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Method for preparing cyclohexanone and cyclohexanol by decomposition of cyclohexane oxidation liquid

A technology of cyclohexane oxidation solution and cyclohexanone is applied in the field of cyclohexanone and cyclohexanol by decomposing cyclohexane oxidation solution, which can solve the problem of high alkali consumption, low selectivity of alcohol and ketone, and conversion of cyclohexyl hydroperoxide. problems such as low rate, to achieve the effect of reducing the consumption of alkali

Active Publication Date: 2017-07-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Purpose of the invention: The present invention aims at the problems of low conversion rate of cyclohexyl hydroperoxide, low selectivity of alcohol and ketone, high alkali consumption and the like in the prior art, and provides a cyclohexane oxidation solution to decompose cyclohexanone and cyclohexanol Methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 12g of chromium oxide and dissolve it in 20g of deionized water, and place the obtained solution in a constant pressure funnel; add 36.95g of isooctyl alcohol into a three-neck flask, start stirring, add dropwise chromium oxide solution, control the dropping speed, and finish dropping within 0.5h , control the reaction temperature at 30°C, after the dropwise addition, continue to stir for 1h, add 150ml of cyclohexane, stir for 0.5h after the addition, put the material in a separatory funnel, let it stand for 0.5h, separate the aqueous phase and the organic phase, organic The phase is isooctyl chromate, a catalyst for slightly acidic decomposition.

[0023] Cyclohexane oxidation liquid and catalyst solution mixed at a volume ratio of 20:1 enter three 1L high-pressure reactors in series at a flow rate of 1.5L / h. The stirring speed of the reactor is 300r / min, the reaction temperature is 110°C, and the pressure is 0.5 Mpa, the decomposed liquid from the third kettle i...

Embodiment 2

[0025] Weigh 12g of chromium oxide and dissolve it in 20g of deionized water, and place the resulting solution in a constant pressure funnel; add 24.63g of isooctyl alcohol to a three-neck flask, start stirring, add the chromium oxide solution dropwise, control the dropping speed, and finish dropping within 1 hour. Control the reaction temperature at 18°C, after the dropwise addition, continue to stir for 1.5h, add 100ml of cyclohexane, stir for 0.5h after the addition, put the material in a separatory funnel, let it stand for 0.5h, separate the aqueous phase and the organic phase, organic The phase is isooctyl chromate, a catalyst for slightly acidic decomposition.

[0026] The cyclohexane oxidation liquid and the catalyst solution mixed according to the volume ratio of 30:1 are sequentially entered into three series-connected 1L high-pressure reactors at a flow rate of 0.75L / h, the stirring speed is 300r / min, the reaction temperature is 130°C, and the pressure is 0.6Mpa. The...

Embodiment 3

[0028] Weigh 12g of chromium oxide and dissolve it in 20g of deionized water, and place the resulting solution in a constant pressure funnel; add 20.52g of isooctyl alcohol to a three-neck flask, start stirring, add chromium oxide solution dropwise, control the dropping speed, and finish dropping within 0.75h , control the reaction temperature at 18°C, after the dropwise addition, continue to stir for 1.2h, add 100ml of cyclohexane, stir for 0.5h after the addition, put the material in a separatory funnel, let it stand for 0.5h, separate the aqueous phase and the organic phase, The organic phase is the catalyst of slightly acidic decomposition of isooctyl chromate.

[0029] The cyclohexane oxidation liquid and the catalyst solution mixed at a volume ratio of 45:1 enter three 1L high-pressure reactors in series at a flow rate of 0.6L / h, the stirring speed is 300r / min, the reaction temperature is 140°C, and the pressure is 0.65Mpa. The decomposed liquid from the third kettle is ...

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Abstract

The invention discloses a method for preparing cyclohexanone and cyclohexanol by decomposition of a cyclohexane oxidation liquid. The method comprises the following steps: a cyclohexane oxidation liquid is subjected to a homogeneous decomposition reaction in the presence of an oil-soluble catalyst isooctyl chromate at the reaction temperature of 100-160 DEG C at the pressure of 0.3-0.8 Mpa for 1.0-5 h; after the decomposition reaction, the decomposition liquor is cooled and then washed with alkali lye, followed by standing and alkali separation; then, an organic phase and an inorganic phase are obtained; and the organic phase is separated and refined so as to obtain cyclohexanone and cyclohexanol. By using the oil-soluble catalyst isooctyl chromate, the traditional thinking of using aqueous alkali for heterogeneous decomposition is broken through. By changing the catalytic system and reaction condition, cyclohexyl hydroperoxide decomposition rate reaches 99.8% and above, yield of cyclohexanone and cyclohexanol obtained after the decomposition is 98% and above, and ketone-to-alcohol ratio is 1.3:1 and above and far higher than the ratio of 1:1 in traditional basic decomposition. As the cyclohexyl hydroperoxide decomposition reaction needn't be carried out under the alkaline condition, consumption of alkali is also greatly reduced.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanone and cyclohexanol by decomposing cyclohexane oxidation liquid, in particular to a method for preparing cyclohexanone and cyclohexanol by changing the catalytic system and reaction conditions. Background technique [0002] The oxidation of cyclohexane to cyclohexanone consists of the following steps: first, cyclohexane is oxidized in the air at 155-165 ° C to obtain a cyclohexane solution of cyclohexyl hydroperoxide, and then the cyclohexane solution in the cyclohexane solution Hexyl hydroperoxide decomposes into cyclohexanone and cyclohexanone at a certain alkalinity, with cobalt acetate as a catalyst, cobalt ion concentration of 1-3ppm, volume ratio of organic phase to inorganic phase of 85:15, and reaction temperature of 85-110°C Alcohol; the decomposed product is separated from the organic phase and the inorganic phase, the organic phase enters the alkane rectification system, the cyclohex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/403C07C45/53C07C35/08C07C29/48C07C27/16
CPCC07C29/48C07C45/53C07C409/14C07C49/403C07C35/08
Inventor 赵思远季峰崎金汉强陈琛
Owner CHINA PETROLEUM & CHEM CORP
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