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Process for producing ethylenediamine by liquid ammonia method

A technology of ethylenediamine and liquid ammonia, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of aminohydroxyl compounds, and can solve problems such as the difficulty in obtaining high-purity piperazine and triethylenediamine products

Active Publication Date: 2018-08-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, piperazine and triethylenediamine are easily soluble in water and form crystalline hydrates with water. It is difficult to obtain high-purity piperazine and triethylenediamine products by simple rectification.

Method used

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  • Process for producing ethylenediamine by liquid ammonia method
  • Process for producing ethylenediamine by liquid ammonia method
  • Process for producing ethylenediamine by liquid ammonia method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Liquid ammonia and MEA enter R101 after heating, reaction product 1 enters ammonia recovery system X101 to recover ammonia, and after ammonia is recovered, the mixture containing MEA enters dehydration tower T101 for azeotropic distillation and dehydration, waste water 3 enters post-treatment, and tower still liquid enters EDA tower T102 EDA product 5 is obtained by separation, the tower bottom liquid enters the PIP tower T103, and the PIP product is obtained by separation. Separation by pressure swing rectification in column T107, the liquid in high-pressure tower T107 is TEDA product 11, the liquid in low-pressure tower T106 is unreacted MEA10, which is recycled to reactor R101, and the liquid in heavy component separation tower T104 enters DETA tower T105 for separation to obtain DETA The product 8 and the still liquid 9, and the still liquid 9 can be further separated to obtain AEEA, AEP, HEP, oligomers, and heavy component mixed amines.

[0055] T101~T107 are all f...

Embodiment 2

[0062] Embodiment is identical with embodiment 1.

[0063] T101~T107 are all filled with 450m 2 / m 3 Metal mesh corrugated packing with specific surface area.

[0064] The operating pressure of the EDA tower T102 is 0.04MPaA, and the extraction from the top of the tower returns to the dehydration tower T101. The EDA product is extracted from the fifth theoretical plate below the top of the tower. The purity of the EDA product is ≥99.6wt%, the organic impurities are ≤0.4wt%, and the water content ≤0.4wt%, APHA≤15.

[0065] The operating pressure of the PIP tower T103 is 0.04MPaA, and the extraction from the top of the tower returns to the EDA tower T102, and the PIP product is extracted from the fourth theoretical plate below the top of the tower. The purity of the PIP product is ≥99.8wt%, the organic impurities are ≤0.2wt%, and the water content ≤0.2wt%, chroma, APHA≤30.

[0066] The operating pressure of the heavy component separation tower T104 is 20kPaA, the output from...

Embodiment 3

[0070] Embodiment is identical with embodiment 1.

[0071] T101~T107 are all filled with 550m 2 / m 3 Metal mesh corrugated packing with specific surface area.

[0072] The operating pressure of EDA tower T102 is 0.06MPaA, and the extraction from the top of the tower returns to the dehydration tower T101. The EDA product is extracted from the third theoretical plate below the top of the tower. The purity of the EDA product is ≥99.9wt%, the organic impurities are ≤0.1wt%, and the water content ≤0.1wt%, APHA≤15.

[0073] The operating pressure of the PIP tower T103 is 0.05MPaA, and the extraction from the top of the tower returns to the EDA tower T102. The PIP product is extracted from the third theoretical plate below the top of the tower. The purity of the PIP product is ≥99.8wt%, the organic impurities are ≤0.1wt%, and the water content ≤0.1wt%, chroma, APHA≤30.

[0074] The operating pressure of the heavy component separation tower T104 is 30kPaA, the output from the top ...

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Abstract

The invention relates to a process of producing ethylene diamine through a liquid ammonia method. In the process, a catalytic ammoniation reaction product is subjected to ammonia recycling and azeotropic distillation to remove free water and crystallized water to obtain a mixture containing monoethanol amine, which then is separated through a plurality of rectification columns to obtain the ethylene diamine (EDA), piperazine (PIP), diethylene triamine (DETA), triethylene diamine (TEDA), a heavy component (including: aminoethyl ethanolamine (AEEA), aminoethyl piperazine (AEP), hydroxyethyl piperazine (HEP), and the like mixed amine and oligomers), and meanwhile, the monoethanol amine (MEA) which is not reacted is separated and recycled and then is fed back to an ammoniation reactor for being used in the process of producing the ethylene diamine.

Description

technical field [0001] The invention relates to a process for producing ethylenediamine by a liquid ammonia method, specifically, a process for producing ethylenediamine by catalytic ammoniation of ethanolamine. Background technique [0002] Ethylenediamine (EDA) is an organic base with an amine functional group. It 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. in ether. EDA has a wide range of uses, and is widely used in organic compounds, polymer compounds, medicine, dyes, pesticides and other industries. It is an important fine chemical intermediate that needs to be imported urgently in China. Chelating agent EDTA, paper wetting enhancer, lubricating oil stabilizer, pesticide fungicide, rubber vulcanization accelerator, dye fixing agent and other fine chemical additives. At present, the domestic market of EDA mainly relies on imports, making ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/16C07C209/06C07C211/10C07C211/14C07C213/08C07C215/14C07D295/088C07D295/13C07D295/027C07D295/023
Inventor 胡松杨卫胜刘仲能
Owner CHINA PETROLEUM & CHEM CORP
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