction conditions, no environmental pollution, and high conversion rate Effect

Inactive Publication Date: 2015-02-18
天津中昊天久工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method does not remove the sec-butanol generated by the system in time during the preliminary transesterification process, so that the reaction conversion rate is low and the reaction time is long; in breaking the chemical equilibrium stage of transesterification, it is necessary to detect the distillate in batches. The amount of s-butyl acetate, and add 1-4 times the amount of s-butyl acetate distilled
This operation makes the production process complicated, and intermittently adds sec-butyl acetate, which makes the temperature of the reaction system unstable and difficult to control the production process; in the separation process of ethylene glycol monoacetate and ethylene glycol diacetate Among them, one or more of benzene, toluene or xylene is used as the extractant, and the extractant is highly toxic; in the separation and purification process of sec-butanol, the azeotropy of sec-butanol and sec-butyl acetate is not considered
Because sec-butanol and sec-butyl acetate have azeotropic phenomenon when the sec-butanol content is 86.3% (wt), so the conventional rectification can not obtain 99% sec-butanol product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A method for synthesizing ethylene glycol diacetate by transesterification, the steps are as follows:

[0018] ⑴ K 2 CO 3 , ethylene glycol and sec-butyl acetate are added to the still with a rectification tower and agitator according to the molar ratio of 0.003:1:0.5, and after heating until the temperature at the top of the tower is stable, sec-butanol and acetic acid are extracted at a reflux ratio of 5:1 The azeotrope of sec-butyl ester, while continuously adding the remaining sec-butyl acetate.

[0019] (2) The total amount of sec-butyl acetate added is 3 times of ethylene glycol (molar ratio). During the feeding process of sec-butyl acetate, the temperature of the tower kettle is kept at 120°C, and the addition speed of sec-butyl acetate passes through the temperature of the tower kettle. To control, the feed time lasted 1 hour.

[0020] (3) After the feeding is completed, continue the reaction and extraction until the temperature of the tower kettle rises to 1...

Embodiment 2

[0023] A method for synthesizing ethylene glycol diacetate by transesterification, the steps are as follows:

[0024] ⑴ CH 3 ONa, ethylene glycol and sec-butyl acetate are added to the distillation still with a rectification tower and agitator according to the molar ratio of 0.01:1:0.85. After heating until the temperature at the top of the tower is stable, sec-butanol and The azeotrope of sec-butyl acetate, while continuously adding the remaining sec-butyl acetate.

[0025] (2) The total amount of sec-butyl acetate added is 4 times (molar ratio) of ethylene glycol. During the feeding process of sec-butyl acetate, the temperature of the tower kettle is kept at 130°C, and the addition speed of sec-butyl acetate passes through the temperature of the tower kettle. To control, the feed time lasted 1.5 hours.

[0026] (3) After the feeding is completed, continue the reaction and extraction until the temperature of the tower kettle rises to 180°C for 3 hours. The tower kettle is e...

Embodiment 3

[0029] A method for synthesizing ethylene glycol diacetate by transesterification, the steps are as follows:

[0030] (1) Add KOH, ethylene glycol and sec-butyl acetate supported on Al2O3 to the still with rectification tower and stirrer according to the molar ratio of 0.015:1:1.2. : 1 extract the azeotrope of sec-butanol and sec-butyl acetate, while continuously adding the remaining sec-butyl acetate.

[0031] (2) The total amount of sec-butyl acetate added is 5 times (molar ratio) of ethylene glycol. During the feeding process of sec-butyl acetate, the temperature of the tower kettle is kept at 140°C, and the addition speed of sec-butyl acetate passes through the temperature of the tower kettle. To control, the feed time lasted 2 hours.

[0032] (3) After the feeding is completed, continue the reaction and extraction until the temperature of the tower kettle rises to 180°C for 4 hours. The tower kettle is ethylene glycol diacetate, ethylene glycol monoacetate and incomplete...

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Abstract

The invention relates to a method for synthesizing ethylene glycol diacetate by adopting a reactive distillation technology. Sec-butyl acetate and ethylene glycol are used as raw materials, ethylene glycol diacetate is produced by transesterification on the presence of a basic catalyst, and a byproduct is ethylene glycol monoethyl acetate. According to the method, the yield of the ethylene glycol diacetate can reach over 90 percent, and the method has the advantages of high conversion rate, mild reaction conditions, high yield, no corrosion, no environmental pollution and the like.

Description

technical field [0001] The invention belongs to the field of organic compound synthesis, in particular to a method for synthesizing ethylene glycol diacetate by transesterification. Background technique [0002] Ethylene glycol diacetate (EGDA), also known as ethylene glycol diacetate, is a colorless liquid with a boiling point of 190.2°C. It is an efficient, safe, non-toxic and environmentally friendly organic solvent. Widely used in the pharmaceutical industry; organic ester curing agent for casting resins; also used as an excellent solvent for various organic resins, especially nitrocellulose, and raw materials for leather brighteners; used as nitro spray paint, printing ink, cellulose ester in paints and coatings , Fluorescent paint solvent. [0003] The traditional methods for the synthesis of ethylene glycol diacetate include acetate esterification, catalytic addition of ethylene oxide and acetic acid, and direct esterification of ethylene glycol and acetic acid. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/16C07C67/03
CPCC07C67/03C07C69/16Y02P20/10
Inventor 简春贵张雪梅
Owner 天津中昊天久工程技术有限公司
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