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Method for synthesizing caprolactam in one step by liquid phase hydrogenation of nitrocyclohexane

A nitrocyclohexane liquid and a technology for nitrocyclohexane are applied in the field of one-step synthesis of caprolactam by liquid-phase hydrogenation of nitrocyclohexane, can solve the problems of complicated method, a large amount of concentrated sulfuric acid, expensive separation of catalysts, etc. The effect of simplified process and mild reaction conditions

Inactive Publication Date: 2012-03-21
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that a large amount of concentrated sulfuric acid is required, and a large amount of waste water is generated to pollute the environment. The method is complicated and the cost is high.
[0006] US3523940 uses iron, nickel, cobalt, vanadium, molybdenum and other metal carbonyls as catalysts, and benzene as an inert solvent to carry out liquid phase synthesis reactions. The caprolactam yield of this method is very low, the catalyst is expensive and difficult to separate

Method used

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  • Method for synthesizing caprolactam in one step by liquid phase hydrogenation of nitrocyclohexane
  • Method for synthesizing caprolactam in one step by liquid phase hydrogenation of nitrocyclohexane
  • Method for synthesizing caprolactam in one step by liquid phase hydrogenation of nitrocyclohexane

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Experimental program
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Effect test

Embodiment 1

[0024] 1.84 g of 2,4,6-trichloro-1,3,5-triazine was dissolved in 10 ml of N,N-dimethylformamide, and the mixture was stirred at room temperature for a period of time and then added to the reaction kettle, Then add 1.29 grams of nitrocyclohexane and 0.2 grams of 5% Pd / C to the kettle, connect the reaction kettle to the hydrogen cylinder, check the airtightness, feed hydrogen and evacuate, repeat five times, to exhaust other gases as much as possible , and then reacted for 6h in an oil bath at 80°C under a hydrogen pressure of 0.2MPa. The reacted mixture was filtered, and the filtrate was analyzed by gas chromatography and the internal standard method. It was calculated that the conversion rate of nitrocyclohexane was 63.87%, and the selectivity of caprolactam was 15.43%.

Embodiment 2

[0026] 1.84 g of 2,4,6-trichloro-1,3,5-triazine was dissolved in 10 ml of N,N-dimethylformamide, and the mixture was stirred at room temperature for a period of time and then added to the reaction kettle, Then add 1.29 grams of nitrocyclohexane and 0.2 grams of 5% Pd / C to the kettle, connect the reaction kettle to the hydrogen cylinder, check the airtightness, feed hydrogen and evacuate, repeat five times, to exhaust other gases as much as possible , and then reacted for 6h in an oil bath at 110°C under a hydrogen pressure of 0.35MPa. The reacted mixture was filtered, and the filtrate was analyzed by gas chromatography and the internal standard method. It was calculated that the conversion rate of nitrocyclohexane was 77.31%, and the selectivity of caprolactam was 7.12%.

Embodiment 3

[0028] 1.84 g of 2,4,6-trichloro-1,3,5-triazine was dissolved in 10 ml of N,N-dimethylformamide, and the mixture was stirred at room temperature for a period of time and then added to the reaction kettle, Then add 1.29 grams of nitrocyclohexane and 0.1 gram of 15% Ni / C to the kettle, connect the reaction kettle to the hydrogen cylinder, check the airtightness, pass in hydrogen and evacuate, repeat five times, to exhaust other gases as much as possible , and then reacted for 6h in an oil bath at 80°C under a hydrogen pressure of 0.2MPa. The reacted mixture was filtered, and the filtrate was analyzed by gas chromatography and the internal standard method. It was calculated that the conversion rate of nitrocyclohexane was 92.35%, and the selectivity of caprolactam was 9.73%.

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Abstract

The invention provides a method for synthesizing caprolactam in one step by liquid phase hydrogenation of nitrocyclohexane, wherein caprolactam is synthesized in one step setting out from nitrocyclohexane and under the action of hydrogen pressure of 0.1-2.0MPa and a composite catalytic system; and the composite catalytic system is the supported catalyst and the mixture composed of triazine compounds and formamide compounds. The method of the invention has temperate reaction conditions and simplifies the technology substantially.

Description

technical field [0001] The invention relates to a method for synthesizing caprolactam in one step by liquid-phase hydrogenation of nitrocyclohexane. Background technique [0002] As a monomer of polyamide, caprolactam is an important petrochemical product and chemical fiber raw material, mainly used in the production of polycaprolactam fiber resin, nylon 6 fiber, nylon 6 fiber, plastics and films and other products. It is widely used in textiles, automobiles, electronics, machinery and other fields, and can also be used in the production of antiplatelet drugs such as 6-aminocaproic acid and laurocaprolactone. Among them, the demand for caprolactam for nylon 6 fiber accounts for about 65% of the total global demand, and the demand for resin and film accounts for 30%-35%. The demand for nylon 6 resin in economically developed regions such as Japan, Western Europe, and the United States is one of the main growth drivers for the caprolactam market demand. [0003] Caprolactam ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/10C07D201/02
Inventor 罗和安刘平乐谭仕荣游奎一艾秋红肖艳娟
Owner XIANGTAN UNIV
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