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Method for preparing 6-aminocapronitrile product

A technology of aminocapronitrile and aminocaproate, applied in the field of preparation of aminonitrile, can solve the problems of unsuitability for large-scale industrialization, harsh reaction conditions, low reaction conversion rate, etc., and achieves saving purification unit consumption, less side reactions, high purity effect

Active Publication Date: 2020-06-05
湖北三宁碳磷基新材料产业技术研究院有限公司 +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. Patent CN107602416A mentions a technology for preparing 6-aminocapronitrile by caprolactam gas phase method, but it requires the reaction temperature to be above 300°C, pressurized, and the reaction conditions are harsh. It is not suitable for large-scale industrialization; although the patent CN107739318A mentions a caprolactam liquid-phase preparation process, its reaction conversion rate is low, and a large amount of nitrile solvents are used, which pollutes the environment

Method used

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  • Method for preparing 6-aminocapronitrile product
  • Method for preparing 6-aminocapronitrile product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Mix 10g of caprolactam and 100g of formic acid aqueous solution evenly, then add them into reaction kettle A and stir and heat at a stirring speed of 1000RPM. When the temperature rises to 110°C, the reflux reaction starts. After reflux for 2 hours, the reaction liquid is discharged to rectification kettle C. Distill to remove low boilers, transfer the rectification still liquid to reactor B, and use methanol-toluene (the volume ratio of methanol to toluene is 1:0.8) for recrystallization (stirring rate is 180 r / min, cooling rate is 2.5°C / min) to get 6-aminocaproic acid salt solid, drain the liquid in the kettle, add 30g of ethylene glycol, 25g of ammonium oxalate and 1g of phosphorus oxychloride into the kettle, mix evenly, stir and heat, the stirring speed is 1000RPM, and reflux reaction at 105°C Discharge after 3h. After the reaction, the reaction liquid was rectified under reduced pressure, separated and purified to obtain 6-aminocapronitrile with a purity of 98.3%...

Embodiment 2

[0037] Mix 10g of caprolactam and 150g of formic acid aqueous solution evenly, then add them into reaction kettle A, stir and heat, the stirring speed is 1100RPM, when the temperature rises to 112°C, the reflux reaction starts, and after reflux for 1.5h, the reaction liquid is discharged to rectification kettle C , to remove low boilers by distillation, transfer the rectification still liquid to reactor B, and recrystallize with ethylene glycol-toluene (the volume ratio of ethylene glycol and toluene is 1:0.5) (stirring speed is 150 r / min, cooling The rate is 2°C / min) to get 6-aminocaproic acid salt solid, drain the liquid in the kettle, add 40g of ethylene glycol, 35g of ammonium oxalate and 0.5g of ethyl phosphate into the kettle, stir and heat after mixing evenly, the stirring speed is 1100RPM , After reflux reaction at 150°C for 5h, the material was discharged. After the reaction, the reaction solution was rectified under reduced pressure, separated and purified to obtain ...

Embodiment 3

[0040]Mix 11g of caprolactam and 155g of acetic acid aqueous solution evenly, then add them into reaction kettle A, stir and heat, the stirring speed is 1200RPM, when the temperature rises to 110°C, the reflux reaction starts, and after reflux for 3 hours, the reaction liquid is discharged to rectification kettle C, Distill to remove low boilers, transfer the rectification still liquid to reactor B, and use methanol-p-xylene (the volume ratio of methanol and p-xylene is 1:0.8) for recrystallization (stirring rate is 190 r / min, cooling rate 3.5°C / min) to get 6-aminocaproic acid salt solid, drain the liquid in the kettle, add 40g of ethylene glycol, 35g of formamide and 0.6g of ethyl phosphate into the kettle, stir and heat after mixing evenly, the stirring speed is 1200RPM, After reflux reaction at 130°C for 2 hours, the material was discharged. After the reaction, the reaction solution was rectified under reduced pressure, separated and purified to obtain 6-aminocapronitrile w...

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Abstract

The invention relates to a method for preparing a 6-aminocapronitrile product. The method comprises the following steps: A, uniformly mixing caprolactam, an acidic solution and the like according to acertain ratio, then adding the mixture into a reaction kettle, heating and stirring the mixture and carrying out a reaction; B, after the caprolactam reaction in the step A is completed, removing low-boiling-point substances under reduced pressure, and recrystallizing the reaction product to obtain 6-aminocaproate; C, uniformly mixing the 6-aminocaproate obtained in the step B, alcohol, an ammoniating agent, a dehydrating agent and the like according to a certain ratio, adding the mixture into a reaction kettle, and heating and stirring the mixture and carrying out a reaction; and D, rectifying the reaction liquid obtained in the step C, and separating and purifying the reaction liquid to obtain 6-aminocapronitrile. According to the method for preparing the 6-aminocapronitrile product, the reaction conversion rate is high, the purity of the 6-aminocapronitrile product can reach 98% or above, the reaction conditions are mild, and the preparation process is relatively simple.

Description

technical field [0001] The invention relates to the technical field of preparation of aminonitriles, in particular to a method for preparing 6-aminocapronitrile products. Background technique [0002] 6-Aminocapronitrile is an important chemical intermediate, which is expensive. After hydrogenation, the downstream product 1,6-hexamethylenediamine is obtained, and 1,6-hexamethylenediamine is one of the three major nylon raw materials. It can be used To produce nylon 66, nylon 610, hexamethylene diisocyanate and other bulk chemical products. At present, the preparation of 6-aminocapronitrile products is mainly obtained by partial hydrogenation of 1,6-adiponitrile, such as patents CN1238334C and CN101309897B, or by hydrogenation of alkenonitriles, such as patent NL812780. There are few patents on the preparation of 6-aminocapronitrile from caprolactam. Patent CN107602416A mentions a technology for preparing 6-aminocapronitrile by caprolactam gas phase method, but it requires t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/22C07C255/24
CPCC07C253/22C07C227/22C07C255/24C07C229/08
Inventor 魏天荣安杰李慧徐国庆张小元陈坤
Owner 湖北三宁碳磷基新材料产业技术研究院有限公司
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