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Production of epsilon-caprolactam

A kind of technology of caprolactam and cyclohexanone oxime, which is applied in the field of preparation of ε-caprolactam

Inactive Publication Date: 2007-01-17
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, gas-phase Beckmann rearrangement and liquid-phase rearrangement prepare ε-caprolactam by-product other organic impurities.

Method used

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  • Production of epsilon-caprolactam
  • Production of epsilon-caprolactam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] In a fixed-bed reactor equipped with RBS-1 zeolite catalyst, the reaction at 380 °C after heating the mixture of cyclohexanone oxime, methanol and ethanol (2:1), water (1:2:0.02 by weight) and nitrogen The Beckmann rearrangement reaction is carried out at high temperature, and the residence time is 8Sec. The reaction gas was cooled, part of the solvent was removed, and a reaction product containing 18 wt% of alcohol, 4 wt% of other impurities and 78 wt% of ε-caprolactam was obtained.

[0054] 500g of the above reaction product was stirred and crystallized at 20°C, and then centrifuged to obtain 308g of crude ε-caprolactam with a purity of 99.5wt%, and 192g of mother liquor. The mother liquor was distilled to obtain 78g of crude ε-caprolactam with a content of 99.3wt%. , The yield of ε-caprolactam is 98.1%. Two kinds of crude ε-caprolactam are mixed with 1500g benzene to form a benzene solution containing 20wt% ε-caprolactam, which is extracted 8 times with 1280g desalte...

Embodiment 2

[0057] According to the method of Example 1, take 500g of the reaction product obtained by stirring and crystallizing at 30°C, and then perform centrifugation to obtain 268g of crude ε-caprolactam with a purity of 99.75wt%, and obtain 232g of mother liquor. After removing 41g of the alcohol solvent in the mother liquor , the remaining 191g was stirred and crystallized at 30°C. After centrifugation, 83g of crude ε-caprolactam with a content of 99.5wt% was obtained. After separation, the mother liquor was distilled to obtain 36g of ε-caprolactam, with a yield of 99.1%. The crude ε-caprolactam obtained above was miscible with 900g benzene to form a benzene solution containing 30wt% ε-caprolactam, extracted 8 times with 580g desalted water to form an aqueous solution containing 40wt% ε-caprolactam, and passed through 50g adsorption at a speed of 5g / min. resin bed.

[0058] Take 600g containing 40wt% ε-caprolactam aqueous solution, with 30h -1 The space velocity is passed through ...

Embodiment 3

[0060] According to the method of Example 1, take 500g of the reaction product obtained by stirring and crystallizing at 36°C, and then perform centrifugation to obtain 238g of crude ε-caprolactam with a purity of 99.8wt%, and obtain 262g of mother liquor. After removing 40g of the alcohol solvent in the mother liquor , the remaining 222g was stirred and crystallized at 30°C. After centrifugation, 101g of crude ε-caprolactam with a content of 99.46wt% was obtained, and the remaining mother liquor was distilled to obtain 45g of ε-caprolactam, with a yield of 98%. The crude ε-caprolactam obtained above was miscible with 580g of benzene to form a benzene solution containing 40wt%ε-caprolactam, extracted 8 times with 390g desalted water to form an aqueous solution containing 48wt%ε-caprolactam, and passed through 50g adsorption at a speed of 5g / min. resin bed.

[0061] Take 600g containing 48wt% ε-caprolactam aqueous solution, with 30h -1 The space velocity is passed through a ma...

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Abstract

Production of epsilon-glycolylnium is carried out by Beckman rearrangement reacting for cyclohexanone-oxime under the existence of solvent to obtain epsilon-glycolylnium contained mixture, crystalline separating for the mixture to obtain crude epsilon-glycolylnium crystal, dissolving by arene, extracting by water, adsorbing by resin hydrogenation catalyzing to obtain the final product. The value of potassium permanganate is less than 5, extinction value is less 0.05, volatile alkali is less than 0.5meq / kg and alkalinity is less than 0.05meq / kg.

Description

technical field [0001] The invention relates to a preparation method of ε-caprolactam. Specifically, the purification method of ε-caprolactam involved in the present invention includes ε-caprolactam obtained from any reaction, such as in the presence of a solvent, after carrying out Beckmann rearrangement reaction of cyclohexanone oxime, the crude ε-caprolactam is obtained through cooling and crystallization. Caprolactam crystals and mixed with aromatic hydrocarbons, followed by water extraction, resin adsorption, and the preparation method of ε-caprolactam aqueous solution contacting with hydrogen in the presence of a hydrogenation catalyst. Background technique [0002] As an intermediate of nylon 6, ε-caprolactam has many preparation methods. For example: use fuming sulfuric acid as a catalyst to perform Beckmann rearrangement of cyclohexanone oxime to produce ε-caprolactam. However, this method has disadvantages such as a large amount of low-value-added ammonium sulfat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D201/06C07D223/10
Inventor 廖洪傅送保朱泽华李瑛王洪波
Owner CHINA PETROLEUM & CHEM CORP
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