Production method for ethylenediamine through catalytic ammoniation process

A technology of ethylenediamine and ethanolamine, which is applied in chemical instruments and methods, preparation of organic compounds, purification/separation of amino compounds, etc., can solve the problems of low purity of ethylenediamine and piperazine products, difficulty in separation of crystal water, etc.

Active Publication Date: 2016-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by the present invention is the problem of low purity of ethylenediamine and piperazine products and difficult separation of crystal water in the prior art, and a new method for producing ethylenediamine by catalytic ammonification is provided. When used in the production of ethylenediamine, it has the advantages of high purity of ethylenediamine and piperazine and effective separation of crystal water

Method used

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  • Production method for ethylenediamine through catalytic ammoniation process
  • Production method for ethylenediamine through catalytic ammoniation process
  • Production method for ethylenediamine through catalytic ammoniation process

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Process flow chart such as figure 1 As shown, liquid ammonia and MEA enter R101 after being heated, and MEA is divided into one or more strands. The reaction product 1 enters the ammonia recovery system X101 to recover ammonia. After the ammonia is recovered, the mixture 2 containing MEA enters the initial distillation tower T101 to separate EDA and free water. EDA and free water enter the EDA tower T102, pressurized rectification, the waste water 3 at the top of the tower goes to post-treatment, and the EDA product 4 is obtained from the bottom of the tower. The liquid in the primary distillation tower T101 enters the azeotropic distillation tower T103, the entrainer replenishment line 6 is connected to the return line at the top of the azeotropic distillation tower T103, the waste water 5 goes to post-treatment, and the liquid in the bottom of the tower goes to the PIP tower T104. The side line discharge 7 at the top of the PIP tower T104 is the PIP product, and the ...

Embodiment 2

[0056] Embodiment is identical with embodiment 1.

[0057] T101, T103~T108 are all filled with 500m 2 / m 3 Metal mesh corrugated packing with specific surface area. T102 loading 500m 2 / m 3 Specific surface area corrugated wire mesh packing or valve tray.

[0058] The operating pressure of the initial distillation column T101 is 0.40MPaA.

[0059] The operating pressure of the EDA tower T102 is 0.52MPaA, the waste water produced at the top of the tower goes to post-treatment, the purity of the EDA product in the tower kettle is ≥99.9wt%, the organic impurities are ≤0.05wt%, the water content is ≤0.05wt%, and the APHA is ≤15.

[0060] The operating pressure of the azeotropic distillation column T103 is 0.07MPaA.

[0061]The operating pressure of the PIP tower T104 is 0.03MPaA, the top of the tower is taken back to the azeotropic distillation tower T103, and the PIP product is taken from the fifth theoretical plate below the top of the tower. The purity of the PIP product ...

Embodiment 3

[0067] Embodiment is identical with embodiment 1, and process flow chart is as figure 2 shown.

[0068] figure 1 The azeotropic distillation column in the dotted line box is cancelled, the T101 column kettle stream directly enters the T104 column, the top of the T104 column is extracted and returned to the T101 column, and the hexahydrate PIP product is extracted from the fifth theoretical plate below the top of the T104 column.

[0069] T101, T104~T108 are all filled with 550m 2 / m 3 Metal mesh corrugated packing with specific surface area. T102 loading 550m 2 / m 3 Specific surface area corrugated wire mesh packing or valve tray.

[0070] The operating pressure of the initial distillation column T101 is 0.45MPaA.

[0071] The operating pressure of the EDA tower T102 is 0.55MPaA, the waste water produced at the top of the tower goes to post-treatment, the purity of the EDA product in the tower kettle is ≥99.9wt%, the organic impurities are ≤0.05wt%, the water content ...

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Abstract

The invention relates to a production method for ethylenediamine through a catalytic ammoniation process. The production method provided by the invention comprises the following steps: firstly recovering ammonia from catalytic amination reaction products, then separating free water and ethylenediamine (EDA) through rectification, and subjecting the free water and ethylenediamine (EDA) to azeotrope removal through pressurized rectification so as to obtain an ethylenediamine (EDA) product; and subjecting a monoethanolamine-contained mixture obtained from separation of the free water and ethylenediamine (EDA) to azeotropic rectification and separating crystal water so as to obtain anhydrous piperazine (PIP), then carrying out ordinary rectifying separation through a plurality of rectifying towers so as to obtain diethylenetriamine (DETA), separating a mixture of monoethanolamine (MEA) and triethylenediamine (TEDA) through pressure-swing rectification, recycling monoethanolamine (MEA) to an ammoniation reactor, and subjecting heavy components (aminoethyl ethanolamine (AEEA), aminoethylpiperazine (AEP), hydroxyethyl piperazine (HEP), oligomers and a heavy-component amine mixture) to stage-by-stage separation through a plurality of falling-film evaporators. Thus, the production method provided by the invention can be applied in industrial production of ethylenediamine.

Description

technical field [0001] The invention relates to a method for producing ethylenediamine by catalytic ammonification, specifically, a method for producing ethylenediamine by catalytic ammonification of ethanolamine. Background technique [0002] Ethylenediamine (EDA) is an important chemical raw material widely used in the production of pesticides, medicines and various chemical auxiliaries. EDA is a chemically active fine intermediate and pharmaceutical intermediate. It has the characteristics of surface activity. It is easy to form a salt when it encounters an acid. It can form an azeotrope with water and is slightly soluble in ether. In recent years, the application of EDA in my country has developed rapidly, and its annual demand growth rate has reached more than 20%. It has become one of the fine petrochemical intermediates that my country urgently needs to develop. At present, the domestic market of EDA mainly relies on imports, making ethylenediamine one of the few che...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/16C07C209/86C07C211/10C07C211/14C07C213/08C07C213/10C07C215/14C07D295/023C07D295/027C07D295/088C07D295/13
Inventor 胡松杨卫胜刘银川
Owner CHINA PETROLEUM & CHEM CORP
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