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A kind of method of synthetic 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 normal operation of the reaction device, reducing the activity and service life of the catalyst, and affecting the reaction efficiency. Improve raw material utilization and product selectivity, reduce surface coking, and simplify the process

Active Publication Date: 2022-03-04
JIANGSU YANGNONG CHEM GROUP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

Method used

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  • A kind of method of synthetic hexamethylenediamine key intermediate
  • A kind of method of synthetic hexamethylenediamine key intermediate

Examples

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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 the key intermediate of hexamethylenediamine, which is particularly suitable for the synthesis of the key intermediate of hexamethylenediamine 6-aminocapronitrile, comprising: preheating the caprolactam and ammonia water respectively into a microchannel reactor, Carrying out the reaction; separating the obtained material after the reaction to obtain 6-aminocaproamide; Nitrile. The present invention breaks through the existing process route, more efficiently synthesizes 6-aminocapronitrile, the key intermediate of hexamethylenediamine, through an innovative method, generates 6-aminocaproamide intermediate through ring-opening hydrolysis of caprolactam, and then dehydrates to generate 6-aminocapronitrile , effectively reduce the polymerization of caprolactam, and reduce coking on the surface of the catalyst, thereby improving the utilization rate of raw materials and product selectivity, prolonging the life of the catalyst, and the process flow is simple, the production cost is low, and it is suitable for realizing 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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Patent Type & Authority Patents(China)
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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