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Method for preparation of cyclohexanone and cyclohexanol by decomposition of cyclohexyl hydroperoxide

A technology of cyclohexyl hydroperoxide and cyclohexane oxidation solution, which is applied in the fields of chemical instruments and methods, preparation of oxygen-containing compounds, and preparation of carbon-based compounds, etc. Problems such as large land area

Inactive Publication Date: 2014-12-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the following problems exist in the decomposition process of cyclohexyl hydroperoxide: the ratio of ketone to alcohol obtained after the decomposition of cyclohexyl hydroperoxide is not high, and the ratio of ketone to alcohol is generally below 1:1, which increases the load of subsequent dehydrogenation of cyclohexanol
The disadvantage of this patent is that the structure of the decomposition kettle is complicated, multiple sets of decomposition kettles are needed to realize the complete decomposition of cyclohexyl hydroperoxide, and the floor space is large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1. It is 85m to add flow rate at the tubular reactor inlet that length is 30 meters 3 / h of cyclohexane oxidation liquid, while adding a flow rate of 10m 3 / h Inorganic phase lye containing catalyst cobalt acetate, cobalt ion concentration 1.5 ppm, alkalinity 0.7mol / kg, inlet reaction temperature 90°C, tube reactor inlet pressure 0.1MPa, added at 15 meters from the tube reactor inlet The flow rate is 5m 3 / h lye, the decomposition rate of cyclohexyl hydroperoxide is 99.54%, the yield of cyclohexanone and cyclohexanol is 90.47%, cyclohexanone:cyclohexanol=1.01:1.

Embodiment 2

[0012] Embodiment 2. It is 85m to add flow rate at the tubular reactor inlet that length is 30 meters 3 / h of cyclohexane oxidation liquid, while adding a flow rate of 8m 3 / h Inorganic phase lye containing catalyst cobalt acetate, cobalt ion concentration 2.5 ppm, alkalinity 1.2mol / kg inlet reaction temperature 92°C, inlet pressure of tubular reactor 0.2MPa, 15m and 20m at the inlet of tubular reactor Add flow at 5m respectively 3 / h and 8m 3 / h of lye, the decomposition rate of cyclohexyl hydroperoxide is 99.62%, the yield of cyclohexanone and cyclohexanol is 91.47%, and cyclohexanone:cyclohexanol=1.08:1.

Embodiment 3

[0013] Embodiment 3. It is 100m to add flow rate at the tubular reactor inlet that length is 45 meters 3 / h of cyclohexane oxidation liquid, while adding a flow rate of 10m 3 / h Inorganic phase lye containing catalyst cobalt acetate, cobalt ion concentration 3.5 ppm, alkalinity 3.0mol / kg inlet reaction temperature 91°C, tube reactor inlet pressure 0.5MPa, 5 meters and 10 meters at the tube reactor inlet The flow rate is 8m respectively 3 / h and 5m 3 / h of lye, the decomposition rate of cyclohexyl hydroperoxide is 99.70%, the yield of cyclohexanone and cyclohexanol is 91.50%, and cyclohexanone:cyclohexanol=1.05:1.

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Abstract

The invention relates to a method for preparation of cyclohexanone and cyclohexanol by decomposition of cyclohexyl hydroperoxide in a cyclohexane oxidation liquid, and the method is characterized in that, a sodium hydroxide solution and a cobalt acetate solution are added in different feeding ports of a tubular reactor, cobalt ion concentration of the inorganic phase is 1.5-10ppm, the volume ratio of organic phase to inorganic phase in the decomposition reactor is 5.0-7.0: 1, and the basicity is 0.7-3.0mol / kg. The decomposition reactor temperature is controlled at 85-120 DEG C, the cyclohexyl hydroperoxide decomposition rate is greater than or equal to 99.5%, the cyclohexanone and cyclohexanol yield is greater than or equal to 90%, and the ketone-alcohol ratio is more than 1.0.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanone and cyclohexanol by decomposing cyclohexyl hydroperoxide in a cyclohexane oxidation liquid in a tubular reactor. 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 cyclohexyl under the conditions of a certain alkalinity, using 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 cyclohexane is recovered from the top of the tower and sent to the ...

Claims

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Application Information

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IPC IPC(8): C07C27/00C07C35/08C07C29/00C07C49/403C07C45/53
CPCC07C45/53C07C29/00C07C2601/14
Inventor 赵思远金汉强贾艳秋
Owner CHINA PETROLEUM & CHEM CORP
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