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Homogeneous catalyst and its application in decomposing cyclohexyl hydroperoxide

A cyclohexyl hydrogen peroxide, catalyst technology, applied in physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, preparation of oxygen-containing compound and other directions

Active Publication Date: 2014-07-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on this type of catalyst and its application in the decomposition of cyclohexyl hydroperoxide

Method used

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  • Homogeneous catalyst and its application in decomposing cyclohexyl hydroperoxide
  • Homogeneous catalyst and its application in decomposing cyclohexyl hydroperoxide
  • Homogeneous catalyst and its application in decomposing cyclohexyl hydroperoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 0.071g of copper chloride dihydrate and dissolve it in 10ml of ethanol, use a micro-injector to take 10ul of the ethanol solution of copper chloride and add it to a 50ml stainless steel reaction kettle with electromagnetic stirring, then add 10ml (about 7.8g) containing cyclohexyl Hydrogen peroxide is 6% (0.5029mmol / g) cyclohexane oxidation solution, wherein the molar ratio of cyclohexyl hydroperoxide to copper chloride=2250;

[0024] Replace the reactor with nitrogen first, then close the gas inlet and outlet valves, and heat to 70°C while stirring. o C, keep the temperature for 30 minutes, lower the temperature, and take out the reaction product.

[0025] The content of cyclohexane hydrogen peroxide before and after the reaction was analyzed by iodine-sodium thiosulfate redox titration method, and the amount of cyclohexanol and cyclohexanone in the reaction solution and the generated solution before and after the reaction were analyzed by gas chromatography inter...

Embodiment 2

[0027] Carry out by the operation process of embodiment 1, difference with embodiment 1 is:

[0028] Use 0.0003388g hexadecyltrimethylammonium chloride (HTAC) as a catalyst (dissolve 0.3388gHTAC in 10ml ethanol, take 10ul with a micro-sampler and add it to the reaction solution, wherein the molar ratio of cyclohexyl hydroperoxide to HTAC = 2250) to repeat the test of Example 1, and the results are listed in Table 1 together.

Embodiment 3

[0030] Carry out by the operation process of embodiment 1, difference with embodiment 1 is:

[0031] Use 0.000071g copper chloride and 0.0001694g HTAC (add 10ul copper chloride solution and 5ul HTAC solution to the reaction solution, the molar ratio of quaternary ammonium salt to copper chloride = 1; the molar ratio of cyclohexyl hydroperoxide to copper chloride = 2250) As a catalyst, the test of Example 1 was repeated, and the results are listed in Table 2 together.

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Abstract

A method for catalytically decomposing cyclohexyl hydroperoxide under non-precious metal and alkali-free conditions, using industrial cyclohexane oxidation liquid as raw material, and under the action of a catalyst, it realizes alkali-free decomposition of cyclohexyl hydroperoxide to generate cyclohexanol and cyclohexyl ketone. The invention is a non-noble metal homogeneous catalyst with simple preparation method and high selectivity to cyclohexanol and cyclohexanone.

Description

technical field [0001] The invention relates to the preparation and application of a catalyst for preparing cyclohexanol and cyclohexanone by using non-noble metals to catalyze and decompose cyclohexyl hydroperoxide under alkali-free conditions. Background technique [0002] The decomposition reaction of cyclohexyl hydroperoxide is one of the important links in the process of preparing cyclohexanol and cyclohexanone by the oxidation of cyclohexane. Its decomposition reaction can be expressed by the chemical reaction formula as follows: [0003] [0004] Inorganic bases such as sodium hydroxide have high efficiency and selectivity for the catalytic decomposition process. Using a large amount of sodium hydroxide lye to catalyze the decomposition of cyclohexane hydroperoxide through cobalt ions is one of the important industrial processes for the preparation of cyclohexanone. . This method has high cost; in particular, a large amount of alkali added generates a large amoun...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/30B01J31/32C07C27/00C07C35/08C07C29/132C07C49/403C07C45/53
Inventor 徐杰郑玺孙志强苗虹王敏杜中田
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI