Method for synthesizing hexamethylenediamine key intermediate

An intermediate, the technology of hexamethylenediamine, which is applied in the field of synthesis of the key intermediate of hexamethylenediamine, 6-aminocapronitrile, can solve the problems affecting the reaction efficiency, affecting the normal operation of the reaction device, reducing the activity and service life of the catalyst, and achieving The process flow is simple, the effect of improving raw material utilization and product selectivity, and reducing surface coking

Active Publication Date: 2020-11-24
JIANGSU YANGNONG CHEM GROUP +3
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  • Abstract
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  • Claims
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Problems solved by technology

[0004] patent CN201710942344.8 provides a method for preparing 6-aminocapronitrile by gas phase method, using caprolactam as raw material, and caprolactam steam and hot ammonia gas in a certain mass ratio Mixing; the obtained mixture of caprolactam vapor and hot ammonia gas is subjected to ammoniation dehydration reaction in the presence of a catalyst to obtain an ammoniated effluent; the obtained ammoniated effluent is separated and purified to obtain pure 6-amino Capronitrile: In this method, caprolactam is dehydrated in the reaction process to generate 6-aminocapronitrile, and a small amount of water promotes the polymerization of caprolactam at high temperature, while the polymer produced by caprolactam polymerization will coke and adhere to the surface of the catalyst, reducing catalyst activity and service life. Affect the normal operation of the reaction device, thereby affecting the response efficiency of the whole set of questions

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  • Method for synthesizing hexamethylenediamine key intermediate
  • Method for synthesizing hexamethylenediamine key intermediate

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Embodiment 1

[0032] A kind of method of synthetic hexamethylenediamine key intermediate of the present invention, comprises the steps:

[0033] (1) The raw material caprolactam and ammonia water with a mass percentage concentration of 25% are transported to different preheaters with high-pressure pumps respectively for preheating. The final caprolactam and ammonia water are passed into the microchannel reactor at a molar ratio of 1:35, and the reaction is carried out at 500°C and 4MPa, and the reaction residence time is 8s;

[0034] (2) The material obtained after the reaction of step (1) is transported to the gas-liquid separator, and the gas-liquid separation is carried out at 120 ° C. The separated gas phase material ammonia and water are sent to step (1) to continue the reaction, and the separation is obtained The liquid phase material is 6-aminocaproamide;

[0035] (3) The 6-aminocaproic amide separated from the step (2) is pumped into the preheater with a high-pressure pump, and nit...

Embodiment 2

[0038] A method for synthesizing the key intermediate of hexamethylenediamine of the present invention, the basic method steps are the same as in Example 1, wherein, the difference is: in step (1), the molar ratio of the amount of raw ammonia and caprolactam is 1:1.

[0039] Result analysis method is the same as embodiment 1, specifically see table 1.

Embodiment 3

[0041] A method for synthesizing the key intermediate of hexamethylenediamine of the present invention, the basic method steps are the same as in Example 1, wherein, the difference is that in the step (1), the molar ratio of the amount of raw material ammonia and caprolactam is 50:1.

[0042] Result analysis method is the same as embodiment 1, specifically see table 1.

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Abstract

The invention relates to a method for synthesizing a hexamethylenediamine key intermediate, and is particularly suitable for synthesizing a hexamethylenediamine key intermediate namely 6-aminocapronitrile. The method comprises the following steps of preheating caprolactam and ammonia water, respectively introducing the caprolactam and the ammonia water into a micro-channel reactor, and performingreaction; separating the material obtained after the reaction to obtain 6-aminocaproamide; and preheating and gasifying the 6-aminocaproamide obtained by separation, introducing the gasified 6-aminocaproamide into a reactor loaded with a catalyst, and performing a reaction to obtain the 6-aminocapronitrile. An existing process route is broken through, the hexamethylenediamine key intermediate namely the 6-aminocapronitrile is synthesized more efficiently by an innovative method, a 6-aminocaproamide intermediate is generated through caprolactam ring-opening hydrolysis, and then dehydrating is performed to generate the 6-aminocapronitrile, so that caprolactam polymerization is effectively reduced, catalyst surface coking is reduced, the utilization rate of raw materials is increased, the selectivity of products is improved, the service life of the catalyst is prolonged, the process flow is simple, the production cost is low, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a method for synthesizing a key intermediate of hexamethylenediamine, and is especially suitable for the synthesis of the key intermediate of hexamethylenediamine, 6-aminocapronitrile. Background technique [0002] Hexamethylenediamine is an important chemical raw material, mainly used in the production of nylon 66, nylon 610 and diisocyanate (HDI). At present, the method for producing hexamethylenediamine mainly includes the production method carried out through the intermediate adiponitrile and the production method carried out through the intermediate 6-aminocapronitrile, wherein, the method for producing hexamethylenediamine is carried out by preparing the intermediate adiponitrile The cost is high. In the method for producing hexamethylenediamine through the intermediate 6-aminocapronitrile, the direct ammoniation of caprolactam is mainly used to synthesiz...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/24
CPCC07C253/20C07C231/08C07C255/24C07C237/06
Inventor 王刚许越王根林丁克鸿徐林聂庆超汪洋王浩张曦廖强殷剑虎郭玉秀陆仁标
Owner JIANGSU YANGNONG CHEM GROUP
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