Method for preparing 6-aminocapronitrile

A technology of aminocapronitrile and aminocaproamide, which is applied in the field of two-step preparation of the key intermediate 6-aminocapronitrile of hexamethylenediamine, which can solve problems such as increased energy consumption, increased polymer, and coking of catalysts

Pending Publication Date: 2021-10-08
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The main purpose of the present invention is to provide a continuous preparation method of 6-aminocapronitrile, a key intermediate of hexamethylenediamine, to solve the problem in the prior art that the catalyst for preparing 6-aminocapronitrile is easy to coke and deactivate, which affects the operation stability of the device , and also solve the problem of hydrolysis and then ammoniation in the original two-step method, resulting in increased energy consumption, increased polymers, and catalyst coking in catalytic ammoniation dehydration

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  • Method for preparing 6-aminocapronitrile

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Embodiment 1

[0054] The method for the synthetic hexamethylenediamine key intermediate 6-aminocapronitrile of the present invention, comprises the steps:

[0055] (1) The raw material caprolactam is transported to different preheaters through a temperature-controlled metering pump and ammonia gas for preheating. The preheating temperature of caprolactam is 280°C, and the preheating temperature of ammonia gas is 350°C. According to the molar ratio of 1:30, the ammonia gas is passed into the microchannel reactor I, and the reaction is carried out at 450°C and 5MPa, and the residence time in the microchannel reactor I is 15s;

[0056] (2) Transport the material obtained after the reaction in step (1) to a gas-liquid separator, and perform gas-liquid separation at 200 ° C. The separated gas phase material ammonia gas is sent to step (1) to continue the reaction, and the liquid phase is separated. The material is 6-aminocaproamide;

[0057] (3) After the 6-aminocaproamide separated from step (...

Embodiment 2

[0060] The method for the synthetic hexamethylenediamine key intermediate 6-aminocapronitrile of the present invention, comprises the steps:

[0061] (1) The raw material caprolactam is transported to different preheaters through a temperature-controlled metering pump and ammonia gas for preheating respectively. The preheating temperature of caprolactam is 300°C, and the preheating temperature of ammonia gas is 350°C. According to the molar ratio of 1:20, the ammonia gas is passed into the microchannel reactor I, and the reaction is carried out at 350°C and 1MPa, and the residence time in the microchannel reactor I is 60s;

[0062] (2) Transport the material obtained after the reaction in step (1) to a gas-liquid separator, and perform gas-liquid separation at 250 ° C. The separated gas phase material ammonia gas is sent to step (1) to continue the reaction, and the liquid phase is obtained by separation. The material is 6-aminocaproamide;

[0063] (3) After the 6-aminocaproa...

Embodiment 3

[0066] The method for the synthetic hexamethylenediamine key intermediate 6-aminocapronitrile of the present invention, comprises the steps:

[0067] (1) The raw material caprolactam is transported to different preheaters through a temperature-controlled metering pump and ammonia gas for preheating respectively. The preheating temperature of caprolactam is 250°C and that of ammonia gas is 200°C. According to the molar ratio of 1:10, the ammonia gas is passed into the microchannel reactor I, and the reaction is carried out at 400°C and 5MPa, and the residence time in the microchannel reactor I is 120s;

[0068] (2) Transport the material obtained after the reaction in step (1) to a gas-liquid separator, and perform gas-liquid separation at 200 ° C. The separated gas phase material ammonia gas is sent to step (1) to continue the reaction, and the liquid phase is separated. The material is 6-aminocaproamide;

[0069] (3) After the 6-aminocaproamide separated from step (2) is pum...

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Abstract

The invention provides a method for preparing 6-aminocapronitrile, which comprises the following steps: (1) respectively preheating caprolactam and ammonia gas, and introducing the preheated caprolactam and ammonia gas into a micro-channel reactor I for reaction to obtain 6-aminohexanamide; (2) carrying out gas-liquid separation on a material obtained after the reaction in the step (1) to obtain a liquid-phase material 6-aminohexanamide; and (3) preheating the 6-aminohexanamide separated in the step (2), introducing the preheated 6-aminohexanamide into a micro-channel reactor II, and simultaneously introducing a dehydrating agent to carry out a dehydration reaction, thereby obtaining the 6-aminocapronitrile. According to the method, polymerization of ammonolysis products is effectively controlled, generation of by-products is reduced, a dehydrating agent is used for a dehydration reaction under the catalyst-free condition, and the problems of catalyst coking, short catalyst service life and the like in a catalytic dehydration process are effectively avoided.

Description

technical field [0001] The invention belongs to the technical field of synthesis of hexamethylenediamine, and specifically relates to a two-step method for preparing the key intermediate of hexamethylenediamine, 6-aminocapronitrile. Background technique [0002] 1,6-hexamethylenediamine is an intermediate of important high-performance materials such as nylon 66, nylon 610, etc. It is also used in the production of polyurethane, such as 1,6-hexamethylene diisocyanate (HDI), and can also be used as urea-formaldehyde resin, ring Curing agent for epoxy resin. [0003] According to different raw materials, there are four main production methods of hexamethylenediamine: butadiene method, acrylonitrile method, adipic acid method and caprolactam method. [0004] The butadiene method usually uses transition metal complexes such as Rh, Ni, and Ru as catalysts, and introduces two molecules of hydrocyanic acid into butadiene, and the addition reaction produces adiponitrile, which is th...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/24B01J19/00
CPCC07C253/20C07C231/10B01J19/0093C07C255/24C07C237/06Y02P20/52
Inventor 谢增勇杨学林王耀红刘东磊王树平陈西波党伟荣
Owner BEIJING RISUN TECH CO LTD
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