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Composite nanometer catalyst for electrocatalytic reduction of nitrobenzene

A nitrobenzene, electrocatalytic technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, nanotechnology for materials and surface science, etc., can solve the problems that are difficult to detect, Chemical properties are difficult to degrade, nitrobenzene is biological and environmental damage, etc., to achieve the effect of sensitive reduction current response, high stability, and enhanced catalytic performance

Inactive Publication Date: 2018-12-21
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because of its own toxicity and stable chemical properties, it is difficult to degrade, making nitrobenzene cause great harm to organisms and the environment
However, nitrobenzene is difficult to detect because it is slightly soluble in water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 30mg of graphene oxide (GO) and 20mL of thionyl chloride to a 50mL round bottom flask, ultrasonically disperse to dissolve it fully, then add 0.5mL of N,N-dimethylformamide, and then Stirred under reflux for 24 hours. After the reaction, distill off the unreacted thionyl chloride solution, then add a small amount of N,N-dimethylformamide to filter, wash the filter cake with deionized water 4 times, and dry the filter cake under vacuum to obtain acid chloride Graphene GO-COCl. It was prepared twice through the above steps to obtain 56 mg of GO-COCl. Then add 50mg GO-COCl and 40mL of anhydrous N,N-dimethylformamide into the round bottom flask, ultrasonically disperse to fully dissolve, then add 50mg of MnTAPP and 1.0mL of anhydrous triethylamine, slowly The temperature was raised to 135° C., and the reaction was carried out for 72 hours under the protection of nitrogen. After the reaction, cool to room temperature, add 300mL of anhydrous ether, let it stand still, ...

Embodiment 2

[0018] Add 36mg of graphene oxide (GO) and 30mL of thionyl chloride to a 50mL round bottom flask, ultrasonically disperse to dissolve it fully, then add 0.7mL of N,N-dimethylformamide, and then Under stirring and reflux for 30 hours. After the reaction, distill off the unreacted thionyl chloride solution, then add a small amount of N,N-dimethylformamide to filter, wash the filter cake with deionized water 4 times, and dry the filter cake under vacuum to obtain acid chloride Graphene GO-COCl. It was prepared twice through the above steps to obtain 60 mg of GO-COCl. Then add 60mg GO-COCl and 50mL of anhydrous N,N-dimethylformamide into the round bottom flask, ultrasonically disperse to fully dissolve, then add 55mg of MnTAPP and 1.5mL of anhydrous triethylamine, slowly The temperature was raised to 140° C., and the reaction was carried out for 50 hours under the protection of nitrogen. After the reaction, cool to room temperature, add 300mL of anhydrous ether, let it stand st...

Embodiment 3

[0021]Add 20mg of graphene oxide (GO) and 20mL of thionyl chloride into a 50mL round bottom flask, ultrasonically disperse to dissolve it fully, then add 0.5mL of N,N-dimethylformamide, and then Stir and reflux for 18 hours. After the reaction, distill off the unreacted thionyl chloride solution, then add a small amount of N,N-dimethylformamide to filter, wash the filter cake with deionized water 4 times, and dry the filter cake under vacuum to obtain acid chloride Graphene GO-COCl. After the above steps were prepared three times, 58 mg of GO-COCl was obtained. Then add 58mg GO-COCl and 50mL of anhydrous N,N-dimethylformamide into the round bottom flask, ultrasonically disperse to fully dissolve, then add 58mg of MnTAPP and 1.5mL of anhydrous triethylamine, slowly The temperature was raised to 145° C., and the reaction was carried out for 72 hours under the protection of nitrogen. After the reaction, cool to room temperature, add 350mL of anhydrous diethyl ether, let it sta...

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PUM

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Abstract

The invention discloses a preparation method of a graphene oxide@polymerizing metalloporphyrin composite nanometer catalyst with a shell-core coating structure for high-efficiency electrocatalytic reduction of nitrobenzene. The preparation method comprises the following steps of fixedly loading tetraaminophenyl manganese porphyrins onto the surface of graphene oxide by a covalent bonding method, and then coupling with the loaded manganese porphyrins via a conjugated bridging agent, so as to obtain a graphene oxide compound coated by a manganese porphyrins polymer film, namely the graphene oxide@polymerizing metalloporphyrin composite nanometer material. Proofed by the experiment results of electrocatalytic reduction of nitrobenzene using the graphene oxide@polymerizing metalloporphyrin compound, the preparation method has the advantages that under the synergistic function of the graphene oxide and the polymerizing metalloporphyrin film, compared with the glass carbon electrode modifiedby the graphene oxide, the reduction potential of the glass carbon electrode modified by the graphene oxide@polymerizing metalloporphyrin composite nanometer material is positively displaced with 50mV or above, and the more positive reduction potential is displayed; the response of the reduction current is more sensitive, the property is more stable, the property of nitrobenzene after catalytic reduction is more excellent, and the higher application value is realized in the electrochemical detection of trace nitrobenzene in the environment.

Description

technical field [0001] The invention relates to the field of a new type of catalyst for electrocatalytic reduction of nitrobenzene, in particular to a preparation method of a graphene oxide@metalloporphyrin composite nanomaterial and its application in electrocatalytic reduction of nitrobenzene. Background technique [0002] Nitrobenzene compounds are important chemical raw materials and are widely used in medicine, pesticides, industrial dyes, and chemical production. Because of its toxicity and stable chemical properties, it is difficult to degrade, which makes nitrobenzene cause great harm to organisms and the environment. However, nitrobenzene is difficult to detect because it is slightly soluble in water. Therefore, how to quickly and efficiently detect and decompose nitrobenzene compounds has attracted the attention of more and more scientific researchers. Currently, there are many methods for detecting nitrobenzene compounds, such as chromatography, spectrophotometr...

Claims

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Application Information

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IPC IPC(8): B01J31/22B82Y30/00B82Y40/00G01N27/30
CPCG01N27/308B82Y30/00B82Y40/00B01J31/1815B01J35/396
Inventor 阳卫军黄灿李营营
Owner HUNAN UNIV
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