Method for producing hexamethylenediamine key intermediate 6-aminocapronitrile by continuous gas-phase two-step method

A technology of aminocapronitrile and hexamethylenediamine, which is applied in the field of preparation of 6-aminocapronitrile, can solve the problems such as easy coking of the catalyst, achieve the effect of reducing catalytic polymerization, avoiding polymerization reaction, and improving stability

Active Publication Date: 2020-08-25
JIANGSU YANGNONG CHEM GROUP +2
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  • Abstract
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  • Application Information

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Problems solved by technology

[0007] The main purpose of the present invention is to provide a method for producing the key intermediate 6-aminocapronitrile of hexamethylenediamine in a continuous gas-phase two-step process, so as to solve the problem that the catalyst is easy to coke when the caprolactam one-step method prepares 6-aminocapronitrile in the prior art

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  • Method for producing hexamethylenediamine key intermediate 6-aminocapronitrile by continuous gas-phase two-step method
  • Method for producing hexamethylenediamine key intermediate 6-aminocapronitrile by continuous gas-phase two-step method

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Effect test

Embodiment 1

[0037] Heat water to 500°C, caprolactam and water are simultaneously pumped into the first reactor filled with inert filler (porcelain balls) at a weight ratio of 1:8, at a gauge pressure of 3MPa, a reaction temperature of 500°C and a residence time of 1s. Hydrolysis reaction to obtain hydrolyzed material (amino caproic acid). Mix 500°C ammonia gas 0.5 times the weight of caprolactam with the hydrolyzed material, pump it into the second reactor filled with silica catalyst, and catalyze it at 300°C, gauge pressure 0.1MPa, reaction temperature 350°C and residence time 2s Ammonification and dehydration reactions generate 6-aminocapronitrile, the one-pass conversion rate of caprolactam is 95.6%, and the one-pass life of the catalyst is determined to be 1320h when the aminocapronitrile selectivity is less than 98%.

Embodiment 2

[0039] Heat 1% ammonia water to 400°C, and simultaneously pump caprolactam and water into the first reactor filled with solid acid (ZSM-5) at a weight ratio of 1:5. The hydrolysis reaction was carried out at a time of 0.6 s to obtain the hydrolyzed material (aminocaproic acid). Mix 400°C ammonia with 3 times the weight of caprolactam with the hydrolyzed material, pump it into the second reactor filled with alumina catalyst, and catalyze it at 400°C, gauge pressure 0.6MPa, reaction temperature 450°C and residence time 0.5s Ammonification and dehydration reactions generate 6-aminocapronitrile, the one-pass conversion rate of caprolactam is 97.1%, and the one-pass life of the catalyst is determined to be 1400h when the aminocapronitrile selectivity is less than 98%.

Embodiment 3

[0041] Heat 10% ammonia water to 400°C, and simultaneously pump caprolactam and ammonia water into the first reactor filled with solid acid (ZSM-5) at a weight ratio of 1:5. Under 0.6s, the hydrolysis and ammoniation reaction is carried out to obtain the hydrolyzed material. Mix 400°C ammonia with 3 times the weight of caprolactam with the hydrolyzed material, send it into the second reactor filled with alumina catalyst, and catalyze it at 400°C, gauge pressure 0.6MPa, reaction temperature 450°C and residence time 0.5s Ammonification and dehydration reactions generate 6-aminocapronitrile, the one-pass conversion rate of caprolactam is 98.8%, and the one-pass life of the catalyst is judged to be 1500h when the aminocapronitrile selectivity is less than 98%.

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Abstract

The invention provides a method for producing a hexamethylenediamine key intermediate 6-aminocapronitrile by a continuous gas-phase two-step method. The method comprises the following steps: S1, mixing caprolactam and water in a gas phase state to carry out continuous hydrolysis or mixing caprolactam and ammonia water in a gas phase state to carry out continuous hydrolysis ammoniation reaction toobtain a first product system containing 6-aminocaproic acid, 6-aminocaproic acid ammonium salt and/or 6-aminocaproamide; and S2, carrying out continuous gas-phase catalytic ammoniation and dehydration reaction on the first product system and ammonia gas to obtain a second product system containing 6-aminocapronitrile. According to the patent of the invention, the problem that water generated by reaction in a one-step process promotes polymerization reaction of the raw material caprolactam is reduced from the source, and the selectivity of aminocapronitrile is improved; and the problems of catalyst deactivation and pressure drop rise caused by polymerization and coking of caprolactam in the reactor are effectively reduced, the stability of the device is improved, and the service life of the catalyst is prolonged.

Description

technical field [0001] The invention relates to the technical field of preparation of 6-aminocapronitrile, in particular to a method for producing 6-aminocapronitrile, a key intermediate of hexamethylenediamine, in a continuous gas-phase two-step process. Background technique [0002] 1,6-Hexamethylenediamine is an important high-performance material intermediate, mainly used in the production of polyamide, such as nylon 66, nylon 610, etc. It can also be used in the production of polyurethane, and can also be used as a curing agent for urea-formaldehyde resin and epoxy resin . [0003] According to different raw materials, the production method of hexamethylenediamine is divided into adiponitrile method and caprolactam method, the former is the main industrial production method, and the production method of adiponitrile can be divided into: butadiene method, acrylonitrile method, adiponitrile method, Diacid method. [0004] The butadiene method is in the presence of trans...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/22C07C253/20C07C255/24C07C227/22C07C229/08C07C231/02C07C237/06
CPCC07C253/22C07C253/20C07C227/22C07C231/02C07C229/08C07C255/24C07C237/06
Inventor 王根林徐林丁克鸿梅学赓王铖殷恒志刘鑫王鑫宇郭博博
Owner JIANGSU YANGNONG CHEM GROUP
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