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Preparation method of 6-aminocaproic acid

A technology of aminocaproic acid and caprolactam, which is applied in the chemical industry, can solve the problems of unresolved treatment difficulties and no proposed treatment methods for mixed waste liquid, and achieve the effects of cost saving and high purity

Pending Publication Date: 2022-03-18
昌德新材科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the concentrated solution is produced during the polymerization of caprolactam, and does not solve the technical problem of the difficult treatment of waste liquids such as benzene extraction waste liquid and separation waste liquid produced in the caprolactam production process.
[0005] Chinese patent document CN101857550A discloses a method for producing 6-aminocaproic acid salt and 6-aminocaproic acid by depolymerizing nylon-6 waste, but this method is aimed at already formed nylon-6 waste, and it is not suitable for containing caprolactam There is no corresponding treatment method for the mixed waste liquid of monomers and their oligomers

Method used

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preparation example Construction

[0025] The present disclosure provides a preparation method of 6-aminocaproic acid, the method comprising:

[0026] S1. Dehydrating the waste liquid of caprolactam produced by the rearrangement method for the first time and performing high-temperature polymerization to obtain a polymer; adding an acidic solution to the polymer and performing reflux depolymerization to obtain the first product;

[0027] S2. Dehydrating the first product under reduced pressure and adding it to an alcoholic solvent for dissolution to obtain a second product; performing a first filtration on the second product to obtain a first filtrate;

[0028] S3. Adding an organic amine or introducing ammonia into the first filtrate, adjusting the pH of the first filtrate to 7-8, and then performing a second filtration to obtain crude 6-aminocaproic acid;

[0029] Wherein, the waste liquid of caprolactam produced by the rearrangement method is at least one selected from the waste liquid of caprolactam produced...

Embodiment 1

[0046] Take 200g caprolactam waste liquid and carry out dehydration treatment, the total weight of caprolactam waste liquid after dehydration is 82g, and water content is 2.4% by weight; High polymer is obtained by high temperature polymerizing the caprolactam waste liquid after dehydration, wherein the condition of high temperature polymerization is: The temperature was raised to 240°C at a heating rate of 5°C / s and then polymerized for 2 hours. 82 g of water and 49.2 g of concentrated sulfuric acid were added to the obtained polymer, and refluxed at 110° C. for 8 hours to obtain the first product.

[0047] The first product was dehydrated under reduced pressure and added to 240 mL of ethanol for dissolution to obtain the second product, and the second product was subjected to the first filtration to obtain the first filtrate. Wherein, the conditions of dehydration under reduced pressure are: the pressure is -0.1MPa, the temperature is 50°C, and the time is 5h. The water con...

Embodiment 2

[0050] Take 100g caprolactam waste liquid and carry out dehydration treatment, the total weight of the caprolactam waste liquid after dehydration is 42g, and water content is 4.8% by weight; The caprolactam waste liquid after dehydration is subjected to high-temperature polymerization to obtain high polymer, wherein the condition of high-temperature polymerization is: The temperature was raised to 230°C at a heating rate of 8°C / s and then polymerized for 6 hours. Add 42 g of water and 20 g of acetic acid to the obtained polymer, and reflux depolymerization at 110° C. for 6 hours to obtain the first product.

[0051] After the first product was dehydrated under reduced pressure, it was added to 120 mL of acetone for dissolution to obtain the second product, and the second product was subjected to the first filtration to obtain the first filtrate. Wherein, the conditions of dehydration under reduced pressure are: the pressure is -0.2MPa, the temperature is 40°C, and the time is ...

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Abstract

The invention relates to a 6-aminocaproic acid preparation method, which comprises: S1, carrying out first dehydration on caprolactam waste liquid, and carrying out high temperature polymerization to obtain a polymer; adding an acid solution into the polymer, and carrying out reflux depolymerization to obtain a first product; s2, dehydrating the first product under reduced pressure, and adding the dehydrated first product into an alcohol solvent for dissolving to obtain a second product; performing first filtration on the second product to obtain first filtrate; and S3, adding organic amine or introducing ammonia gas into the first filtrate, adjusting the pH value of the first filtrate to 7-8, and carrying out second filtration to obtain crude 6-aminocaproic acid. According to the method disclosed by the invention, the cost of directly treating the caprolactam waste liquid as wastewater is saved, effective substances in the caprolactam waste liquid can be extracted, and aminocaproic acid is synthesized.

Description

technical field [0001] The disclosure relates to the field of chemical technology, in particular to a method for separating and preparing 6-aminocaproic acid by using the waste liquid of caprolactam produced by the rearrangement method as a raw material. Background technique [0002] At present, there are two general treatment methods for caprolactam waste liquid in industry: one is to increase the mass fraction of organic matter and salt in the waste liquid to 40%-70%, and then carry out spray combustion under the condition of 900°C; Biochemical systems are used to reduce the organic matter content in wastewater. However, these two traditional treatment methods have disadvantages such as high energy consumption, high operating costs, high ammonia content in the discharged wastewater, and no recycling of valuable components in the waste liquid. [0003] Aminocaproic acid is used as a hemostatic agent in the medical field. It has obvious effects on some severe bleeding cause...

Claims

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Application Information

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IPC IPC(8): C07C227/20C07C229/08C08G69/08C08G69/14
CPCC07C227/20C08G69/08C08G69/14C07C229/08
Inventor 杨浴刘文瑞杜立秋蒋卫和屈铠甲易伟
Owner 昌德新材科技股份有限公司
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