Method and device for producing hexamethylenediamine from caprolactam

A technology of caprolactam and hexamethylenediamine, applied in separation methods, bulk chemical production, chemical instruments and methods, etc., can solve the problems of no industrial application value, many by-products, high reaction temperature, etc.

Active Publication Date: 2021-05-18
宁波迦尔新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method integrates ammonification and hydrogenation of caprolactam, but has the disadvanta

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  • Method and device for producing hexamethylenediamine from caprolactam

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Experimental program
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Embodiment 1

[0055] Production of hexamethylenediamine from caprolactam

[0056] Evaporate caprolactam in the evaporator, mix it with hot ammonia gas at a molar ratio of 1:30, and enter the fixed-bed reactor filled with magnesium phosphate catalyst. The temperature is controlled at 300-400°C, and the reaction pressure is 0-1.0MPa; 720~3600h -1 ;

[0057] The ammoniated dehydration reaction product obtained above is subjected to primary condensation, cooled to 300-315°C, and the heavy component is separated; then the primary condensed gas phase is subjected to secondary condensation, cooled to 140-210°C, and the caprolactam, 6- The condensate of aminocapronitrile; the gas phase of the secondary condensation is condensed in the third stage, cooled to 40-60°C, and the water is separated, and the ammonia gas in the gas phase is returned to the ammoniation dehydration reaction as a raw material for reuse;

[0058] The caprolactam and 6-aminocapronitrile condensate obtained by the secondary co...

Embodiment 2

[0063] Production of hexamethylenediamine from caprolactam

[0064] Evaporate caprolactam in the evaporator, mix it with hot ammonia gas at a molar ratio of 1:30, and enter the fixed-bed reactor filled with magnesium phosphate catalyst. The temperature is controlled at 300-400°C, and the reaction pressure is 0-1.0MPa; the gas phase space velocity is 730~3600h -1 ;

[0065] The ammoniated dehydration reaction product obtained above is subjected to primary condensation, cooled to 300-315°C, and the heavy component is separated; then, the primary condensed gas phase is subjected to secondary condensation, cooled to 140-210°C, and the caprolactam, 6- The condensate of aminocapronitrile; the gas phase of the secondary condensation is condensed in the third stage, cooled to 40-60°C, and the water is separated, and the ammonia gas in the gas phase is returned to the ammoniation dehydration reaction for reuse as a raw material;

[0066] The caprolactam and 6-aminocapronitrile conden...

Embodiment 3

[0071] Production of hexamethylenediamine from caprolactam

[0072] Evaporate caprolactam in the evaporator, mix it with hot ammonia gas at a molar ratio of 1:30, and enter the fixed-bed reactor filled with magnesium phosphate catalyst. The temperature is controlled at 300-400°C, and the reaction pressure is 0-1.0MPa; 730~3600h -1 ;

[0073] The ammoniated dehydration reaction product obtained above is subjected to primary condensation, cooled to 300-315°C, and the heavy component is separated; then, the primary condensed gas phase is subjected to secondary condensation, cooled to 140-180°C, and the caprolactam, 6- The condensate of aminocapronitrile; the gas phase of the secondary condensation is condensed in the third stage, cooled to 40-60°C, and the water is separated, and the ammonia gas in the gas phase is returned to the ammoniation dehydration reaction for reuse as a raw material;

[0074] The caprolactam and 6-aminocapronitrile condensate obtained by the secondary c...

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Abstract

The invention discloses a method and a device for producing hexamethylenediamine from caprolactam, ammonia gas and caprolactam are subjected to ammoniation and dehydration reaction under the action of a catalyst, and the obtained ammoniation and dehydration reaction product is subjected to three-stage condensation separation; caprolactam obtained through secondary condensation and 6-aminocapronitrile condensate are subjected to a hydrogenation reaction under the action of a catalyst, a mixture containing hexamethylenediamine and caprolactam obtained through the reaction is separated to obtain hexamethylenediamine, and water accounting for 5%-500% of the total weight of the condensate is added in the hydrogenation reaction process to serve as a hydrogenation reaction diluent. According to the method, the caprolactam aqueous solution is used as the 6-aminocapronitrile hydrogenation reaction diluent, ethanol does not need to be added as the diluent, and generation of by-products N-Et-HMD, BHT and tar is reduced. The ammoniation dehydration reaction liquid is not subjected to rectification separation, so that the energy consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of organic chemicals, and relates to a method for producing hexamethylenediamine from caprolactam, in particular to a method and a device for producing hexamethylenediamine by hydrogenating a mixture of 6-aminocapronitrile and caprolactam. Background technique [0002] Hexamethylenediamine is a key raw material in the nylon industry. It is often used to synthesize nylon 66 and nylon 610, and then to make nylon resin, nylon fiber and engineering plastics and other products. The industrial production method of hexamethylenediamine is mainly the catalytic hydrogenation of adiponitrile, which produces diaminocyclohexane, an impurity that has a great impact on the quality of nylon products, and is difficult to separate when producing hexamethylenediamine. At present, with the increasing capacity of caprolactam and the decreasing price, the caprolactam method is expected to be promoted industrially. The caprolact...

Claims

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Application Information

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IPC IPC(8): C07C211/12C07C209/48C07C255/24C07C253/20C07C253/34C07C209/86B01D5/00B01J19/00
CPCC07C209/48C07C209/86C07C253/34C07C253/20B01D5/0036B01J19/00C07C211/12C07C255/24Y02P20/52
Inventor 陈天然虞新建
Owner 宁波迦尔新材料技术有限公司
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