Preparation method of Co4S3 / nitrogen doped graphene composite material and application thereof

A technology of nitrogen-doped graphene and composite materials, which is applied in the fields of analyzing materials, electrochemical variables of materials, and material analysis by electromagnetic means, and can solve the problems of low sensitivity and selectivity of electrochemical sensing, narrow linear response range, raw materials, etc. Excessive consumption and other problems, to achieve the effect of wide detection linear range, easy separation and purification, and less raw material consumption

Active Publication Date: 2017-06-30
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the defects such as complex synthetic process of modifier, excessive consumption of raw materials, harsh reaction conditions, low sensitivity and selectivity of electrochemical sensing, and narrow linear response range in the existing electrochemical sensor technology for measuring hydrogen peroxide. , through a simple reaction process, relatively mild reaction conditions, a green reaction environment, and an efficient separation method to prepare a new type of Co with strong electrocatalysis 4 S 3 / Nitrogen-doped graphene composite material, and make full use of graphene with unique properties as an excellent carrier doping Co which can significantly improve electronic activity and electron transfer performance 4 S 3 Nanomaterials for Sensitive and Selective Determination of Hydrogen Peroxide

Method used

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  • Preparation method of Co4S3 / nitrogen doped graphene composite material and application thereof
  • Preparation method of Co4S3 / nitrogen doped graphene composite material and application thereof
  • Preparation method of Co4S3 / nitrogen doped graphene composite material and application thereof

Examples

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Effect test

Embodiment 1

[0032] (1) Weigh 50 mg of graphene oxide powder in 50 mL of twice distilled water, and disperse it into a uniform solution by ultrasonication for 2 hours.

[0033] (2) Adjust the graphene dispersion to a pH of about 9 with ammoniacal liquor with a mass concentration of 30%, then add 0.8mL of hydrazine hydrate with a mass concentration of 85% and stir for 15 minutes, and heat the resulting mixed solution at 40°C Reflux for 36 hours.

[0034] (3) After the reaction, centrifuged and washed several times with secondary water and ethanol, and finally the centrifuged product was dried in a vacuum oven at 15° C. for 18 hours to obtain nitrogen-doped graphene powder.

[0035] (4) Take by weighing 15mg of nitrogen-doped graphene powder in a mixed solution of 70mL of secondary water and ethanol (1.0:1.0), ultrasonic for 30 minutes, after making it uniformly dispersed, add 525mg of cobalt acetate tetrahydrate and 140mg of thiourea, Continue to sonicate for 15 minutes and stir to dissolv...

Embodiment 2

[0037] (1) Weigh 50 mg of graphene oxide powder in 50 mL of twice distilled water, and disperse it into a uniform solution by ultrasonication for 3 hours.

[0038] (2) Adjust the graphene dispersion to a pH of about 10 with ammoniacal liquor with a mass concentration of 30%, then add 1.0 mL of hydrazine hydrate with a mass concentration of 85% and stir for 8 minutes, and place the resulting mixed solution at 50° C. Heat to reflux for 24 hours.

[0039] (3) After the reaction, centrifuge and wash with secondary water and ethanol for several times, and finally dry the centrifuged product in a vacuum oven at 20° C. for 15 hours to obtain nitrogen-doped graphene powder.

[0040] After the reaction was completed, it was centrifuged, the product was washed three times with absolute ethanol, and the product was vacuum-dried at 50°C for 12h

[0041] (4) Take by weighing 15mg of nitrogen-doped graphene powder in the mixed solution of 70mL of secondary water and ethanol (1.2:1.0), ultr...

Embodiment 3

[0043] (1) Weigh 50 mg of graphene oxide powder in 50 mL of twice distilled water, and disperse it into a uniform solution by ultrasonication for 4 hours.

[0044] (2) Adjust the graphene dispersion to a pH of about 10 with ammoniacal liquor with a mass concentration of 30%, then add 1.2mL of hydrazine hydrate with a mass concentration of 85% and stir for 10 minutes, and place the resulting mixed solution at 50°C Heat to reflux for 24 hours.

[0045] (3) After the reaction, centrifuged and washed several times with secondary water and ethanol, and finally the centrifuged product was dried in a vacuum oven at 30° C. for 12 hours to obtain nitrogen-doped graphene powder.

[0046] (4) Take by weighing 15mg of nitrogen-doped graphene powder in the mixed solution of 70mL of secondary water and ethanol (1.0:1.0), ultrasonic for 30 minutes, after making it uniformly dispersed, add 560mg of cobalt acetate tetrahydrate and 170mg of thiourea, Continue to sonicate for 15 minutes and sti...

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Abstract

The invention discloses a preparation method of a Co4S3 / nitrogen doped graphene composite material and application thereof, and belongs to the field of inorganic material synthesis and analysis. The composite material is prepared as follows: firstly using ammonia water to regulating alkaline environment, then using hydrazine hydrate and graphene oxide for reaction and conversion into nitrogen doped graphene, and then adding cobalt acetate and thiourea to prepare the Co4S3 / nitrogen doped graphene composite material by a solvent thermal process. The method has simple process and low cost, the main reaction is performed in an aqueous phase, reaction conditions are mild, an electrochemical sensor constructed by use of the Co4S3 / nitrogen doped graphene composite material can show a strong catalytic effect on electrochemical reduction of hydrogen peroxide because of synergistic effect of the nitrogen doped graphene with a high surface area, high conductivity and good biocompatibility and a Co4S3 nano material with good electronic transfer characteristics, and the electrochemical sensor has the advantages of wide detection linear range, low detection limit and high sensitivity and selectivity, and is successfully used to detect the hydrogen peroxide in real samples.

Description

technical field [0001] The invention belongs to the field of synthesis and analysis of inorganic materials, in particular to a simple method for preparing Co 4 S 3 / Nitrogen-doped graphene composites and their applications. Background technique [0002] As an important chemical product, hydrogen peroxide is widely used in textile, chemical industry, papermaking, electronics, food hygiene and other fields. At the same time, hydrogen peroxide is also the active product of all enzymes in the human body except oxidase. Its Excessive content will directly lead to human cell damage or aging, and then imbalance. Toxicological studies have also confirmed that a certain amount of hydrogen peroxide has a strong stimulating and damaging effect on human mucous membranes. Therefore, rapid quantitative detection of hydrogen peroxide is of great significance. The detection methods of hydrogen peroxide include fluorescence method, chromatography method, photometric method and capillary ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30G01N27/48
CPCG01N27/308G01N27/48
Inventor 魏先文张琴吴芳辉杨俊卿
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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