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Preparation method of 6-aminocaproic acid

A technology of aminocaproic acid and organic acid, which is applied in the field of preparation of 6-aminocaproic acid, can solve the problems of high energy consumption, cumbersome operation, unfavorable large-scale industrial production, etc., and achieve the effect of high content, simple purification and easy acquisition

Pending Publication Date: 2022-05-13
ZHUHAI UNITED LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to use dilute sulfuric acid to adjust the pH value, and adopts electrodialysis to carry out desalination treatment. The desalination treatment takes the sulfate radical content in the effluent as the end point of <100ppm, which has high energy consumption and cumbersome operation, which is not conducive to large-scale industrial production.

Method used

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  • Preparation method of 6-aminocaproic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A kind of preparation method of 6-aminocaproic acid

[0038] Mix 100g of caprolactam (0.88mol), 73.9g of potassium hydroxide (1.32mol) and 266g of water evenly, raise the temperature to 90°C, and react for 3h. Cool to 25°C, neutralize with 79.2g acetic acid (1.32mol), concentrate to dryness, add 598g ethanol, stir at 50°C for 4h, grow crystals at 0°C for 2h, filter to obtain a crude product. Add 59g of water to the crude product, heat until the crude product dissolves, add 467g of ethanol, grow crystals at 0°C for 2 hours, filter, and dry to obtain 89.5g of 6-aminocaproic acid with a purity of 99.8%, a content of 99.7%, and a mass yield of 89.5%. The theoretical yield is 115.4g, and the converted yield is 77.4%.

Embodiment 2

[0040] A kind of preparation method of 6-aminocaproic acid

[0041] Mix 100g of caprolactam (0.88mol), 147.8g of potassium hydroxide (2.64mol) and 266g of water evenly, raise the temperature to 120°C, and react for 1h. Cool to 25°C, neutralize with 195.4g propionic acid (2.64mol), concentrate to dryness, add 620g isopropanol, stir at 20°C for 4h, grow crystals at 5°C for 2h, filter to obtain a crude product. Add 59g of water to the crude product, heat until the crude product dissolves, add 480g of isopropanol, grow crystals at 5°C for 2h, filter, and dry to obtain 90.0g of 6-aminocaproic acid with a purity of 99.8%, a content of 99.7%, and a mass yield of 90.0 %. The theoretical yield is 115.4g, and the converted yield is 77.8%.

Embodiment 3

[0043] A kind of preparation method of 6-aminocaproic acid

[0044] Mix 100g of caprolactam (0.88mol), 147.8g of potassium hydroxide (2.64mol) and 500g of water evenly, raise the temperature to 105°C, and react for 6h. Cool to 25°C, neutralize with 380.7g isooctanoic acid (2.64mol), concentrate to dryness, add 580g n-propanol, stir at 80°C for 4h, grow crystals at 3°C ​​for 2h, filter to obtain a crude product. Add 59g of water to the crude product, heat until the crude product dissolves, add 480g of n-propanol, grow crystals at 3°C ​​for 2h, filter, and dry to obtain 90.2g of 6-aminocaproic acid with a purity of 99.8%, a content of 100.0%, and a mass yield of 90.2 %. The theoretical yield is 115.4g, and the converted yield is 78.2%.

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Abstract

The invention relates to the field of organic synthesis, in particular to a preparation method of 6-aminocaproic acid. The method comprises the following steps: hydrolyzing caprolactam by using potassium salt as alkali to obtain 6-aminocaproic acid potassium salt, acidifying by using organic acid to obtain 6-aminocaproic acid and organic potassium salt, and finally recrystallizing by using the solubility difference of the organic potassium salt and 6-aminocaproic acid in an alcohol solvent to obtain high-purity, high-content and high-stability 6-aminocaproic acid. The preparation method does not need special equipment, is simple to operate, reduces the production cost, and is easy for industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of 6-aminocaproic acid. Background technique [0002] 6-Aminocaproic acid is often used in the synthesis of functional materials, and it is also the raw material for two drugs, zinc acexacaproate and neriphosphonate. It is also used for hemoptysis, gastrointestinal bleeding, and obstetrics and gynecological hemorrhagic diseases. Early medication or preoperative medication in internal and surgical operations can reduce bleeding during operations and reduce blood transfusions. quantity. [0003] 6-aminocaproic acid mostly uses caprolactam as the starting material, which is hydrolyzed to generate 6-aminocaproic acid. [0004] Patent CN101125821A discloses a method of hydrolyzing caprolactam with hydrochloric acid, replacing and refining with ion exchange resin to obtain aminocaproic acid. This method requires the regeneration of acid and alkali aqueous soluti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/22C07C227/40C07C227/42C07C229/08
CPCC07C227/22C07C227/40C07C227/42C07C229/08
Inventor 黄颜炯邓培玲李冰刘义乔明福韩玉波
Owner ZHUHAI UNITED LAB
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