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Subcritical catalytic hydrolysis MC nylon method for preparing caprolactam

A technology for catalytic hydrolysis and caprolactam, applied in the preparation of lactam, chemical instruments and methods, organic chemistry, etc., can solve problems such as corrosion equipment and separation difficulties, achieve recyclable recovery, improve degradation rate, and hydrothermal stability Good results

Active Publication Date: 2015-07-08
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention solves the technical problems of subsequent separation difficulties and corrosion equipment in traditional liquid catalysts, and provides a method for preparing caprolactam by subcritical catalytic hydrolysis of MC nylon

Method used

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  • Subcritical catalytic hydrolysis MC nylon method for preparing caprolactam
  • Subcritical catalytic hydrolysis MC nylon method for preparing caprolactam
  • Subcritical catalytic hydrolysis MC nylon method for preparing caprolactam

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specific Embodiment approach 1

[0018] Specific embodiment one: In this embodiment, a method for preparing caprolactam by subcritical catalytic hydrolysis of MC nylon is carried out according to the following steps:

[0019] 1. Roast the molecular sieve catalyst for 3-5 hours at a temperature of 500-600°C;

[0020] 2. Crush MC nylon, then wash with distilled water for 1-2 times, control the temperature at 50°C-70°C, and dry for 5-8h;

[0021] 3. Mix 0.1-0.6g of the molecular sieve catalyst roasted in step 1, 1.0g of MC nylon obtained in step 2 and distilled water, and add it into a stainless steel reaction kettle, seal it, wherein the solid-liquid ratio is 1g: (10-50)mL;

[0022] 4. Put the reaction kettle in step 3 into a salt bath with a temperature of 300-350° C., keep it for 20-50 minutes, and control the pressure in the kettle to be 7.0-10.0 MPa;

[0023] 5. Put the reaction kettle after the reaction in step 4 into an ice-water bath to cool to room temperature, then filter and separate the product, and...

specific Embodiment approach 2

[0024] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the calcination temperature in Step 1 is 550°C. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0025] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the roasting time in step 1 is 4 hours. Others are the same as in the first or second embodiment.

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Abstract

The invention discloses a subcritical catalytic hydrolysis MC nylon method for preparing caprolactam and relates to a method for preparing monomer caprolactam using an H-type molecular sieve to catalyze waste MC nylon to degrade in subcritical water. The subcritical catalytic hydrolysis MC nylon method for preparing the caprolactam aims at solving the technical problems that a traditional liquid catalyst is difficult in follow-up separation and capable of etching apparatus. The subcritical catalytic hydrolysis MC nylon method for preparing the caprolactam comprises the steps of 1, calcining molecular sieve based catalysts; 2, processing the MC nylon; 3, placing the MC nylon, the molecular sieve and the water in a reaction kettle; 4, performing subcritical conditional reaction; 5, separating and analyzing products. The H-type molecular sieve solid acid catalyst adopted by the subcritical catalytic hydrolysis MC nylon method for preparing the caprolactam can effectively replace liquid acid to catalyze the MC nylon to be hydrolyzed to prepare the caprolactam (CPL), meanwhile, the reaction time and temperature can be reduced, the reaction is gentler, and the yield of the target monomer CPL can reach 78.26%. The subcritical catalytic hydrolysis MC nylon method for preparing the caprolactam is used for subcritical catalytic hydrolysis MC nylon to prepare the caprolactam.

Description

technical field [0001] The invention relates to a method for preparing monomer caprolactam by using H-type molecular sieve to catalyze the degradation of waste MC nylon in subcritical water. Background technique [0002] Caprolactam (CPL) is an important organic chemical raw material with a wide range of uses, mainly used in the production of nylon 6 engineering plastics and nylon 6 fibers. At present, the recovery methods of caprolactam by degrading waste nylon mainly include thermal degradation and hydrolysis. The energy consumption of pyrolysis is large, the cost of the catalyst used is high, and the catalyst is easy to react with the impurities in the polymer to reduce the catalytic efficiency. [0003] Catalytic hydrolysis or super / subcritical hydrolysis using water as the degradation medium is more environmentally friendly, and there are more substances with small molecular weight in the product, and no environmentally harmful products are produced, which is the main ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/10C07D201/12
CPCC07D201/12C07D223/10
Inventor 孟令辉王巍黄玉东冷坤岳陈中武谢非
Owner HARBIN INST OF TECH
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