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Catalyst for preparing benzenediol through phenol hydroxylation and preparation method of catalyst

A technology of phenol hydroxylation to quinone and hydroxylation to quinone, which is applied in the production of bulk chemicals, etc., can solve the problems of low catalytic activity and short life, and achieve high phenol conversion rate, easy separation, and low catalyst price cheap effect

Inactive Publication Date: 2013-11-20
TANGSHAN NORMAL UNIV
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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 address many deficiencies in the prior art, and the use of metal oxide catalysts in the preparation of phenol by the hydroxylation of phenol hydrogen peroxide has two major problems of low catalytic activity and short life. A small catalyst for the hydroxylation of phenol to diphenol, and the second is to provide a preparation method for a catalyst for the hydroxylation of phenol to diphenol that is suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 5 g of diatomaceous earth, soak it with 1 mol / L hydrochloric acid solution for 2 h, filter, wash until neutral, dry, and set aside. Take 24 g of copper nitrate, add 100 mL of water, stir to dissolve, add 4 g of diatomaceous earth, 25 o C stirred for 12 h. filter, dry, 500 o C air atmosphere, calcined for 2 h to obtain diatomite-supported copper oxide catalyst.

[0026] Take 2 g phenol, 20 mL deionized water, 0.2 g diatomaceous earth supported copper oxide catalyst, 50 o Under stirring at C, add 10 mL of hydrogen peroxide with a mass fraction of 30% dropwise to the above solution, after the dropwise addition, add 1-2 drops of acetic acid dropwise, react for 2 h and remove the catalyst by filtration, wash and dry the catalyst with ethanol reuse. Detected by liquid chromatography, the calculated conversion rate of phenol was 50%, and the selectivity of hydroquinone was 82%. Catechol / hydroquinone was 1.54.

Embodiment 2

[0028] Take 5 g of diatomaceous earth, soak it with 1 mol / L sodium hydroxide solution for 24 h, filter, wash until neutral, dry, and set aside. Take 24 g of copper nitrate, add 100 mL of water, stir to dissolve, add the treated diatomaceous earth, 35 o C stirred for 2 h. filter, dry, 500 o C air atmosphere, calcined for 2h to obtain diatomaceous earth supported copper oxide catalyst.

[0029] Take 2 g phenol, 20 mL deionized water, 0.1 g diatomaceous earth supported copper oxide catalyst, 50 o Under stirring, 10 mL of hydrogen peroxide with a mass fraction of 30% was added dropwise to the above solution, reacted for 2 h, and filtered to remove the catalyst. The catalyst was washed and dried with ethanol and reused. Detected by liquid chromatography, the calculated conversion rate of phenol was 40%, and the selectivity of hydroquinone was 78%. Catechol / Hydroquinone is 1.50.

Embodiment 3

[0031] Take 5 g of diatomite, soak it with 2 mol / L hydrochloric acid solution for 10 h, filter, wash until neutral, dry, and set aside. Take 24 g of copper nitrate and 40 g of ferric nitrate, add 100 mL of water, stir and dissolve, then add the treated diatomaceous earth, 30 o C stirred for 10 h. filter, dry, 400 o C air atmosphere, calcined for 2 h to obtain diatomaceous earth supported copper-iron oxide catalyst.

[0032] Take 2 g phenol, 20 mL deionized water, 0.1 g diatomaceous earth supported copper-iron oxide catalyst, 50 o Under stirring, 10 mL of hydrogen peroxide with a mass fraction of 30% was added dropwise to the above solution, reacted for 2 h, and filtered to remove the catalyst. The catalyst was washed and dried with ethanol and reused. Detected by liquid chromatography, the calculated conversion rate of phenol was 80%, and the selectivity of hydroquinone was 65%. Catechol / hydroquinone is 1.45.

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Abstract

The invention provides a catalyst for preparing benzenediol through phenol hydroxylation and a preparation method of the catalyst. The preparation method comprises the following steps: treating the diatomite serving as a carrier of the catalyst by using an alkaline solution or an acidic solution, loading copper or iron to the diatomite by using an impregnation method, and washing and baking to obtain the copper / diatomite, iron / diatomite or iron and copper composite oxide / diatomite catalyst. Through liquid-phase chromatographic detection, the conversion rate of phenol, the selectivity of the phenol and the ratio of the catechol to the phenol are calculated. The catalyst has the characteristics of simple preparation method, low cost and environmental-friendliness and is suitable for industrial production.

Description

technical field [0001] The present invention relates to a catalyst and its preparation method, in particular to a preparation method of a diatomite-loaded metal oxide catalyst used for phenol hydroperoxide hydroxylation to produce catechol and hydroquinone, referred to as phenol for short. Catalyst for hydroxylation of quinone and its preparation method. Background technique [0002] Catechol and hydroquinone are important chemical raw materials. The traditional production process has problems such as complex production process, many by-products, and serious environmental pollution. [0003] Hydroxylation of phenol with hydroperoxide to co-produce catechol and hydroquinone has attracted more and more attention because of its fewer steps, mild reaction conditions, less by-products and less environmental pollution. The main difference between the already industrialized production processes lies in the catalysts used. There are certain deficiencies in the catalysts used in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/745C07C39/08C07C37/60
CPCY02P20/52
Inventor 沈玉龙舒世立王丽红
Owner TANGSHAN NORMAL UNIV
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