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Nitrogen-doped graphene catalyst as well as preparation method and application thereof

A nitrogen-doped graphene and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of expensive raw materials, unsatisfactory effects, and high technical requirements, and achieve a simple method. , the effect of rich oxygen-containing groups and cheap raw materials

Inactive Publication Date: 2015-04-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the effect of post-treatment is not very ideal. The CVD method in in-situ nitrogen doping is more commonly used, but the technical requirements are high, it is not easy to control, and the price of raw materials is relatively expensive.

Method used

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  • Nitrogen-doped graphene catalyst as well as preparation method and application thereof
  • Nitrogen-doped graphene catalyst as well as preparation method and application thereof
  • Nitrogen-doped graphene catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of nitrogen-doped graphene

[0041] NG950 7.5 / 2.5 / 0.8 The preparation process is as follows: take 7.5g of urea, 2.5g of melamine and 0.8g of glucose, and put them into a drying oven at 80°C for 24 hours. Mix and grind the medicine in a crucible evenly, put it into a covered crucible and calcinate at 550°C for 3h. Take it out and cool it, grind it evenly, and then calcinate it in a tube furnace at 950°C for 1h.

[0042] (NGT X / Y / Z , where T is the tube furnace temperature, X is the amount of urea, Y is the amount of melamine, and Z is the amount of glucose (the default temperature of the muffle furnace is 550°C). CNt x / y / z , t is the temperature of the muffle furnace, x is the amount of urea, y is the amount of melamine, z is the amount of glucose)

[0043] Of which NG900 6.7 / 3.3 / 1 、NG900 7.5 / 2.5 / 1 、NG900 8.0 / 2.0 / 1 、NG850 7.5 / 2.5 / 1 、NG950 7.5 / 2.5 / 1 、NG1000 7.5 / 2.5 / 1 、NG950 7.5 / 2.5 / 1.2 、NG950 7.5 / 2.5 / 0.6 Prepare as above.

[0044] Through the nit...

Embodiment 2

[0046] XPS Characterization of Nitrogen-doped Graphene

[0047] NG950 7.5 / 2.5 / 1 、NG950 7.5 / 2.5 / 0.8 、NG950 7.5 / 2.5 / 0.6 The XPS tests of the three kinds of nitrogen-doped graphene were carried out on a multifunctional X-ray photoelectron spectrometer (model Axis Ultra DLD), and the vacuum degree of the analysis chamber was about 5×10 -9 torr, the X light source used is a monochromatic Al Kα source (Mono AlKα), the energy is 1486.6eV, 10mA×15KV, and the beam spot size is 700×300μm; The energy is 40eV, and the number of scans is 1 time. Before the result analysis, the C1s and N1s of each sample were first divided into peaks, and then the binding energy of C1s at the lowest energy end was calibrated to 284.6eV, and the N1s element was corrected according to the shift of the C1s peak position.

[0048] Through this example to NG950 7.5 / 2.5 / 1 、NG950 7.5 / 2.5 / 0.8 and NG950 7.5 / 2.5 / 0.6 XPS analysis of three materials, in which nitrogen is divided into four peaks, representing fou...

Embodiment 3

[0050] XRD Characterization of Nitrogen-doped Graphene Catalysts

[0051] XRD analysis: used to analyze NGT X / Y / Z The crystal structure of the catalyst, the test process is realized on the D8ADVANCE instrument, the test conditions are copper target, incident ray λ=0.15418nm, Ni filter, tube pressure 40KV, tube flow 40mA; scan step size 0.02 degrees, scan speed 0.1 sec / step; slit DS0.5°RS8mm (corresponding to LynxExe array detector).

[0052] Through the XRD analysis of the nine catalysts in this example, the presence of a strong diffraction peak around 2θ=26° proves the existence of a graphitized structure, proving that the material is graphene. With the change of raw material ratio or temperature, 2θ did not change greatly, indicating that the graphitized structure did not change greatly. However, when the ratio of urea and melamine is changed, NG900 7.5 / 2.5 / 1 The performance is the best, but the peak intensity is the lowest, indicating that nitrogen has a greater influenc...

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Abstract

The invention discloses a nitrogen-doped graphene catalyst as well as a preparation method and application thereof. The preparation method comprises the following steps: drying and dehydrating glucose and urea, and mixing with melamine, wherein the mass ratio of the urea to melamine is 2-4; uniformly grinding the mixture, and calcining the mixture into a muffle furnace at the temperature of 550 DEG C for 3 hours; cooling and grinding uniformly, adding the mixture into a tube furnace, introducing into nitrogen protection, calcining at the temperature of 850-1000 DEG C for an hour, thereby obtaining the nitrogen-doped graphene catalyst. According to the in-situ nitrogen-doped graphene disclosed by the invention, the used raw materials are low in price, the method is simple, the yield is high, and graphite-like nitrogen doped graphene with the highest ratio is obtained by changing the rate of the raw materials and the temperature, so that the catalyst has a good oxidation-reduction effect, and expensive Pt can be replaced to a certain degree.

Description

technical field [0001] The invention belongs to the field of biological energy materials, and in particular relates to a preparation method and application of a nitrogen-doped graphene catalyst. Background technique [0002] Microbial fuel cells (MFCs) are an advanced energy technology that uses microorganisms as catalysts to convert the chemical energy of organic matter into electrical energy. At present, there are two major crises of environmental pollution and resource shortage in the human world. MFCs have become a research hotspot in the field of environmental protection by processing organic waste (including organic wastewater and organic solid waste) while generating electricity to achieve a win-win situation in waste treatment and energy recovery. [0003] So the scale-up of the microbial fuel cell system is the main problem faced at present. The key to the scale-up of microbial fuel cells is direct (no need to add exogenous electron transfer intermediates), single-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24H01M4/90
CPCY02E60/50
Inventor 朱能武杨婷婷黄健键吴平霄
Owner SOUTH CHINA UNIV OF TECH
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