Method and device for preparing 6-amino-capronitrile with caprolactam liquid phase method

A technology of caprolactam liquid and aminocapronitrile is applied in the field of preparation of aminocapronitrile, which can solve the problems of high reaction temperature and high energy consumption of gas phase method, and achieve the effects of low reaction temperature, low energy consumption and low energy consumption

Inactive Publication Date: 2018-02-27
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are few patents on the preparation of 6-aminocapronitrile from caprolactam. At present, the methods for preparing 6-aminocapronitrile from caprolactam can be divided into gas-phase method and liquid-phase method according to the reaction state of caprolactam. Among them, the gas-phase method reacts The higher the temperature, the greater the energy consumption; the lower the temperature of the liquid phase method, the easier the reaction

Method used

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  • Method and device for preparing 6-amino-capronitrile with caprolactam liquid phase method
  • Method and device for preparing 6-amino-capronitrile with caprolactam liquid phase method
  • Method and device for preparing 6-amino-capronitrile with caprolactam liquid phase method

Examples

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Effect test

Embodiment 1

[0040] Mix 10g of caprolactam, 100g of adiponitrile, and 0.02g of phosphoric acid, and add them into a reaction kettle with an ammonia water separator to stir and heat at a stirring speed of 1000RPM. 2 hours. During the reaction, the mass ratio of ammonia to caprolactam was 5.8:1. After the reaction, the conversion rate of caprolactam was 58%, and the selectivity was 97.8%. The reaction product was subjected to rectification and separation to obtain 6-aminocapronitrile with a purity of 99.1%.

[0041] In this embodiment, when the temperature at the bottom of the vacuum distillation tower is 152° C., the temperature at the top of the tower is 130° C., and the vacuum degree is 2.4 torr, 6-aminocapronitrile is distilled from the top of the tower.

Embodiment 2

[0043] Mix 10g of caprolactam, 100g of adiponitrile, and 0.5g of ammonium phosphate, and add them into a reaction kettle with an ammonia water separator to stir and heat at a stirring speed of 1500RPM. Time 1.5 hours. During the reaction, the mass ratio of ammonia to caprolactam was 10:1. After the reaction, the conversion rate of caprolactam was 65%, and the selectivity was 98.2%. The reaction product was subjected to rectification and separation to obtain 6-aminocapronitrile with a purity of 99.2%.

[0044] In this embodiment, the temperature at the bottom of the vacuum distillation tower is 155° C., the temperature at the top of the tower is 134° C., and the vacuum degree is 2.8 torr, 6-aminocapronitrile is distilled from the top of the tower.

[0045] The product prepared in this embodiment is detected by gas chromatography and mass spectrometry, and the detection results are shown in figure 1 and figure 2 . Depend on figure 1 and figure 2It can be seen that the p...

Embodiment 3

[0047] Mix 10g of caprolactam, 50g of adiponitrile, and 1g of aluminum phosphate, and add them into a reaction kettle with an ammonia water separator to stir and heat at a stirring speed of 1300RPM. 2 hours. During the reaction, the mass ratio of ammonia to caprolactam was 18.2:1. After the reaction, the conversion rate of caprolactam was 56%, and the selectivity was 98.1%. The reaction product was subjected to rectification and separation to obtain 6-aminocapronitrile with a purity of 99.5%.

[0048] In this embodiment, the temperature at the bottom of the vacuum distillation tower is 158° C., the temperature at the top of the tower is 139° C., and when the vacuum degree is 3.5 torr, 6-aminocapronitrile is distilled from the top of the tower.

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Abstract

The invention provides a method and device for preparing 6-amino-capronitrile from caprolactam by adopting a liquid phase method. In the method for preparing the 6-amino-capronitrile, the caprolactamis taken as a raw material; the method for preparing the 6-amino-capronitrile comprises the following step: S1: mixing the caprolactam, an organic solvent and a catalyst at a certain mass ratio, so asto obtain a mixed solution, adding the mixed solution into a reaction kettle and stirring and heating the mixed solution; S2: when the mixed solution in step S1 reaches certain temperature, introducing ammonia gas into the mixed solution for a reaction; S3, after the reaction in step S2 is ended, rectifying and purifying a reaction product, so as to obtain pure 6-amino-capronitrile. In the methodfor preparing the 6-amino-capronitrile, the caprolactam is taken as the raw material, the reaction conversion rate is comparatively high, and the preparation process is simple.

Description

technical field [0001] The invention belongs to the technical field of preparation of aminocapronitrile, and in particular relates to a method and a device for preparing 6-aminocapronitrile by a caprolactam liquid phase method. Background technique [0002] 6-Aminocapronitrile is an important chemical intermediate that can be used to produce 1,6-hexamethylenediamine by complete hydrogenation, which can be used to produce the polymer nylon 66. At present, the preparation of 6-aminocapronitrile is mainly obtained by partial hydrogenation of 1,6 adiponitrile, such as patents CN1238334C and CN101309897B, or by hydroformylation of pentenenitrile, such as patent CN1100752C. There are few patents on the preparation of 6-aminocapronitrile from caprolactam. Currently, the methods for preparing 6-aminocapronitrile from caprolactam can be divided into gas-phase method and liquid-phase method according to the reaction state of caprolactam. Among them, the gas-phase method reacts The hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C255/24
CPCC07C253/20C07C255/24
Inventor 史文涛杨克俭王聪武金丹杨琦武孙承宇崔艳杰
Owner CHINA TIANCHEN ENG
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