Method for recycling hexanediamine key intermediate reaction residues and co-producing carboxylic acid

A technology for the parallel co-production of carboxylic acid and intermediates, which is applied in the field of recycling and co-production of carboxylic acid from the key intermediate reaction residue of hexamethylenediamine, which can solve problems such as serious environment, production efficiency and product quality impact, residue solid waste, etc. Achieve the effects of reducing pollution, less side reactions, and reducing the discharge of three wastes

Active Publication Date: 2020-09-08
JIANGSU YANGNONG CHEM GROUP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the caprolactam ammonification process, a small amount of free caprolactam and aminocapronitrile will polymerize to form a polymer during the reaction and post-treatment process, and finally form a solid waste residue, which is serious to the environment and also affects production efficiency and product quality.

Method used

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  • Method for recycling hexanediamine key intermediate reaction residues and co-producing carboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of hexamethylenediamine key intermediate reaction residue of the present invention recycles and utilizes the method for co-producing carboxylic acid, comprises the steps:

[0032] (1) Continuously pump the residue and water into the first fixed-bed reactor simultaneously with a high-pressure pump to carry out the depolymerization reaction; wherein, the mass ratio of the residue to water is 0.1; the first fixed-bed reactor The inner diameter is 10mm and the length is 1000mm; in the first fixed bed reactor, the reaction temperature is 150°C, the reaction pressure is normal pressure, and 50g of BF 3 / Al 2 o 3 Solid catalyst, the total raw material space velocity is 20h -1 The residue and water are all imported from the lower end of the first fixed bed reactor, and the depolymerization reaction liquid material obtained after the depolymerization reaction is output from the upper end of the first fixed bed reactor; the first fixed bed reaction The feed and discharg...

Embodiment 2

[0038] A kind of hexamethylenediamine key intermediate reaction residue of the present invention recycles and utilizes the method for co-producing carboxylic acid, comprises the steps:

[0039] (1) Continuously pump the residue and water into the first fixed-bed reactor simultaneously with a high-pressure pump to carry out the depolymerization reaction; wherein, the mass ratio of the residue to water is 0.5; the first fixed-bed reactor The inner diameter is 10mm and the length is 1000mm; in the first fixed bed reactor, the reaction temperature is 200°C, the reaction pressure is 1MPa, and 50g of SiO 2 Solid catalyst, the total raw material space velocity is 5h -1 The residue and water are all imported from the lower end of the first fixed bed reactor, and the depolymerization reaction liquid material obtained after the depolymerization reaction is output from the upper end of the first fixed bed reactor; the first fixed bed reaction The feed and discharge of the device are kep...

Embodiment 3

[0045] A kind of hexamethylenediamine key intermediate reaction residue of the present invention recycles and utilizes the method for co-producing carboxylic acid, comprises the steps:

[0046] (1) Continuously pump the residue and water into the first fixed-bed reactor simultaneously with a high-pressure pump to carry out the depolymerization reaction; wherein, the mass ratio of the residue to water is 0.25; the first fixed-bed reactor The inner diameter is 10mm and the length is 1000mm; in the first fixed bed reactor, the reaction temperature is 250°C, the reaction pressure is 6MPa, and 50g of SiO 2 -Al 2 o 3 Solid catalyst, the total raw material space velocity is 10h -1 The residue and water are all imported from the lower end of the first fixed bed reactor, and the depolymerization reaction liquid material obtained after the depolymerization reaction is output from the upper end of the first fixed bed reactor; the first fixed bed reaction The feed and discharge of the ...

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Abstract

The invention relates to a method for recycling hexanediamine key intermediate reaction residues and co-producing carboxylic acid. The method comprises the following steps: introducing residues and water into a first fixed bed reactor, and carrying out a depolymerization reaction; carrying out heat exchange on the obtained depolymerization reaction liquid, then introducing into a second fixed bedreactor, and carrying out a hydrolysis reaction; carrying out a hydrogenation reaction on the obtained hydrolysis reaction solution, carrying out negative pressure distillation on the obtained hydrogenation reaction solution after the reaction is finished, and removing water to obtain a concentrated solution; and carrying out negative pressure rectification on the obtained concentrated solution, and collecting fractions at different gas phase temperatures to obtain corresponding products of aminocaproic acid, n-valeric acid and n-caproic acid. According to the invention, the method effectivelysolves the problem of key intermediate reaction residue pollution generally existing in existing hexanediamine production, realizes recovery and resource utilization of the key intermediate reactionresidue of hexanediamine, obtains a high-added-value product, reduces the production cost, increases the economic benefit, reduces the emission of three wastes, substantially reduces the pollution tothe environment and provides a guarantee for green and safe production.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a method for recycling the reaction residue of a key intermediate of hexamethylenediamine and co-producing carboxylic acid. Background technique [0002] Hexamethylenediamine has a wide range of uses and is a very important organic raw material in the field of chemical production. For example, hexamethylenediamine is used to manufacture nylon 66 salt. Nylon 66 is the earliest polyamide to achieve industrialization. It is listed as the two most important polyamides with nylon 6. Large polyamide material category; another example, the application of hexamethylenediamine in the field of polyamide has been developed and expanded, and has been able to successfully manufacture products such as nylon 610 and nylon 612. At the same time, polyimide carboxylate foam, polyurethane foam Plastics, coatings, epoxy resin curing agents, organic crosslinking agents, pesticides, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/08C07C227/40C07C227/00C07C51/00C07C53/126C07C51/44
CPCC07C227/40C07C227/00C07C51/00C07C51/44C07C229/08C07C53/126
Inventor 王刚聂庆超王根林丁克鸿徐林汪洋殷剑虎陈耀坤李良善何成义
Owner JIANGSU YANGNONG CHEM GROUP
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