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Method and equipment for continuously producing epsilon-caprolactam

A technology of caprolactam and cyclohexanone oxime, applied in the field of continuous production of ε-caprolactam and equipment, can solve the problem of energy consumption in the distillation area

Active Publication Date: 2014-07-02
CAP III
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The disadvantage of the prior art method is that a lot of energy is spent in the distillation zone

Method used

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  • Method and equipment for continuously producing epsilon-caprolactam
  • Method and equipment for continuously producing epsilon-caprolactam
  • Method and equipment for continuously producing epsilon-caprolactam

Examples

Experimental program
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Effect test

Embodiment 1

[0067] use Figure 4 the device. The heat generated in the first stage of the Beckmann rearrangement reaction zone was used as an energy source for the separation of a mixture containing ε-caprolactam and benzene in a two-step distillation process.

[0068] Cyclohexanone oxime was added to the tertiary Beckmann rearrangement reaction zone. 19 ton / hr cyclohexanone oxime was fed to the first stage mixture plant [K] via line [102]. Input 25 ton / hr oleum (sulfuric acid and SO 3 ). The heat removed from the ε-caprolactam-containing mixture in the in-process heat exchanger [N] was about 13 MW. The temperature of the ε-caprolactam-containing mixture entering the in-process heat exchanger [N] was 96°C and the temperature of the ε-caprolactam-containing mixture leaving the in-process heat exchanger [N] was 75°C.

[0069] The third-stage ε-caprolactam-containing mixture leaving the Beckmann rearrangement reaction zone was neutralized with aqueous ammonia, thereby obtaining a two-ph...

Embodiment 2

[0080] use image 3 Said plant, where the only difference is that the feed to the distillation column, a 148 ton / hr benzene mixture containing 18.3 wt.% ε-caprolactam, is not fed into line [208] but is fed from the distillation column [P] The top of the column is added to the theoretical plate 4 ( image 3 not shown). The heat generated in the first stage of the Beckmann rearrangement reaction zone was used as an energy source for the separation of a mixture containing ε-caprolactam and benzene in a one-step distillation process.

[0081] Cyclohexanone oxime was added to the tertiary Beckmann rearrangement reaction zone. Input 19 ton / hr cyclohexanone oxime via line [102] phase first stage mixing device [K]. Input 25 ton / hr oleum (sulfuric acid and SO 3 ). The heat removed from the ε-caprolactam-containing mixture in the in-process heat exchanger [N] was about 13 MW. The temperature of the ε-caprolactam-containing mixture entering the in-process heat exchanger [N] was 96°...

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Abstract

The invention provides a method and equipment for continuously producing epsilon-caprolactam. The method orderly comprises the following steps: a) inputting i) fuming sulphuric acid and / or ii) cyclohexanone-oxime into a beckmann rearrangement reaction zone; b) discharging the generated mixture containing epsilon-caprolactam from the beckmann rearrangement reaction zone; c) adding ammonia to the mixture containing the epsilon-caprolactam; d) separating out ammonium sulfate from the mixture containing the epsilon-caprolactam; e) extracting the epsilon-caprolactam from the mixture containing the epsilon-caprolactam in an organic solvent; and f) adding water to remove an organic solvent from the extracted epsilon-caprolactam in a distillation zone by using distillation. The method is characterized in that at least one part of reaction heat generated in the beckmann rearrangement reaction zone is exchanged to the distillation zone. The invention also provides equipment for executing the method and the epsilon-caprolactam obtained according to the method.

Description

technical field [0001] The present invention relates to a process for the production of ε-caprolactam and its recovery from organic solutions in an energy-efficient manner. Background technique [0002] In the process for preparing ε-caprolactam, it is generally necessary to recover ε-caprolactam from a solution containing ε-caprolactam dissolved in an organic solvent in which cyclohexanone oxime is converted to ε-caprolactam by means of an acid. Such transformations are known as Beckmann rearrangements. Beckmann rearrangement reactions are highly exothermic reactions, and thus are usually governed by cooling systems. After the rearrangement reaction has occurred, a base, preferably ammonia, can be added to the Beckmann rearrangement mixture to produce a neutralized Beckmann rearrangement mixture. The ammonium sulfate is removed and the remaining ε-caprolactam is extracted in an organic solvent. Organic solvents must be removed by distillation. The purpose is that in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/10C07D201/04C01C1/242
CPCC01C1/242C07D201/04C07D223/10
Inventor 约翰·托马斯·廷格迈克尔·威廉颂·玛丽亚·博伊斯坦迈斯·约翰内斯·赛姆林克
Owner CAP III
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