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Method for preparing 6-aminocapronitrile from cyclohexanone-oxime

A technology of aminocapronitrile and cyclohexanone oxime, which is applied to the preparation of lactam, chemical instruments and methods, and dehydration of carboxylic acid amide, can solve the problems of high energy consumption, many wastes, and large investment, and achieve steam saving consumption, cyclohexanone oxime consumption reduction effect

Inactive Publication Date: 2020-02-25
HUNAN BAILI ENGINEERING SCIENCE AND TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no patent on the preparation of 6-aminocapronitrile from cyclohexanone oxime. Although patents such as US2234566 and FR1573490 mention the technology of using caprolactam to prepare 6-aminocapronitrile, the rearrangement of cyclohexanone oxime to obtain caprolactam requires a complicated refining process. , large investment, high energy consumption, and many wastes

Method used

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  • Method for preparing 6-aminocapronitrile from cyclohexanone-oxime
  • Method for preparing 6-aminocapronitrile from cyclohexanone-oxime
  • Method for preparing 6-aminocapronitrile from cyclohexanone-oxime

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Embodiment 1

[0039] Preparation of 6-Aminocapronitrile by Liquid Phase Rearrangement of Cyclohexanone Oxime

[0040]70-80% of the total flow rate of cyclohexanone oxime is initially reacted with oleum at 85-105°C under normal pressure to obtain a rearrangement mixture containing ε-caprolactam. The reaction conditions are oleum:cyclohexane Ketoxime ratio is 1.5-1.8:1, SO in the rearrangement mixture after reaction 3 The content is 4%-5% (wt); continue to react 20-30% flow of cyclohexanone oxime with oleum at 85-105°C under normal pressure to obtain a rearrangement mixture containing ε-caprolactam.

[0041] The obtained rearrangement mixture containing ε-caprolactam is neutralized and crystallized with ammonia in a neutralization crystallization reactor to obtain amide oil containing 70% ε-caprolactam, and ammonium sulfate is produced as a by-product.

[0042] Extract ε-caprolactam from amide oil with benzene to obtain 15-25% ε-caprolactam benzene solution.

[0043] The extracted ε-caprola...

Embodiment 2

[0048] Others are the same as in Example 1, except that before the ε-caprolactam in the amide oil is extracted with benzene, the amide oil is washed and desalted with 4% NaOH solution, and the desalted amide oil is extracted with benzene.

[0049] Due to the use of alkali to elute the salt, the operating cycle of the caprolactam evaporator can be extended, and the selectivity of 6-aminocapronitrile is 97.2%. Save steam consumption by 2.0-3.0t / t 6-aminocapronitrile, and reduce cyclohexanone oxime consumption by 20-50kg / t 6-aminocapronitrile.

Embodiment 3

[0051] Preparation of 6-Aminocapronitrile by Vapor Phase Rearrangement of Cyclohexanone Oxime

[0052] In the presence of a molecular sieve catalyst with an MFI structure, cyclohexanone oxime in a gas phase is reacted in the presence of a carrier gas and a solvent. The conditions of the gas-phase Beckmann rearrangement reaction may include: the temperature is 320-450°C, preferably 370-400°C; the pressure is 0.05-0.5MPa, preferably 0.1-0.3MPa; the mass space velocity of cyclohexanone oxime is 0.1-5h -1 . The solvent can be low-carbon alcohol; the carrier gas is nitrogen and inert gas.

[0053] The reaction gas is cooled, and high-boiling components as impurities are separated from the cooled reaction liquid to obtain a mixed gas containing ε-caprolactam, lower alcohols and inert gases, and the crude ε-caprolactam mixture containing ε-caprolactam is subjected to Distillation separates light and heavy components.

[0054] The vacuum-state caprolactam vapor separated from the ...

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Abstract

The invention discloses a method for preparing 6-aminocapronitrile from cyclohexanone-oxime. The method comprises the following steps: carrying out a rearrangement reaction on cyclohexanone-oxime to obtain a rearranged reaction material; and treating the rearranged reaction material to obtain caprolactam, carrying out an ammoniation dehydration reaction on the caprolactam to obtain an ammoniated dehydrated reaction material, and performing separation to obtain the 6-aminocapronitrile. Compared with the prior art, the method of the invention reduces complex separation and refining processes such as back extraction, ion exchange, hydrogenation, evaporation and distillation required after liquid phase rearrangement of the cyclohexanone-oxime, reduces the processes of crystallization, solventrefining and recovery needed after gas phase rearrangement, and organically combines the caproamide evaporation and rearrangement treatment processes in the ammoniation dehydration reaction process. The steam consumption can be reduced by 2.0-3.0 t / t 6-aminocapronitrile, and the cyclohexanone-oxime consumption is reduced by 20-50 kg / t 6-aminocapronitrile.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to a method for preparing 6-aminocapronitrile from cyclohexanone oxime, in particular to a method for preparing 6-aminocapronitrile through rearrangement, ammoniation and dehydration of cyclohexanone oxime. Background technique [0002] 6-Aminocapronitrile is an important chemical intermediate that can be used to produce 1,6-hexamethylenediamine by complete hydrogenation, which can be used to produce the polymer nylon 66. At present, the preparation of 6-aminocapronitrile is mainly obtained by partial hydrogenation of 1,6 adiponitrile, such as patents CN1238334C and CN101309897B, or by hydroformylation of pentenenitrile, such as patent CN1100752C. There is no patent on the preparation of 6-aminocapronitrile from cyclohexanone oxime. Although patents such as US2234566 and FR1573490 mention the technology of using caprolactam to prepare 6-aminocapronitrile, the rearran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C255/24
CPCC07C253/20C07D201/04C07D201/16C07D223/10
Inventor 邵寒梅蒋遥明陈超
Owner HUNAN BAILI ENGINEERING SCIENCE AND TECHNOLOGY CO LTD
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