Separation method of triethylene diamine and ethanolamine azeotrope

A triethylenediamine and separation method technology, which is applied in the field of separation and purification of fine chemicals, can solve the problems of high energy consumption and large amount of entrainer used, and achieve the goal of reducing energy consumption, reducing energy consumption, and reducing the amount of use Effect

Active Publication Date: 2013-04-03
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When this patent adopts azeotropic distillation, a large amount of xylene or ethylbenzene is recycled, and there are problems of large amount of entrainer used and high energy consumption

Method used

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  • Separation method of triethylene diamine and ethanolamine azeotrope
  • Separation method of triethylene diamine and ethanolamine azeotrope
  • Separation method of triethylene diamine and ethanolamine azeotrope

Examples

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Embodiment 1

[0028] Example 1: The azeotrope and entrainer of triethylenediamine and ethanolamine enter the azeotropic rectification tower, the overhead fraction is the azeotrope of the entrainer and ethanolamine, and the bottom fraction is triethylenediamine and the entrainer mixture, the mixture is cooled and crystallized to precipitate solids, and the solid product obtained after filtration is triethylenediamine. The purity of the product is 99.8%. The entrainer is dicyclohexane, and ethanolamine and dicyclohexane The molar ratio of the azeotropic distillation column is 1:1.25, the operating pressure of the azeotropic distillation column is 20kPa, the temperature at the top of the column is 122.4°C, the temperature at the bottom of the column is 145.8°C, and the reflux ratio is 1.5; the top fraction of the azeotropic distillation column T1 enters the phase separation The phase separator V1 is used for phase separation, the upper layer is the entrainer, which is circulated to the azeotrop...

Embodiment 2

[0033] Example 2: The azeotrope and entrainer of triethylenediamine and ethanolamine enter the azeotropic rectification tower T1. agent mixture, the solid product obtained after cooling, crystallization and filtration of the mixture is triethylenediamine with a purity of 99.8%. The entrainer is decahydronaphthalene, ethanolamine and decalin in the azeotrope The molar ratio of the azeotropic distillation column is 1:2.25, the operating pressure of the azeotropic distillation column is 20kPa, the temperature at the top of the column is 113.5°C, the temperature at the bottom of the column is 126.1°C, and the reflux ratio is 1.5; the top fraction of the azeotropic distillation column T1 enters the phase separation The phase separator V1 is used for phase separation, the upper layer is an azeotropic agent, which is circulated to the azeotropic distillation tower, and the lower layer is the crude ethanolamine, which enters the ethanolamine refining tower T2, wherein the operating pre...

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Abstract

The invention aims at providing a separation method of triethylene diamine and ethanolamine azeotrope which has low use amount of an azeotrope former and small energy consumption. The separation method of triethylene diamine and ethanolamine azeotrope provided by the invention is carried out according to the following steps: (1) the azeotrope of triethylene diamine and ethanolamine and the azeotrope former are sent into an azeotropic distillation column, wherein an overhead fraction is azeotrope of the azeotrope former and ethanolamine, the tower kettle fraction is a mixture of triethylene diamine and azeotrope former, and the azeotrope former is bicyclohexyl or decalin; (2) the overhead fraction of the azeotropic distillation column enters a phase splitter to carry out phase separation, wherein the upper layer is the azeotrope former which is recycled to the azeotropic distillation column and the lower layer is an ethanolamine crude product which enters an ethanolamine refined tower; and (3) the overhead fraction of the ethanolamine refined tower is azeotrope of the azeotrope former and ethanolamine which is recycled to the azeotropic distillation column, and the tower kettle fraction of the ethanolamine refined tower is ethanolamine. The separation method of triethylene diamine and ethanolamine azeotrope provided by the invention can effectively reduce the use amount of the azeotrope former and obviously lower the energy consumption.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of fine chemicals, and relates to a separation method of triethylenediamine and ethanolamine azeotrope. Background technique [0002] Triethylenediamine is a foaming agent for the production of polyurethane soft, semi-rigid, and rigid foams, and is also used in ethylene polymerization catalysts, coatings, and plastic products. [0003] At present, the raw materials for the preparation of triethylenediamine are mainly N-hydroxyethylpiperazine, ethylenediamine, ethanolamine, [0004] piperazine etc. When ethanolamine and liquid ammonia are used as raw materials to catalyze amination to synthesize ethylenediamine or piperazine, triethylenediamine can be co-produced. Since the boiling points of triethylenediamine (boiling point: 174°C) and ethanolamine (boiling point: 170°C) are very close, the two are easy to form an azeotrope, and it is difficult to separate them by conventiona...

Claims

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Application Information

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IPC IPC(8): C07D487/08C07C215/08C07C213/10
Inventor 杨建明吕剑王伟王博余秦伟曾纪珺赵锋伟袁俊杨志强王为强梅苏宁
Owner XIAN MODERN CHEM RES INST
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