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Method for preparing cyclohexenyl cyclohexanone with high conversion rate

A technology of cyclohexanone and catalyst, which is applied in the field of preparation of cyclohexenyl cyclohexanone, can solve the problems of environmental pollution, low single-pass conversion rate of cyclohexanone, etc., and achieve the effect of reducing waste water discharge and high conversion rate

Inactive Publication Date: 2012-01-11
SHANDONG XINGANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101003471 relates to a method for continuously producing cyclohexenyl cyclohexanone from cyclohexanone under solid superacid catalysis, the single-pass conversion rate of cyclohexanone is lower than 50%, and the selectivity of cyclohexenyl cyclohexanone is below 97%
[0004] The above-mentioned method for preparing cyclohexenylcyclohexanone is mostly sulfuric acid or solid acid catalyst with catalyzer, and the single-pass conversion rate of reaction is generally about 50%. After the reaction finishes, the catalyzer will be separated, generally through water washing and alkali washing, resulting in certain A large amount of waste water containing organic matter will pollute the environment

Method used

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  • Method for preparing cyclohexenyl cyclohexanone with high conversion rate
  • Method for preparing cyclohexenyl cyclohexanone with high conversion rate
  • Method for preparing cyclohexenyl cyclohexanone with high conversion rate

Examples

Experimental program
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Effect test

Embodiment 1

[0025] In the reaction device shown in Figure 1, the cyclohexanone condensation reactor is 1000 L, the stirring is paddle type, and the rotation speed is 130 rpm. The catalyst filter device is a metal sintered filter tube with a diameter of Φ50 mm and a length of 200 mm. Add 700kg of cyclohexanone into the 1000L reactor, and add 120 mesh γ-Al under stirring 2 o 3 Catalyst 20kg, close the feeding port, heat the jacket with circulating heat transfer oil at 250°C, feed circulating cooling water into the total reflux condenser, and react under normal pressure. When the temperature of the kettle rises above 80°C, the condensation reaction of cyclohexanone begins, and the water and cyclohexanone vapor generated by the reaction rise to the total reflux condenser to condense, and then are collected in the oil-water separator for phase separation, and the water is kept at the bottom of the separator intermittently. Or discharge continuously, and the upper oil phase returns to the reac...

Embodiment 2

[0028] Same device as in Example 1, add 600kg of cyclohexanone in the reactor, and add 120 mesh γ-Al under stirring 2 o 3 20kg of catalyst, 100kg of cyclohexane with water agent, the maximum reaction temperature is 140°C, and other conditions are the same.

[0029] Stop heating after reaction finishes, sampling adopts gas chromatographic analysis condensation product to form: cyclohexanone 26.5%, cyclohexenyl cyclohexanone 72.0%, polycondensation compound is 1.5% (does not comprise cyclohexanone), cyclohexanone one-way The conversion rate is about 75%, the reaction selectivity is above 97.0%, and the purity of the cyclohexenyl cyclohexanone after direct distillation of the condensation product reaches 99.6%.

Embodiment 3

[0031] Same device as in Example 1, add 700kg of cyclohexanone in the reactor, and add 120 mesh WO 3 / TiO 2 、WO 3 / SiO 2 、WO 3 / γ-Al 2 o 3 Catalyst 20kg, other conditions are all the same, and its reaction result is shown in the following table.

[0032]

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Abstract

The invention relates to a method for preparing cyclohexenyl cyclohexanone which is the intermediate of o-phenyl phenol, particularly to a method for preparing the cyclohexenyl cyclohexanone with high conversion rate and high selectivity by taking cyclohexanone as raw material and taking solid oxide as catalyst.

Description

1. Technical field [0001] The invention relates to a method for preparing cyclohexenyl cyclohexanone, an intermediate of o-phenylphenol, in particular to a method for preparing cyclohexanone with high conversion rate and high selectivity using cyclohexanone as raw material and solid oxide as catalyst Process for the preparation of alkenyl cyclohexanone. 2. Background technology [0002] Cyclohexenyl cyclohexanone is an organic intermediate prepared by condensation and dehydration of cyclohexanone, and its main use is to produce o-phenylphenol (OPP) through catalytic dehydrogenation. OPP is a fine chemical and organic intermediate with a wide range of uses. It can be used as antiseptic, antifungal agent, broad-spectrum fungicide, used for fruit preservation, cosmetics, wood preservation, and disinfection of homes, public places, swimming pools and hospitals. It can also produce oil-soluble o-phenylphenol formaldehyde resin, non-ionic emulsifier, synthetic dye, etc. In recent...

Claims

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Application Information

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IPC IPC(8): C07C49/613C07C45/74
Inventor 傅桂华姚勇李慎伟
Owner SHANDONG XINGANG CHEM
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