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A kind of decomposition method of cyclohexyl hydroperoxide

A technology for cyclohexyl hydrogen peroxide and cyclohexane oxidation solution, which is applied in the field of decomposition of cyclohexyl hydrogen peroxide, can solve the problems of complex catalyst preparation process, environmental pollution by alkaline waste water, low ratio of ketone and alcohol, etc. Consumption, easy handling, high selectivity effect

Inactive Publication Date: 2016-03-02
SHANGHAI HONGLU CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following problems in the decomposition process of cyclohexyl hydroperoxide at present: the production energy consumption is higher, and a large amount of alkali is added in the production, generate a large amount of alkaline waste water and pollute the environment, in addition, the ratio of ketone alcohol obtained after the decomposition of cyclohexyl hydroperoxide is not high High, generally the ketone-alcohol ratio is around 1:1
Most of the above-mentioned catalysts are noble metal catalysts, and the catalyst preparation process is complicated and the cost is high, so it is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under normal pressure, in a three-necked flask with a volume of 250ml, add 100ml of cyclohexane oxidation liquid containing cyclohexyl hydroperoxide and 20ml of nitric acid aqueous solution containing ferric nitrate (inorganic phase catalyst), and the aqueous nitric acid solution containing ferric nitrate (inorganic phase catalyst) ) with an acidity of 0.16mol / kg, an iron ion concentration of 1000mg / L, a reaction temperature of 75°C, and a reaction time of 1h. After the reaction, the organic phase and the inorganic phase were separated into liquid and liquid.

[0021] Before the reaction, the cyclohexane oxidation solution contained 0.46% cyclohexanone, 0.72% cyclohexanol, and 3.63% cyclohexyl hydroperoxide; after the reaction, the organic phase contained 2.32% cyclohexanone, 1.78% cyclohexanol, and cyclohexanol. Hexyl Hydroperoxide 0.12%. The conversion rate of cyclohexyl hydroperoxide is 96.69%, and the yield of cyclohexanone and cyclohexanol is 97.74%, cyclohexanone:...

Embodiment 2

[0023] In a stainless steel reaction kettle with a volume of 1000ml, add 300ml cyclohexane oxidation solution containing cyclohexyl hydroperoxide and 60ml aqueous nitric acid solution (inorganic phase catalyst) containing copper nitrate, the acidity of the aqueous nitric acid solution (inorganic phase catalyst) containing copper nitrate 0.16mol / kg, copper ion concentration 1000mg / L, flush nitrogen to 0.2Mpa, reaction temperature 100°C, reaction time 1h, after the reaction, separate the organic phase and inorganic phase liquid-liquid.

[0024] Before the reaction, the cyclohexane oxidation solution contained 0.46% of cyclohexanone, 0.72% of cyclohexanol, and 3.63% of cyclohexyl hydroperoxide; after the reaction, the organic phase contained 1.97% of cyclohexanone, 2.11% of cyclohexanol, and cyclohexanol Hexyl Hydroperoxide 0.11%. The conversion rate of cyclohexyl hydroperoxide is 96.97%, and the yield of cyclohexanone and cyclohexanol is 96.58%, cyclohexanone:cyclohexanol=1.11:1...

Embodiment 3

[0026] Under normal pressure, in a three-necked flask with a volume of 250ml, add 100ml of cyclohexane oxidation solution containing cyclohexyl hydroperoxide and 20ml of aqueous nitric acid solution containing vanadium nitrate (inorganic phase catalyst), and the aqueous nitric acid solution containing vanadium nitrate (inorganic phase catalyst) ) with an acidity of 0.32mol / kg, a concentration of vanadium ions of 1000mg / L, a reaction temperature of 75°C, and a reaction time of 1 hour. After the reaction, the organic phase and the inorganic phase were separated into liquid and liquid.

[0027] Before the reaction, the cyclohexane oxidation solution contained 0.46% cyclohexanone, 0.72% cyclohexanol, and 3.63% cyclohexyl hydroperoxide; after the reaction, the organic phase contained 2.04% cyclohexanone, 1.70% cyclohexanol, and cyclohexanol. Hexyl Hydroperoxide 0.29%. The conversion rate of cyclohexyl hydroperoxide is 92.01%, and the yield of cyclohexanone and cyclohexanol is 90.03...

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Abstract

The invention discloses a decomposition method of cyclohexyl hydrogen peroxide, belongs to the technical field of organic chemistry. The decomposition method of cyclohexyl hydrogen peroxide comprises the following steps: an acidic aqueous solution of transition metal nitrate is added into a cyclohexane oxidation solution containing cyclohexyl hydrogen peroxide; the mixed solution reacts for 0.1 to 3 hours at the temperature of 60 to 120 DEG C under the pressure condition of 0.1 to 1 Mpa; the volume ratio of the acidic aqueous solution to the cyclohexane oxidation solution is 1:1 to 100; the concentration of the transition metal ion in the acidic aqueous solution is 1 to 10,000mg / L, and the acidity is 0 to 5 mol / kg. According to the decomposition method of cyclohexyl hydrogen peroxide, the decomposing and transforming rate of cyclohexyl hydrogen peroxide is greater than or equal to 90%, and the reaction yield of cyclohexanone and cyclohexanol is greater than or equal to 90%, the alcohol ketone ratio is between 1.1 to 2.0; besides, an inorganic phase solution containing a catalyst (transition metal nitrate) can be reused, so that the consumption of the catalyst is reduced, the cost is reduced, and waste liquid emission is reduced.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a method for decomposing cyclohexyl hydroperoxide. Background technique [0002] The preparation of cyclohexanone by the oxidation of cyclohexane includes the following steps: 1) Catalytic oxidation of cyclohexane at 160-180°C in the air to obtain a cyclohexane oxidation solution whose main product is cyclohexyl hydroperoxide; 2) Cyclohexane The cyclohexyl hydroperoxide in the alkoxylation solution decomposes under a certain alkalinity, using a cobalt ion concentration of 1-3ppm cobalt acetate solution as a catalyst, the volume ratio of the organic phase to the inorganic phase is 85:15, and the reaction temperature is 80-110°C For cyclohexanone and cyclohexanol. The decomposed product is separated from the organic phase and the inorganic phase, the organic phase enters the alkane rectification system, the cyclohexane recovered from the top of the tower is sent to the o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/00C07C29/132C07C35/08C07C45/53C07C49/403
CPCY02P20/584
Inventor 余洪勇王敬松吴化林杨志强孙伟康传瑞岳远会郭园
Owner SHANGHAI HONGLU CHEM TECH