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Caprolactam refining method and system

A technology of caprolactam and refining method, which is applied in the field of chemical refining, and can solve the problems of complex process control, long process flow, and shortened life of ion exchange resins, etc.

Active Publication Date: 2018-01-09
沧州旭阳化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the refining of amide oil for preparation of caprolactam by liquid-phase Beckmann rearrangement of cyclohexanone oxime is mainly through benzene extraction, water stripping, ion exchange, hydrogenation, evaporation and distillation related process operations. The process flow is long and the process control is complicated. More equipment is required, which not only increases energy consumption and material consumption, but also shortens the life of the ion exchange resin with the increase of production time, increases the regeneration frequency of the ion exchange resin, produces a large amount of industrial wastewater, and brings a certain burden to water treatment.

Method used

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  • Caprolactam refining method and system

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Experimental program
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Effect test

Embodiment 1

[0026] The benzene ethyl alcohol liquid formed after the amide oil is extracted by benzene is washed with 0.2wt% NaOH to remove the alkali-soluble substances, ammonium sulfate and esters and other impurities; The debenzene tower removes the benzene solvent therein, and its operating conditions are tower top temperature 70°C, tower bottom temperature 100°C, tower top pressure 90kpaA, tower bottom pressure 100kpaA; then enter the light removal tower to remove light component impurities therein, The condition is that the temperature at the top of the tower is 80°C, the temperature at the bottom of the tower is 100°C, the pressure at the top of the tower is 0.1kpaA, and the pressure at the bottom of the tower is 0.3kpaA; finally, it enters the weight removal tower to remove the heavy component impurities. The temperature at the bottom is 100°C, the pressure at the top of the tower is 0.1kpaA, and the pressure at the bottom of the tower is 0.7kpaA, and the caprolactam that meets the...

Embodiment 2

[0028] The benzene ethyl alcohol liquid formed after the amide oil is extracted by benzene is subjected to alkali washing with 5wt% NaOH to remove impurities such as alkali-soluble substances, ammonium sulfate and esters therein; The benzene tower removes the benzene solvent therein, and its operating conditions are tower top temperature 100°C, tower bottom temperature 150°C, tower top pressure 120kpaA, tower bottom pressure 120kpaA; The condition is that the temperature at the top of the tower is 120°C, the temperature at the bottom of the tower is 140°C, the pressure at the top of the tower is 0.5kpaA, and the pressure at the bottom of the tower is 1.0kpaA; finally, it enters the deweighting tower to remove the heavy component impurities. The temperature is 140°C, the pressure at the top of the tower is 0.6kpaA, and the pressure at the bottom of the tower is 1.2kpaA, and the caprolactam that meets the national standard GBT13254-2008 is obtained.

Embodiment 3

[0030] The benzene ethyl alcohol liquid formed after the amide oil is extracted by benzene is subjected to alkali washing with 2.6wt% NaOH to remove impurities such as alkali-soluble substances, ammonium sulfate and esters; The debenzene tower removes the benzene solvent therein, and its operating conditions are tower top temperature 85°C, tower bottom temperature 125°C, tower top pressure 105kpaA, tower bottom pressure 110kpaA; then enter the light removal tower to remove the light component impurities therein, The condition is that the temperature at the top of the tower is 100°C, the temperature at the bottom of the tower is 120°C, the pressure at the top of the tower is 0.3kpaA, and the pressure at the bottom of the tower is 0.65kpaA. The temperature at the bottom is 120°C, the pressure at the top of the tower is 0.35kpaA, and the pressure at the bottom of the tower is 0.95kpaA, and the caprolactam that meets the national standard GBT13254-2008 is obtained.

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Abstract

The invention relates to a caprolactam refining method. The method comprises the steps as follows: 1) amide oil enters a benzene extraction tower, and benzene is used as an extraction agent to extractcaprolactam in the amide oil; 2) a benzene-caprolactam solution obtained after extraction is subjected to alkali washing and water washing for removal of alkali-soluble and water-soluble substances;3) a product in the step 2) sequentially passes through a benzene removal tower, a light component removal tower and a heavy component removal tower, wherein the benzene removal tower removes a benzene solvent, the light component removal tower removes light component impurities, the heavy component removal removes heavy component impurities, and refined caprolactam is obtained. The invention alsorelates to a caprolactam refining system.

Description

technical field [0001] The invention belongs to the technical field of chemical refining, in particular to a method for refining caprolactam and a system for refining caprolactam. Background technique [0002] Caprolactam is an important chemical raw material in the field of synthetic fibers and engineering plastics. When it is used as a raw material for the polymerization of nylon 6, its quality requirements are very strict. Especially the presence of some impurities in caprolactam, although the content is very small, has a great impact on the quality of caprolactam finished products, and will also seriously affect the quality of synthetic fibers. For example, reducing impurities contained in caprolactam such as aniline, ketoxime, furan, phenazine, and alcohols can lead to a decrease in the PM value and stability of caprolactam; impurities with chromogenic groups such as aromatic amines can cause caprolactam to deteriorate. The color chroma increases, and the transparency ...

Claims

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Application Information

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IPC IPC(8): C07D223/10C07D201/16
Inventor 刘怡宏邢亚峰刘冬然赵朋伟石峰陈西波
Owner 沧州旭阳化工有限公司
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