Method for resource utilization of hexamethylenediamine key intermediate reaction residues

A technology for intermediate and hexamethylene diamine, which is applied in the field of recycling caprolactam, aminocapronitrile, and hexamethylene diamine key intermediate reaction residue resource utilization, can solve the impact of production efficiency and product quality, complex catalyst preparation process and harsh reaction conditions. and other problems to achieve the effect of solving the problem of residue pollution, realizing resource utilization and simple operation

Inactive Publication Date: 2020-10-09
JIANGSU YANGNONG CHEM GROUP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In caprolactam ammonification process, caprolactam and aminocapronitrile inevitably polymerize to form polymers during the reaction and post-treatment process, and finally form residue solid waste, which pollutes the environment and also has a certain impact on production efficiency and product quality
[0004] Patent CN1167483A discloses a preparation method of caprolactam, the method is in the presence of a heterogeneous catalyst and an organic solvent, in the liquid phase by cracking oligomers or polymers at high temperature and in the presence of a catalyst to prepare caprolactam; The advantage of the method is that it does not need to consume energy to separate a large amount of water and remove the catalyst, but the catalyst preparation process is complicated and the reaction conditions are harsh

Method used

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Examples

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Effect test

Embodiment 1

[0028] A method for resource utilization of a hexamethylenediamine key intermediate reaction residue of the present invention comprises the following steps:

[0029] (1) Put the residue and water into the high-pressure reaction kettle at the same time according to the mass ratio of 1:1, and carry out the depolymerization reaction at 100°C under normal pressure. After keeping the temperature at 100°C for 2 hours, cool down and release the pressure to take out the depolymerization reaction solution;

[0030] (2) Dehydrating the depolymerization reaction solution obtained in step (1) under negative pressure; then, performing negative pressure distillation to collect fractions to obtain aminocapronitrile and caprolactam products.

[0031] In the above examples, the high polymer content in the residue in step (1) is 15%; in step (2), when carrying out negative pressure dehydration, the absolute pressure is 1kPa, and the temperature is 100°C; , the absolute pressure is 0.1kPa, and t...

Embodiment 2

[0034] A method for resource utilization of a hexamethylenediamine key intermediate reaction residue of the present invention comprises the following steps:

[0035] (1) Put the residue and water into the high-pressure reaction kettle at the same time according to the mass ratio of 1:10, and carry out the depolymerization reaction at 300°C and 8.5MPa. After keeping the temperature at 300°C for 8 hours, cool down and release the pressure to take out the depolymerization reaction liquid;

[0036] (2) Dehydrating the depolymerization reaction solution obtained in step (1) under negative pressure; then, performing negative pressure distillation to collect fractions to obtain aminocapronitrile and caprolactam products.

[0037] In the above examples, the high polymer content in the residue in step (1) is 90%; in step (2), when carrying out negative pressure dehydration, the absolute pressure is 1.5kPa, and the temperature is 100°C; carry out negative pressure distillation , the abs...

Embodiment 3

[0040] A method for resource utilization of a hexamethylenediamine key intermediate reaction residue of the present invention comprises the following steps:

[0041] (1) the residue, water and catalyst Al 2 o 3 At the same time, put them into the high-pressure reactor respectively, and carry out the depolymerization reaction at 150°C and 0.5MPa. After keeping the temperature at 150°C for 3 hours, cool down and release the pressure to take out the depolymerization reaction liquid;

[0042] (2) Dehydrating the depolymerization reaction solution obtained in step (1) under negative pressure; then, performing negative pressure distillation to collect fractions to obtain aminocapronitrile and caprolactam products.

[0043] In above-mentioned embodiment, in step (1), the polymer content in the residue is 80%, the mass ratio of residue and water is 1:8, residue and Al 2 o 3 The mass ratio is 1:0.01; in step (2), when carrying out negative pressure dehydration, the absolute pressure...

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Abstract

The invention relates to a method for resource utilization of hexamethylenediamine key intermediate reaction residues. The method comprises the following steps: adding residues and water into a reaction kettle or a fixed bed reactor, and carrying out depolymerization reaction; and sequentially carrying out negative pressure dehydration and negative pressure distillation on the obtained depolymerization reaction solution, and collecting fractions to obtain aminocapronitrile and caprolactam. The process method is optimized in design and simple in operation, the hexamethylenediamine key intermediate reaction residues are subjected to efficient, green and environment-friendly recovery treatment, the problem of residue pollution in existing hexamethylenediamine production is well solved, resource utilization of residue solid waste is achieved, the recycled caprolactam and aminocapronitrile can be reused as raw materials for preparing hexamethylenediamine, and thus the method reduces pollution, enhances environmental protection, reduces production cost, improves economic benefits and is suitable for application and popularization in related industrial fields.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a method for resource utilization of the reaction residue of a key intermediate of hexamethylenediamine, which is especially suitable for recovering caprolactam and aminocapronitrile. Background technique [0002] Hexamethylenediamine (CAS No. 124-09-4) is widely used, mainly used in the production of nylon 66. Nylon 66 is the earliest polyamide to realize the industrialization mark. It is listed as the most important two polyamide material categories together with nylon 6, and it is used in polyimide carboxylate foam, polyurethane foam, coating, epoxy resin curing agent, There are also a large number of applications and developments in organic crosslinking agents, pesticides, iron ore and copper ore flotation agents. Hexamethylenediamine is a very important organic raw material in the field of chemical production, and the research and development of its produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D201/12C07D201/16C07D223/10C07C253/00C07C253/34C07C255/24
CPCC07C253/00C07C253/34C07D201/12C07D201/16C07D223/10C07C255/24
Inventor 王刚汪洋王根林丁克鸿徐林聂庆超殷剑虎陈耀坤李良善何成义
Owner JIANGSU YANGNONG CHEM GROUP
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