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A kind of method utilizing microreactor to prepare caprolactam by α-amino-ε-caprolactam

A technology of caprolactam and micro-reactor, applied in the field of chemical synthesis and technology, to achieve the effects of easy disassembly, cost reduction, and large industrial application potential

Active Publication Date: 2016-08-17
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a method for preparing caprolactam from α-amino-ε-caprolactam using a microreactor in view of the cost and resource problems currently faced by caprolactam

Method used

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  • A kind of method utilizing microreactor to prepare caprolactam by α-amino-ε-caprolactam

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] according to figure 1 The flow chart, the α-amino-ε-caprolactam lye (wherein, alkali is potassium hydroxide, concentration is 2wt%) and the hydroxylamine-O-sulfonic acid solution that concentration is 6wt% as mobile phase respectively with concentration is 2wt% Pump into the mixer to mix, control the flow rate to keep the pH at 10, and the molar ratio of α-amino-ε-caprolactam to hydroxylamine-O-sulfonic acid to potassium hydroxide is 1:2:4. The material passes through the 0°C low-temperature reactor with a residence time of 10 minutes, and directly flows into the 90°C high-temperature reactor with a residence time of 10 minutes. After the completion, the materials were concentrated, extracted with dichloromethane, and the organic extracts were combined, and the solvent was distilled off under reduced pressure to obtain the product caprolactam, with a yield of 80% and a selectivity of 94%.

Embodiment 2

[0025] according to figure 1 The flow chart, the concentration is the α-amino-ε-caprolactam lye (wherein, alkali is potassium hydroxide, concentration is 3wt%) and the concentration is the hydroxylamine-O-sulfonic acid solution of 3wt% as mobile phase respectively with the concentration of 1wt% Pump into the mixer to mix, control the flow rate to keep the pH at 10, and the molar ratio of α-amino-ε-caprolactam to hydroxylamine-O-sulfonic acid to potassium hydroxide is 1:2.5:5. The material passes through the 0°C low-temperature reactor with a residence time of 15 minutes, and directly flows into the 90°C high-temperature reactor with a residence time of 10 minutes. After the completion, the materials were concentrated, extracted with dichloromethane, and the organic extracts were combined, and the solvent was distilled off under reduced pressure to obtain the product caprolactam, with a yield of 85% and a selectivity of 91%.

Embodiment 3

[0027] according to figure 1The flow chart, the α-amino-ε-caprolactam lye (wherein, alkali is potassium hydroxide, concentration is 2wt%) and the hydroxylamine-O-sulfonic acid solution that concentration is 6wt% as mobile phase respectively with concentration is 2wt% Pump into the mixer for mixing, control the flow rate to keep the pH at 12, and the molar ratio of α-amino-ε-caprolactam to hydroxylamine-O-sulfonic acid to potassium hydroxide is 1:2:4. The material passes through the -5°C low-temperature reactor with a residence time of 5 minutes, and directly flows into the 95°C high-temperature reactor with a residence time of 10 minutes. After the completion, the materials were concentrated, extracted with ethyl acetate, and the organic extracts were combined, and the solvent was distilled off under reduced pressure to obtain the product caprolactam, with a yield of 81% and a selectivity of 90%.

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Abstract

The invention discloses a method for preparing caprolactam from alpha-amino-epsilon-caprolactam by utilizing a microreactor. The method comprises the following steps: dissolving the alpha-amino-epsilon-caprolactam and potassium hydroxide in water to obtain a solution (a); dissolving hydroxylamine-O-sulphonic acid in water to obtain a solution (b); simultaneously pumping the solution (a) and the solution (b) into a micro-channel modular reaction device respectively, staying in a low-temperature micro-structure reactor for 2 to 15 minutes under the conditions that the temperature is -5 to 5 DEG C and the pH value is 8 to 12; introducing the material discharged from the low-temperature micro-structure reactor into a high-temperature micro-structure reactor, staying for 2 to 15 minutes under 90 to 100 DEG C, concentrating a reaction product, leading the concentrated reaction product into a separating device, adding an organic solvent for extracting, mixing the obtained organic extract liquid, performing reduced pressure distillation for removing a solvent, and obtaining the final product, namely the caprolactam. According to the method disclosed by the invention, a preparation process is easy to operate and control, so that the method has enlarged industrial potential.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and technology, in particular to a method for preparing caprolactam from α-amino-ε-caprolactam in a microchannel reactor. Background technique [0002] Caprolactam (CPL) is an important organic chemical raw material, more than 98% is used in the production of nylon 6 fiber and nylon 6 engineering plastics, used in the manufacture of gears, bearings, pipes, medical equipment and electrical, insulating materials, etc.; also used in coatings, plastics Agent and a small amount for the synthesis of lysine and so on. Caprolactam can also be used to prepare caprolactam resin, fiber and artificial leather, etc., and is also used as a raw material for medicine. [0003] In recent years, China's caprolactam industry has developed rapidly, and the domestic caprolactam production capacity exceeded 2 million tons per year by the end of 2014. The substantial expansion of production capacity has all...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/10C07D201/02
CPCC07D201/02C07D223/10
Inventor 郭凯方正曾文波朱宁欧阳平凯
Owner NANJING TECH UNIV
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