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Separation method of ethylenediamine and water azeotrope

A separation method, the technology of ethylenediamine, applied in the purification/separation of amino compounds, organic chemistry, etc., can solve the problems of high energy consumption and impact on application, and achieve the effect of low energy consumption and high-efficiency separation

Active Publication Date: 2014-01-29
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two separation methods will introduce a third substance, which will cause unwanted impurities in the product and affect the application in high-end fields such as ethylenediamine medicine; in addition, extractive distillation and azeotropic distillation usually adopt a double-tower process, and energy consumption larger

Method used

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  • Separation method of ethylenediamine and water azeotrope

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The mixture whose mass percentage content is 70% of ethylenediamine and 30% of water is fed from the middle part of rectifying tower A under the condition of temperature of 80 ℃. is 2, the top temperature of the tower is 100 °C, the top of the A tower is water, and the purity is 99.9%; the temperature of the tower A of the rectification tower is 120 °C, and the tower still is an azeotrope of ethylenediamine and water.

[0025] The temperature of the azeotrope of ethylenediamine and water drops to 60 °C, and enters the pervaporation device B. The feed liquid side is operated at a pressure of 100 kPa. The operating temperature of the feed liquid is measured at 60 °C, and the pressure after the membrane is 0.5 kPa. After the permeate is condensed, it returns to In the rectifying tower A, the retentate is ethylenediamine product with a purity of 99.9%.

Embodiment 2

[0027] The mass percentage content is that the mixture of ethylenediamine 75% and water 25% is fed from the middle of rectifying tower A under the condition of temperature of 90 ℃. is 3, the tower top temperature is 105 ℃, the A tower top is water, and the purity is 99.9%; the A tower still temperature of the rectification tower is 125 ℃, and the tower still is the azeotrope of ethylenediamine and water.

[0028] The temperature of the azeotrope of ethylenediamine and water drops to 60 °C, and enters the pervaporation device B. The feed liquid side is operated at a pressure of 120 kPa. The operating temperature of the feed liquid is measured at 60 °C, and the pressure behind the membrane is 1 kPa. In distillation column A, the retentate is an ethylenediamine product with a purity of 99.6%.

Embodiment 3

[0030] The mixture whose mass percentage content is 80% of ethylenediamine and 20% of water is fed from the middle of rectifying tower A under the condition of temperature of 95 ℃. For 5, A tower top, the tower top is water, the temperature is 120 ℃, the purity is 99.9%; the temperature of the distillation tower A tower still is 140 ℃, and the tower still is the azeotrope of ethylenediamine and water.

[0031] The temperature of the azeotrope of ethylenediamine and water drops to 60 °C, and enters the pervaporation device B. The feed liquid side is operated at a pressure of 200 kPa. The operating temperature of the feed liquid is measured at 70 °C, and the pressure after the membrane is 2 kPa. In distillation column A, the retentate is an ethylenediamine product with a purity of 99.8%.

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Abstract

The invention discloses a separation method of ethylenediamine and water azeotrope. The separation method is mainly used for solving the problems that the third impurity can be introduced through extractive distillation and azeotropic distillation and the separation energy consumption is high. A rectifying tower and a pervaporation device are adopted in the separation method. The separation method disclosed by the invention specifically comprises the following steps that (1), ethylenediamine and water mixture enter into the rectifying tower to be separated, wherein the operation pressure is 100-200 kPa, the temperature of the tower top is 100-120 DEG C, the temperature of the tower bottom is 120-142 DEG C, the reflux ratio is 0.5-10, the tower top fraction is pure water, and the tower bottom fraction is highest azeotrope of ethylenediamine and water; (2), the tower bottom fraction of the rectifying tower enters into the pervaporation device to be separated, wherein the operation pressure at the feed liquid side is 100-2000 kPa, the operation temperature at the feed liquid side is 40-100 DEG C, the pressure of the membrane back is 0.5-2 kPa; water at the feed liquid side preferentially enters the membrane back through the membrane, permeable substances are circulated into the rectifying tower through condensation, and the retentate is ethylenediamine. According to the method disclosed by the invention, the third substance is unnecessary to introduce; furthermore, compared with extractive distillation and azeotropic distillation, the separation method has the advantages that the energy consumption is low and the separation cost of the ethylenediamine is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a separation method of ethylenediamine and water azeotrope. Background technique [0002] Ethylenediamine is a widely used basic organic chemical raw material, mainly used in epoxy resin curing agent, pesticide, medicine, chelating agent, etc. In the production process of ethanolamine hydroreductive amination or condensation amination to prepare ethylenediamine, water is generated in the product. Because the boiling points of water (boiling point is 100°C) and ethylenediamine (boiling point is 117.15°C) are very close, they form the highest azeotrope, and it is difficult to separate the two by conventional rectification. [0003] Industrially, extractive distillation and azeotropic distillation are generally adopted, such as: CN200910250469.X discloses a method for purifying ethylene diamine and water azeotrope, and the method utilizes an extractant to dest...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/10C07C209/86
Inventor 袁俊吕剑杨建明张伟赵锋伟王博余秦伟王伟王为强梅苏宁李亚妮张前
Owner XIAN MODERN CHEM RES INST
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