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A kind of graphene-supported iron-aluminum composite magnetic catalyst and its preparation method and application

A composite magnetic and catalyst technology, which can be used in chemical instruments and methods, oxidative preparation of carbonyl compounds, catalysts for physical/chemical processes, etc., and can solve problems such as low selectivity or conversion rate, no industrialization prospect, and difficulty in separating products from catalysts. , to achieve the effect of solving difficult separation

Inactive Publication Date: 2019-08-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above catalysts have disadvantages such as difficulty in separating the product from the catalyst, low selectivity or conversion, and no industrialization prospects.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The first step of catalyst preparation: 0.12 g of graphite oxide prepared by the Hummers method was dispersed in 120 mL of ethylene glycol and ultrasonically stripped for two hours, then aluminum nitrate nonahydrate (1.500 g, 4 mmol) and ferric chloride hexahydrate (1.081 g, 4mmol) and urea 1.3g continued to ultrasonically disperse for two hours, and then added 2mL of 1-methyl-2-pyrrolidone. Transfer the dispersed mixed solution to a polytetrafluoroethylene lining, put it into a high-pressure reactor, set the temperature to 180°C, and heat for 12 hours. Then take it out and let it cool naturally. The solid in the obtained reaction solution was centrifuged, washed, and then vacuum-dried for 12 hours, and then heat-treated in a tube furnace. The burning temperature was 400°C, and the temperature rate was 10°C / min. After reaching 400°C, react for 2 hours to obtain graphite Alkene-supported iron-aluminum composite magnetic catalysts.

[0029] The second step catalytic rea...

Embodiment 2

[0031]The first step of catalyst preparation: Disperse 0.12 g of graphite oxide prepared by the Hummers method in 120 mL of water and ultrasonically peel it off for two hours, then add aluminum nitrate nonahydrate (0.6 g, 1.6 mmol) and iron nitrate nonahydrate (0.6 g, 1.5 mmol) And 0.96 g of melamine was continued to be ultrasonically dispersed for two hours, and then 1.8 mL of 1-methyl-2-pyrrolidone was added. Transfer the dispersed mixed solution to a polytetrafluoroethylene lining, put it into a high-pressure reactor, set the temperature to 180°C, and heat for 20 hours. Then take it out and let it cool naturally. The solids in the obtained reaction solution were centrifuged and washed, then vacuum-dried for 12 hours, and then heat-treated in a tube furnace. The burning temperature was 300°C, and the temperature rate was 10°C / min. After reaching 300°C, react for 6 hours to obtain graphite Alkene-supported iron-aluminum composite magnetic catalysts.

[0032] The second step...

Embodiment 3

[0034] The first step of catalyst preparation: Disperse 0.12 g of graphite oxide prepared by the Hummers method in 120 mL of DMF and ultrasonically peel it off for two hours, then add aluminum nitrate nonahydrate (1.2 g, 3.2 mmol) and ferric chloride hexahydrate (1.44 g, 5.3 mmol) and 2.4 g of N-methyl-N-ethyl-p-toluidine continued to be ultrasonically dispersed for two hours, and then 2.3 mL of 1-methyl-2-pyrrolidone was added. Transfer the dispersed mixed solution to a polytetrafluoroethylene lining, put it into a high-pressure reactor, set the temperature to 180°C, and heat for 10 hours. Then take it out and let it cool naturally. The solid in the obtained reaction solution was centrifuged, washed, and then vacuum-dried for 12 hours, and then heat-treated in a tube furnace. The burning temperature was 500°C and the temperature rate was 10°C / min. After reaching 500°C, react for 8 hours to obtain graphite Alkene-supported iron-aluminum composite magnetic catalysts.

[0035]...

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Abstract

The invention discloses a graphene-loading iron and aluminum composite magnetic catalyst as well as a preparation method and application thereof. The preparation method of the catalyst comprises the following steps: adding graphite oxide prepared with a Hummers method in a polar solvent, carrying out ultrasonic peeling to obtain graphene oxide, then adding aluminum nitrate nonahydrate, iron salts and a nitrogen-containing reagent to continuously carry out ultrasonic dispersion, then adding 1-methyl-2-pyrrolidone, transferring a reaction solution into a high-pressure reactor to carry out heating reaction, and then carrying out thermal treatment with a tube furnace to obtain the graphene-loading iron and aluminum composite magnetic catalyst. The graphene-loading iron and aluminum composite magnetic catalyst prepared by the method carries out catalytic oxidation on benzyl alcohol to produce benzaldehyde, the time required by reaction is short, the conversion ratio is 80 percent or above, and the selectivity is 99 percent; because of special magnetism, the graphene-loading iron and aluminum composite magnetic catalyst can be separated from a reaction system under the action of an external magnetic field, so that the separation cost of the reaction solution and the catalyst is lowered, and the production cost can also be lowered; and in addition, the graphene-loading iron and aluminum composite magnetic catalyst is good in recycling performance and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and in particular relates to a graphene-supported iron-aluminum composite magnetic catalyst, a preparation method thereof and an application in preparing benzaldehyde by catalytic oxidation. Background technique [0002] Benzaldehyde is a very important fine chemical intermediate, widely used in medicine, pesticide, cosmetics and other fields. At present, the preparation methods of benzaldehyde are mainly chlorination hydrolysis, gas phase oxidation and liquid phase oxidation using toluene as raw material. Chlorination hydrolysis is one of the most commonly used methods to prepare benzaldehyde in industry. Toluene is chlorinated in the side chain under appropriate conditions, and then acidic or alkaline hydrolysis and rectification can be used to obtain benzaldehyde. Benzoic acid is the process major by-products. The reaction process of this method is long and complicated, the reaction con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745C07C45/29C07C47/54
Inventor 戴立言李启晨张玲玲王晓钟陈英奇
Owner ZHEJIANG UNIV
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