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Method for separating and purifying cyclohexyl acetate hydrogenation reaction liquid

A technology of cyclohexyl acetate and hydrogenation reaction, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as the inability to obtain high-purity cyclohexanol products easily, and achieve economical and feasible improvement Sexuality, reduced generation of by-products, and simple operation

Pending Publication Date: 2022-08-05
JIANGSU YANGNONG CHEM GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, crude cyclohexyl ester is hydrogenated to obtain cyclohexanol and ethanol, but cyclohexyl acetate, cyclohexanol and other by-products also exist in the mixture, and high-purity cyclohexanol cannot be obtained simply

Method used

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  • Method for separating and purifying cyclohexyl acetate hydrogenation reaction liquid

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Effect test

Embodiment 1

[0057] The present embodiment provides a method for separation and purification of cyclohexyl acetate hydrogenation reaction liquid, the schematic flow diagram of the method is as follows figure 1 shown, including the following steps:

[0058] (1) adding the cyclohexyl acetate hydrogenation reaction liquid into the first rectifying tower 1 to carry out reactive distillation, the components of the cyclohexyl acetate hydrogenation reaction liquid include 70.6wt% of cyclohexanol by mass content , 28.9wt% of ethanol, 0.08wt% of cyclohexyl acetate, 0.05wt% of ethyl acetate and other impurities; the first rectification column 1 is a reactive rectification column, and the first rectification column 1 Filling basic resin catalyst, the basic resin catalyst is polystyrene strong basic anion exchange resin with organic amine functional group, and the filling volume fraction of the basic resin catalyst is 40%;

[0059] The tower still temperature of the first rectifying tower 1 is 130°C,...

Embodiment 2

[0062] The present embodiment provides a method for separating and purifying cyclohexyl acetate hydrogenation reaction liquid, and the method comprises the following steps:

[0063] (1) adding the cyclohexyl acetate hydrogenation reaction liquid into the first rectifying tower 1 to carry out reactive distillation, and the components of the cyclohexyl acetate hydrogenation reaction liquid include 67.6wt% of cyclohexanol by mass content , 31.9wt% of ethanol, 0.2wt% of cyclohexyl acetate, 0.1wt% of ethyl acetate and other impurities; the first rectification column 1 is a reactive rectification column, and the first rectification column 1 Filling the basic resin catalyst, the basic resin catalyst is a polystyrene strong basic anion exchange resin with organic amine functional groups, and the filling volume fraction of the basic resin catalyst is 60%;

[0064] The tower still temperature of the first rectifying tower 1 is 135°C, the tower top temperature is 80°C, the tower still pr...

Embodiment 3

[0067] The present embodiment provides a method for separating and purifying cyclohexyl acetate hydrogenation reaction liquid, and the method comprises the following steps:

[0068](1) adding the cyclohexyl acetate hydrogenation reaction liquid into the first rectifying tower 1 to carry out reactive distillation, and the components of the cyclohexyl acetate hydrogenation reaction liquid include 68.1wt% of cyclohexanol by mass content , 30.9wt% of ethanol, 0.6wt% of cyclohexyl acetate, 0.2wt% of ethyl acetate and other impurities; the first rectification column 1 is a reactive rectification column, and the first rectification column 1 Filling basic resin catalyst, the basic resin catalyst is polystyrene strong basic anion exchange resin with organic amine functional group, and the filling volume fraction of the basic resin catalyst is 80%;

[0069] The tower still temperature of the first rectifying tower 1 is 140°C, the tower top temperature is 83°C, the tower still pressure o...

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Abstract

The invention provides a method for separating and purifying cyclohexyl acetate hydrogenation reaction liquid, which comprises the following steps: adding cyclohexyl acetate hydrogenation reaction liquid into a first rectifying tower for reactive distillation, and filling the first rectifying tower with an alkaline resin catalyst to obtain a first light component and a first heavy component; and adding the first heavy component into a second rectifying tower for rectifying to obtain a cyclohexanol fraction at the tower top and a second heavy component at the tower bottom. According to the method disclosed by the invention, hydrolysis of ester substances such as cyclohexyl acetate is realized through reactive distillation according to the composition of cyclohexyl acetate hydrogenation reaction liquid, so that cyclohexanol and cyclohexyl acetate are completely separated, cyclohexanol and ethanol are fully separated, cyclohexanol is purified through a distillation mode, and the yield of cyclohexanol is improved. High-purity cyclohexanol and ethanol products are obtained; the method has the advantages of simple operation, mild process conditions, effective reduction of the generation of by-products, reduction of the separation energy consumption, and improvement of the economical efficiency and feasibility of the process.

Description

technical field [0001] The invention belongs to the technical field of organic separation, and relates to a method for separation and purification of cyclohexyl acetate hydrogenation reaction liquid. Background technique [0002] Cyclohexanol is an important organic solvent and organic chemical raw material. It is an important intermediate in the synthesis of caprolactam, adipic acid, etc. It can also be widely used as a solvent in the production of paint, shellac, varnish, dyes, etc. Emulsifying ability also plays an important role in fine chemical auxiliaries and plastic recycling; among them, synthesis of caprolactam and adipic acid is its most important use, so as to further prepare nylon fiber products. [0003] At present, the synthesis methods of cyclohexanol mainly include benzene hydrogenation-cyclohexane oxidation method, phenol hydrogenation method and benzene hydrogenation-cyclohexene hydration method. In the study, cyclohexene and acetic acid are used as raw ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/09C07C29/80C07C35/08C07C31/08
CPCC07C29/095C07C29/80C07C2601/14C07C35/08C07C31/08Y02P20/10
Inventor 黄杰军邓生财徐林丁克鸿张政吕丽马庆炎李明薛维海张寅张子鑫蒋旭史晓波秦娜娣
Owner JIANGSU YANGNONG CHEM GROUP