Method for purifying ethylenediamine

A purification method, ethylenediamine technology, applied in amino compound purification/separation, organic chemistry, etc., can solve the problems of low color stability of products, inability to effectively remove carbadiene components, etc., and achieve high color stability Effect

Active Publication Date: 2013-11-27
山西玉龙格兰特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] This hydrotreating purification method can reduce the content of carbadiene components, but in hydrotreating, new aldehydes and enamine carbadiene components will be produced along with dehydrogenation or deamination reactions, which cannot effectively remove carbon Diene components, and the problem of low color stability of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Mix 135ppm of acetaldehyde, 68ppm of ethylene amine, crude ethylenediamine with a purity of 98.6% and ammonia at a molar ratio of 1:30, heat and vaporize, and pass through a hydrogen-type hydrogen-filled solution with a pore size of 0.5nm to 0.7nm. Mordenite adsorbent bed, the temperature is 140°C, the pressure is 0.3MPa, and the liquid space velocity of ethylenediamine is 3 hours -1 , the gas after adsorption is processed through condensation, deamination, distillation and other treatment steps to obtain pure ethylenediamine. The content of each component is determined by gas chromatography, and the purity of ethylenediamine is 99.9%, and no acetaldehyde and ethyleneamine impurities are detected.

[0018] The ethylenediamine pure product obtained is measured color stability according to "acid neutralization test method", and its color number is 19 Hazen units. 27 Hazen units.

Embodiment 2

[0020] Mix the crude product of ethylenediamine containing 195ppm of acetaldehyde and 96ppm of ethyleneamine with a purity of 97.3% and ammonia at a molar ratio of 1:50. Mordenite adsorbent bed, the temperature is 120°C, the pressure is 0.4MPa, and the liquid space velocity of ethylenediamine is 6 hours -1 , the gas after adsorption is processed through condensation, deamination, distillation and other treatment steps to obtain pure ethylenediamine. The content of each component is determined by gas chromatography, and the purity of ethylenediamine is 99.8%, and no acetaldehyde and ethyleneamine impurities are detected.

[0021] The ethylenediamine pure product obtained is measured color stability according to "acid neutralization test method", and its color number is 29 Hazen units. 34 Hazen units.

Embodiment 3

[0023] The operation process is basically the same as in Example 1, except that the crude product of ethylenediamine has a purity of 98.5%, contains 281ppm of acetaldehyde and 173ppm of ethyleneamine, the temperature of the adsorption bed is 150°C, and the pressure is 0.5MPa. Liquid space velocity is 10 hours -1 , The molar ratio of crude ethylenediamine to ammonia is 1:20. The content of each component was determined by gas chromatography, and the purity of ethylenediamine was 99.4%, containing 31ppm of acetaldehyde and 17ppm of ethyleneamine.

[0024] Measure the color stability of the obtained ethylenediamine pure product according to the "acid neutralization test method", there is no obvious yellowing, and its color number is 34 Hazen units. Its color number was determined to be 39 Hazen units.

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Abstract

The invention discloses a method for purifying ethylene dimine, which is to solve a problem of ethylene dimine of low color stability. The invention mixes ethylene dimine containing carbon dienes impurity and ammonia according to molar ratio of 1:20-50; then at the temperature of 120-200 DEG C, pressure of 0.1-0.5MPa, airspeed of ethylene dimine 1-10 hours<-1>, an absorbent bed is led in; ethylene dimine sterling is obtained after processing procedures of condensation, deaminase, distillation and the like are carried out on absorbed gas; the absorbent is H-mordenite with aperture of 0.5-0.7nm. The method for purifying ethylene dimine is mainly applied to purification of ethylene dimine.

Description

technical field [0001] The invention relates to a method for purifying ethylenediamine. technical background [0002] Generally, the methods for industrially producing ethylenediamine mainly include the dichloroethane method and the ethanolamine method, and the ethanolamine method has developed into a preferred method for producing ethylenediamine. The ethanolamine method uses ethanolamine and ammonia as raw materials to react in the presence of an amination catalyst to obtain an aminated product containing ethylenediamine, and then deaminates and dehydrates the aminated product, obtains a crude product of ethylenediamine through distillation, and further refines it. The pure product was obtained by distillation. [0003] US7271292 records that there are dehydroxylation and deamination reactions in the ethanolamine method to form carbodiene components such as vinylamine and acetaldehyde. These carbadiene components are the main factors that affect the discoloration of ethyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/10C07C209/86
Inventor 吕剑杨建明赵锋伟谷玉杰寇联岗
Owner 山西玉龙格兰特化工有限公司
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