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Caprolactam preparation method

A technology of caprolactam and cyclohexanone, which is applied in the field of organic chemical raw material production, can solve the problems of industrial application limitations, difficulty in meeting industrial requirements, and high production costs, and achieve the goals of shortening the production process, reducing ammonium sulfate by-products, and reducing energy consumption Effect

Inactive Publication Date: 2015-09-16
河北美邦工程科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ionic liquid and acetic anhydride used in this method are expensive, the production cost is high, and the selectivity of caprolactam is low, so it is difficult to meet the industrial requirements.
In summary, although the conversion rate of cyclohexanone oxime and the selectivity of caprolactam in some patents are high, and the output of by-product ammonium sulfate is low, its industrial application is limited due to economic, quality and process reasons.

Method used

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  • Caprolactam preparation method

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Experimental program
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Effect test

Embodiment 1

[0028] (1) In the catalytic oximation reaction unit, cyclohexanone, hydrogen peroxide, ammonia and the formed TS-1 catalyst are continuously added from the corresponding feed nozzles of the microreactor in the order of feed inlets from top to bottom, and continuous Catalyzed oximation reaction to obtain cyclohexanone oxime solution;

[0029] Among them, the particle size of the formed TS-1 catalyst used is 0.1 μm; the molar ratio of hydrogen peroxide and cyclohexanone is 1.0; the molar ratio of ammonia and cyclohexanone is 1.0; the mass fraction of hydrogen peroxide is 15%; the catalytic oximation reaction temperature is 70°C; the pressure is 200KPa (gauge pressure); the circulation volume of the circulating fluid is 600m3 / h; the mass fraction of the catalyst in the circulating fluid is 3.0%.

[0030] (2) In the extraction and separation unit, add solvent A to the cyclohexanone oxime solution obtained in step (1) and carry out extraction and separation, obtain the A solution o...

Embodiment 2

[0044] (1) In the catalytic oximation reaction unit, the raw powder after cyclohexanone, hydrogen peroxide, ammonia and TS-1 molecular sieve have changed the hydrophilicity is fed from the corresponding feeding ports of the microreactor in the order from top to bottom. The nozzle is continuously added, and the continuous catalytic oximation reaction is carried out to obtain the cyclohexanone oxime solution;

[0045] Among them, the particle size of the original powder after the TS-1 molecular sieve is used to change the hydrophilicity is 1.0 μm; the molar ratio of hydrogen peroxide and cyclohexanone is 1.1; the molar ratio of ammonia and cyclohexanone is 1.2; the concentration of hydrogen peroxide is 20% (wt %); the catalytic oximation reaction temperature is 80°C; the pressure is 250KPa (gauge pressure); the circulation volume of the circulating fluid is 700m3 / h; the catalyst concentration in the circulating fluid is 2.7% (wt%).

[0046] (2) In the extraction and separation u...

Embodiment 3

[0060] (1) In the catalytic oximation reaction unit, cyclohexanone, hydrogen peroxide, ammonia and the formed TS-1 catalyst are continuously added from the corresponding feed nozzles of the microreactor in the order of feed inlets from top to bottom, and continuous Catalytic oximation reaction obtains cyclohexanone oxime solution;

[0061] Among them, the particle size of the formed TS-1 catalyst used is 5.0 μm; the molar ratio of hydrogen peroxide to cyclohexanone is 1.2; the molar ratio of ammonia to cyclohexanone is 1.3; the concentration of hydrogen peroxide is 25% (wt%); The temperature is 85°C; the pressure is 300KPa (gauge pressure); the circulation volume of the circulating fluid is 800m3 / h; the catalyst concentration in the circulating fluid is 2.5% (wt%).

[0062] (2) In the extraction and separation unit, add solvent A to the cyclohexanone oxime solution obtained in step (1) and carry out extraction and separation, obtain the A solution of the organic phase cyclohex...

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Abstract

The invention discloses a caprolactam preparation method. The method is characterized in that caprolactam is prepared from cyclohexanone through oximation and rearrangement, and the method comprises the following steps: carrying out a catalytic reaction on cyclohexanone, hydrogen peroxide and ammonia to generate cyclohexanone oxime, extracting and separating by using a solvent A, adding a solvent B to the above obtained oil phase, carrying out a Beckmann rearrangement reaction under the action of oleum, carrying out slaking flash evaporation separation on the obtained product, hydrolyzing, extracting by using water, and carrying out original process refining to prepare finished caprolactam. The method shortens the caprolactam production process flow, reduces the consumption of raw materials and energy, generates less ammonium sulfate than original technologies, and improves the quality of the caprolactam product.

Description

technical field [0001] The invention relates to a method for preparing organic compounds, in particular to a method for preparing caprolactam, and belongs to the technical field of organic chemical raw material production. Background technique [0002] Caprolactam is an important chemical raw material for synthetic fibers and engineering plastics. About 90% of caprolactam in the world is prepared from cyclohexanone oxime through Beckmann rearrangement reaction. The traditional Beckmann rearrangement reaction process is: using oleum to form caprolactam sulfate from cyclohexanone oxime. In order to obtain a high yield of caprolactam, it is necessary to add excess oleum, and then neutralize the mixture with ammonia water to obtain caprolactam and ammonium sulfate. In a typical industrial rearrangement process, the conversion of cyclohexanone oxime is almost 100%, the selectivity to caprolactam is 99%, and 1.3-1.8 kg ammonium sulfate / kg cyclohexanone oxime is produced. This tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/10C07D201/04
CPCC07D223/10C07D201/04
Inventor 张玉新
Owner 河北美邦工程科技股份有限公司
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