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Method for complex catalytic decomposition of cyclohexyl hydrogen peroxide

A cyclohexyl hydrogen peroxide, catalytic decomposition technology, applied in chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, preparation of oxygen-containing compounds, etc. High low temperature activity, good water phase stability and good overall selectivity

Active Publication Date: 2009-06-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, chromic anhydride is easily reduced to Cr3+ ions with low activity, and chromic anhydride is toxic and cannot be used in industry

Method used

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  • Method for complex catalytic decomposition of cyclohexyl hydrogen peroxide
  • Method for complex catalytic decomposition of cyclohexyl hydrogen peroxide
  • Method for complex catalytic decomposition of cyclohexyl hydrogen peroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 0.05 gram of ammonium molybdate, 0.1 gram of oxalic acid and 1 gram of water into a 50 milliliter stainless steel reaction kettle, and stir at room temperature to form a blue solution, which is an aqueous solution of complexed molybdenum oxalate. 10 g of a 2.1% cyclohexane solution containing cyclohexane hydroperoxide was added thereto. Replace the reactor with nitrogen first, then close the gas inlet and outlet valves, heat up to 85°C while stirring, continue the constant temperature reaction for 20 minutes, then cool down, and take out the upper organic phase for analysis.

[0033] The test results are shown in Table 2.

Embodiment 2

[0035] Add 0.01 gram of ammonium molybdate, 0.05 gram of tartaric acid and 1 gram of water into a 50 milliliter stainless steel reaction kettle, stir at room temperature to generate a blue solution, which is an aqueous solution of complexed molybdenum tartrate. 10 g of a 2.1% cyclohexane solution containing cyclohexane hydroperoxide was added thereto. Replace the reactor with nitrogen, then close the gas inlet and outlet valves, heat up to 125°C while stirring, continue the constant temperature reaction for 20 minutes, then cool down, and take out the upper organic phase for analysis.

Embodiment 3

[0037] Add 0.05 gram of ammonium molybdate, 0.1 gram of pyridine-2-formic acid and 1 gram of water into a 50 milliliter stainless steel reaction kettle, stir at room temperature to generate complex pyridine-2-formic acid molybdenum aqueous solution. 10 g of a 2.1% cyclohexane solution containing cyclohexane hydroperoxide was added thereto. The reaction kettle was first replaced with nitrogen, and then the gas inlet and outlet valves were tightly closed, and the temperature was raised to 105°C while stirring, and the constant temperature reaction was continued for 30 minutes, then the temperature was lowered, and the upper organic phase was taken out for analysis.

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Abstract

The invention relates to a process for producing cyclohexanol and cyclohexanone by air oxidation of cyclohexane, in particular to a method for complex catalytic decomposition of cyclohexyl hydroperoxide. The method takes the cyclohexyl hydroperoxide as reaction substrate and uses water soluble transition metal organic complex as a catalyst, and the cyclohexyl hydroperoxide is transformed into the mixture of the cyclohexanol and the cyclohexanone with high selectivity under the two phase of cyclohexane-aqueous condition. Compared with the existing catalyst for decomposing the cyclohexane hydroperoxide, the method of the invention uses the decomposition catalyst with the characteristics of low temperature, high activity, good aqueous phase stability, good overall selection of the cyclohexanol and the cyclohexanone, and no need to add alkali, etc.

Description

technical field [0001] The present invention relates to the process that air oxidizes cyclohexane to produce cyclohexanol and cyclohexanone, specifically a method for complexing and catalytically decomposing cyclohexyl hydroperoxide, using cyclohexane oxidation solution containing cyclohexyl hydroperoxide as the The raw material is a method for converting cyclohexane hydroperoxide into cyclohexanol and cyclohexanone under the catalysis of a water-soluble transition metal organic complex catalyst. technical background [0002] The decomposition reaction of cyclohexane hydroperoxide is one of the important links in the process of preparing cyclohexanol and cyclohexanone by the oxidation of cyclohexane. [0003] Its decomposition reaction can be expressed by the chemical reaction formula as follows: [0004] [0005] The existing industrial method is to use a large amount of sodium hydroxide lye containing cobalt ions to decompose cyclohexane hydroperoxide. This method has...

Claims

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Application Information

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IPC IPC(8): C07C27/00C07C29/00C07C35/08C07C45/53C07C49/11B01J31/04
Inventor 孙志强徐杰李德财聂鑫陈晨
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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