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Preparation method and application of nano MgO catalyst

A catalyst and nanotechnology, applied in the field of preparation of alkaline earth metal oxide catalysts, can solve the problems of high cost and low selectivity, and achieve the effects of low manufacturing cost, high selectivity and mild reaction conditions

Inactive Publication Date: 2017-10-27
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method and application of a nano-MgO catalyst for the technical deficiency of low selectivity or high cost of existing catalysts in the cumene oxidation reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 0.5molMg(NO 3 ) 2 .6H 2 O was dissolved in 167ml of deionized water and 83ml of absolute ethanol, and stirred in a water bath at 20°C for 15 minutes. While stirring, slowly drop in 1.5mol of ammonia solution as a precipitant, and continue stirring for 0.5h after the addition. Then crystallize at 150°C for 12 hours, wash with water, filter with suction, and dry after crystallization, and roast the dried sample at 550°C for 6 hours to obtain a nano-MgO catalyst. According to the method described in Comparative Example 1, the catalytic performance of the catalyst for cumene oxidation was investigated. The analysis results of the reaction product were: the conversion rate of cumene was 32.5%, and the selectivity of cumene hydroperoxide was 92.3%.

Embodiment 2

[0039] 0.5molMg(NO 3 ) 2 .6H 2 O was dissolved in 83ml of deionized water and 167ml of absolute ethanol, and stirred in a water bath at 40°C for 60 minutes. While stirring, slowly drop 1.25mol of ammonia solution as a precipitant, and continue stirring for 2 hours after the addition. Then crystallize at 170°C for 48h, wash with water, suction filter and dry after crystallization, and roast the dried sample at 550°C for 6h to prepare the nano-MgO catalyst. According to the method described in Comparative Example 1, the catalytic performance of the catalyst for cumene oxidation was investigated. The analysis results of the reaction product are: the conversion rate of cumene is 33.5%, and the selectivity of cumene hydroperoxide is 95.8%.

Embodiment 3

[0041] 0.5molMg(NO 3 ) 2 .6H 2O was dissolved in 125ml of deionized water and 125ml of absolute ethanol, and stirred in a 60°C water bath for 30 minutes. While stirring, slowly drop 1 mol of ammonia solution as a precipitant, and continue stirring for 1 hour after the addition. Then crystallize at 170°C for 24 hours, wash with water, filter with suction, and dry after crystallization, and roast the dried sample at 550°C for 6 hours to obtain a nano-MgO catalyst. According to the method described in Comparative Example 1, the catalytic performance of the catalyst for cumene oxidation was investigated. The analysis results of the reaction product are: the conversion rate of cumene is 36.5%, and the selectivity of cumene hydroperoxide is 97.3%.

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Abstract

The invention relates to a preparation method and application of a nano MgO catalyst. The preparation method comprises the following steps: dissolving Mg(NO3)2.6H2O into a mixed solution of water and absolute ethyl alcohol, and stirring in a water bath until Mg(NO3)2.6H2O is completely dissolved in the mixed solution of water and absolute ethyl alcohol; dropping an aqueous solution of ammonia into the abovementioned solution with stirring, wherein the molar ratio of the aqueous solution of ammonia to Mg(NO3)2.6H2O is (2-3):1; continuously stirring after dropwise adding, and then realizing crystallization at the temperature of 150-170 DEG C; and performing water washing, pumping filtration, drying and roasting after the crystallization, so as to obtain the nano MgO catalyst. The catalyst is applied to the process of synthesizing cumyl hydroperoxide with isopropylbenzene through catalytic oxidation; the isopropylbenzene oxidization reaction is performed in the presence of oxygen-containing gas which is one of air and oxygen-rich gas; in the catalyst reaction, reaction conditions are mild, the catalyst activity is high, the selectivity is high, the economy is high, and the method and the application can be used for industrial production.

Description

technical field [0001] The invention relates to a preparation method and application of an alkaline earth metal oxide catalyst, in particular to a preparation method of a nanometer MgO catalyst and a method for preparing cumene hydroperoxide by catalytic oxidation of cumene. Background technique [0002] The oxidation of cumene to generate cumene hydroperoxide is a key step in the phenol-acetone process. The cumene oxidation product cumene hydroperoxide (CHP) is not only used for the synthesis of phenol, but also widely used in other fields of fine chemicals, polymer materials and organic synthesis. It can be used as an initiator for chain auto-oxidation and polymerization reactions, an accelerator for rubber vulcanization, and an oxidant for organic compounds. CHP is also commonly used in the synthesis of dicumyl peroxide (DCP), and DCP is a widely used fine chemicals. With the increasing development of phenol chemical industry and the continuous expansion of the applicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/10B01J37/03B01J35/10C07C407/00C07C409/10
CPCC07C407/00B01J21/10B01J37/031B01J35/643B01J35/647C07C409/10
Inventor 赵克品吴美玲周灵杰段大勇李军
Owner CHINA PETROLEUM & CHEM CORP
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