Methods for separating the binary azeotropic mixture of ethylene glycol and ethylene glycol diacetate with sulfolane entrainer

Patent metadata

Field	Value
Publication number	US-12428367-B2
Application number	US-202519022985-A
Country	US
Kind code	B2
Filing date	Jan 15, 2025
Priority date	Jul 18, 2022
Publication date	Sep 30, 2025
Grant date	Sep 30, 2025

Abstract

Method for separating ethylene glycol (EG) and ethylene glycol diacetate (EGDA) with sulfolane entrainer, including: obtaining EG and a mixture of EGDA and sulfolane through separating a mixture of EG and EGDA under an action of sulfolane by an extractive distillation tower; obtaining EGDA and sulfolane through separating the mixture of the EGDA and the sulfolane by an entrainer recovery tower; and obtaining recycled sulfolane through cooling the sulfolane by a heat exchanger, and mixing the recycled sulfolane with fresh sulfolane and circulating into the extractive distillation tower for recycling. Through the method, a yield of the EG is greater than or equal to 99.50% and a mass purity of the EG is greater than or equal to 99.50%, and a yield of the EGDA is greater than or equal to 99.80% and a mass purity of the EGDA is greater than or equal to 99.90%.

First claim

What is claimed is:

1. A method for separating ethylene glycol and ethylene glycol diacetate using sulfolane as an entrainer, wherein a yield of the ethylene glycol is greater than or equal to 99.50% and a mass purity of the ethylene glycol is greater than or equal to 99.50%, a yield of the ethylene glycol diacetate is greater than or equal to 99.80% and a mass purity of the ethylene glycol diacetate is greater than or equal to 99.90%, and the method comprises:
(a) obtaining the ethylene glycol and a mixture of the ethylene glycol diacetate and the sulfolane through separating a mixture of the ethylene glycol and the ethylene glycol diacetate under an action of the sulfolane by an extractive distillation tower;

(b) obtaining the ethylene glycol diacetate and the sulfolane through separating the mixture of the ethylene glycol diacetate and the sulfolane by an entrainer recovery tower; and
(c) obtaining recycled sulfolane through cooling the sulfolane by a heat exchanger, mixing the recycled sulfolane with fresh sulfolane and circulating into the extractive distillation tower for recycling;
wherein a theoretical plate count of the extractive distillation tower is 18-30, an operating pressure at a top of the extractive distillation tower is 7-8 kPa, a temperature at the top of the extractive distillation tower is 120-130° C., and a temperature at a bottom of the extractive distillation tower is 160-170° C.,
a feeding position of the mixture of the ethylene glycol and the ethylene glycol diacetate is the 16th-18th theoretical plate of the extractive distillation tower, and a feeding position of the recycled sulfolane and the fresh sulfolane is the 6th-8th theoretical plate of the extractive distillation tower,
a ratio of a total mass of the recycled sulfolane and the fresh sulfolane to a mass of the mixture of the ethylene glycol and the ethylene glycol diacetate is (5-7):1;
a theoretical plate count of the entrainer recovery tower is 10-15, an operating pressure at the top of the entrainer recovery tower is 3-7 kPa, a temperature at the top of the entrainer recovery tower is 90-100° C., and a temperature at the bottom of the entrainer recovery tower is 160-175° C.,
a feeding position of the mixture of the ethylene glycol diacetate and the sulfolane is the 4th-6th plate of the entrainer recovery tower; and
a heat exchange temperature difference of the heat exchanger is 65-75° C., and an operating pressure of the heat exchanger is 15-20 kPa.

Assignees

• Univ Changzhou

Inventors

• Li Jiashu
• Li Jinlong
• Wang Fang

Classifications

• C07C29/82

  by azeotropic distillation · CPC title

• C07C67/54 Primary

  by distillation · CPC title

• Y02P20/10

  Process efficiency · CPC title

• C07C29/84 Primary

  by extractive distillation · CPC title