Method for preparing 6-aminocaproic acid

An aminocaproic acid and benchmark technology, applied in the chemical industry, can solve problems such as the inability to apply caprolactam waste liquid, and achieve the effect of solving adverse effects and high purity

Pending Publication Date: 2022-03-11
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

[0004] Chinese patent document CN109369430A provides a method for preparing 6-aminocaproic acid, but the raw material of this method is a mixed solution prepared by dissolving pure caprolactam in an acidic aqueous solution, which cannot be applied to caprolactam with complex components produced in industry waste liquid

Method used

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preparation example Construction

[0032] The preparation method of 6-aminocaproic acid in the present disclosure can extract the effective substances in the waste liquid of caprolactam produced by the rearrangement method, and synthesize the substances into 6-aminocaproic acid. Specifically, in the present disclosure, organic acid is added to the waste liquid of caprolactam produced by the rearrangement method, and the reflux reaction is carried out to convert the caprolactam, aminocaproic acid and caprolactam oligomers in the waste liquid into aminocaproic acid acetate; the first product After dehydration under reduced pressure, add it to an alcohol solvent for dissolution and filter to obtain the first filtrate, which can remove ammonium sulfate in the system, and the first filtrate is mainly the alcohol solution of aminocaproic acid acetate; add the first filtrate to Organic amine or ammonia gas is introduced to adjust the pH to 7-8, and the crude aminocaproic acid is obtained by filtration. The disclosed m...

Embodiment 1

[0048] Take 200g of caprolactam waste liquid, add 35mL of formic acid to carry out reflux reaction to obtain the first product; then dehydrate the first product to near dryness under reduced pressure, and then add 160mL of ethanol to dissolve it to obtain the second product; filter the second product to obtain ammonium sulfate, etc. Inorganic salts and first filtrate. Slowly add 20 g of triethylamine to the first filtrate, and filter to obtain 20 g of crude aminocaproic acid.

[0049] Wherein, the conditions of the reflux reaction include: reacting at 100° C. for 8 hours under total reflux conditions; the conditions of dehydration under reduced pressure include: the pressure is -0.1 MPa, the temperature is 60° C., and the time is 4 hours.

Embodiment 2

[0051] Take 200g of caprolactam waste liquid, add 30mL of acetic acid to carry out reflux reaction to obtain the first product; then dehydrate the first product to near dryness under reduced pressure, and then add 300mL of methanol to dissolve it to obtain the second product; filter the second product to obtain ammonium sulfate, etc. Inorganic salts and first filtrate. Slowly add 30 g of ethylenediamine to the first filtrate, and filter to obtain 24 g of crude aminocaproic acid.

[0052] Wherein, the conditions of the reflux reaction include: reacting at 120° C. for 5 hours under total reflux conditions; the conditions of dehydration under reduced pressure include: the pressure is -0.2 MPa, the temperature is 55° C., and the time is 2 hours.

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Abstract

The invention relates to a method for preparing aminocaproic acid, which comprises the following steps: S1, adding organic acid into caprolactam waste liquid, and carrying out reflux reaction 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; s3, adding organic amine or introducing ammonia gas into the first filtrate, adjusting the pH value of the first filtrate to 7-8, and then carrying out second filtration to obtain crude aminocaproic acid; wherein the waste liquid of caprolactam prepared by the rearrangement method is selected from at least one of waste liquid of caprolactam prepared by a sulfuric acid liquid-phase rearrangement method and waste liquid of caprolactam prepared by a sulfuric acid gas-phase rearrangement method. According to the method, the problem of environmental pollution caused by the waste liquid is solved, valuable components are extracted and converted into the high-added-value product aminocaproic acid, and the adverse effect of hydrochloric acid serving as a catalyst on the product is solved.

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] As a fine chemical product, aminocaproic acid is widely used in the field of drug synthesis, and it is mainly used and sui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/08C07C227/22C07C227/16
CPCC07C227/22C07C227/16C07C229/08
Inventor 刘文瑞杨浴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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