Unlock instant, AI-driven research and patent intelligence for your innovation.

Production method of ethylenediamine

A technology of ethylenediamine and ethanolamine, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve problems such as ammonia recovery and water separation difficulties

Active Publication Date: 2018-02-13
CHINA PETROLEUM & CHEM CORP +1
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] The technical problem to be solved by the present invention is the difficult problem of ammonia recovery and water separation in the prior art, and a new method for producing ethylenediamine with ethanolamine and liquid ammonia as raw materials is provided, which is used to produce ethylenediamine In the amine process, it has the advantages of convenient ammonia recovery and water separation

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Production method of ethylenediamine
  • Production method of ethylenediamine
  • Production method of ethylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] The reaction temperature of the ammoniation reactor is 180°C, the reaction pressure in terms of absolute pressure is 6MPa, and in terms of mass percentage, the reaction product is composed of 13.35% of water, 46.08% of ethanolamine, 27.6% of ethylenediamine, 1.14% of diethylenetriamine, three Ethylenediamine is 3.61%, piperazine is 4.7%, hydroxyethylpiperazine is 3.5%, and the single pass conversion rate of ethanolamine is 50.59%.

[0058] The theoretical plate number of the ammonia recovery tower is 25. In terms of absolute pressure, the operating pressure at the top of the ammonia recovery tower is 25kPa, the temperature at the top of the tower is -9°C, the temperature of the deamination tower is 163°C, and the liquid ammonia content in the bottom of the tower is less than 0.2 %.

[0059] Dehydration tower theoretical plate number is 20, selects toluene and n-butyl acetate composition as entrainer, wherein toluene and n-butyl acetate mass ratio are 80:20, in absolute ...

Embodiment 2

[0062] The reaction temperature of the ammoniation reactor is 190°C, the reaction pressure is 9MPa in terms of absolute pressure, and the reaction product is composed of 13.91% of water, 42.91% of ethanolamine, 33.01% of ethylenediamine, 0.77% of diethylenetriamine, and three Ethylenediamine is 2.93%, piperazine is 3.86%, hydroxyethylpiperazine is 2.59%, and the single pass conversion rate of ethanolamine is 52.99%.

[0063] The theoretical plate number of the ammonia recovery tower is 30. In terms of absolute pressure, the operating pressure at the top of the ammonia recovery tower is 35kPa, the temperature at the top of the tower is -5°C, the temperature at the bottom of the deammonization tower is 168°C, and the liquid ammonia content at the bottom of the tower is less than 0.15 %.

[0064] The number of theoretical plates of the dehydration tower is 25, and the composition of benzene and n-propyl acetate is selected as the entrainer, wherein the mass ratio of benzene and n...

Embodiment 3

[0067] The reaction temperature of the ammoniation reactor is 200°C, the reaction pressure in terms of absolute pressure is 12MPa, and in terms of mass percentage, the reaction product is composed of 14.57% of water, 40.63% of ethanolamine, 32.97% of ethylenediamine, 1.23% of diethylenetriamine, three Ethylenediamine is 3.35%, piperazine is 4.50%, hydroxyethylpiperazine is 2.72%, and the single pass conversion rate of ethanolamine is 54.89%.

[0068] The theoretical plate number of the ammonia recovery tower is 40. In terms of absolute pressure, the operating pressure at the top of the ammonia recovery tower is 45kPa, the temperature at the top of the tower is 1.3°C, the temperature at the bottom of the deamination tower is 176.8°C, and the liquid ammonia content at the bottom of the tower is less than 0.1%. .

[0069] Dehydration tower theoretical plate number is 35, selects toluene and sec-butyl acetate composition as entrainer, wherein toluene and sec-butyl acetate mass rat...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
boiling pointaaaaaaaaaa
Login to View More

Abstract

The invention relates to a method for producing ethylenediamine by a liquid ammonia method, which mainly solves the problems of difficult ammonia recovery and water separation in the prior art. In the present invention, liquid ammonia and ethanolamine are fed into the ammoniation reactor after being preheated, and the reaction product enters the ammonia recovery tower to recover ammonia, and the recovered liquid ammonia is circulated to the ammoniation reactor, and the liquid in the ammonia recovery tower is sent to the azeotropic refiner in the dehydration tower. Distillation and dehydration, the entrainer is a composition composed of at least one A selected from C6-C10 hydrocarbons and at least one B selected from C2-C8 esters, the dehydration tower still liquid mainly contains ethylenediamine, Unreacted ethanolamine, triethylenediamine, diethylenetriamine, piperazine, hydroxyethylpiperazine and other by-products are removed from the still liquid to the ethylenediamine product tower, and the ethylenediamine product is obtained from the top of the tower, and the still liquid is removed for subsequent refining and separation A series of high value-added by-products are obtained, and ethanolamine is recovered and recycled to the ammoniation reactor. The technical solution obtained by separation solves this problem well, and can be used in the process production of ethylenediamine.

Description

technical field [0001] The invention relates to a method for producing ethylenediamine by catalytic ammonification using ethanolamine and liquid ammonia as raw materials. Background technique [0002] Ethylenediamine (EDA) is an important chemical raw material, widely used in the manufacture of organic compounds, polymer compounds, drugs, etc. Herbicides are chemical raw materials that are in short supply in China and mainly rely on imports. [0003] The current methods for producing ethylenediamine mainly include the dichloroethane method (EDC method) and the ethanolamine method (MEA method). The dichloroethane method is directly synthesized from dichloroethane and ammonia, and is carried out in a molybdenum-titanium stainless steel reaction pipe. The reaction temperature is controlled at 160-190°C, the pressure is 2.5MPa, and the reaction time is 1.5min. After the reaction, the synthetic liquid is evaporated. Part of the water and excess ammonia enter the neutralizer, ne...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/16C07C209/86C07C211/10
Inventor 胡松杨卫胜刘银川刘仲能王德举
Owner CHINA PETROLEUM & CHEM CORP