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Anti-stacking nitrogen doped three-dimensional graphene and preparation method thereof

A graphene and nitrogen-doped technology, applied in chemical instruments and methods, hydrogen production, inorganic chemistry, etc., can solve problems such as performance impact, achieve good stability, high catalytic efficiency, and be conducive to sustainable development

Inactive Publication Date: 2017-05-31
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide an anti-stacking nitrogen-doped 3D graphene and its preparation method to solve the impact of graphene stacking and defects on the performance of graphene-based photocatalytic materials. The prepared anti-stacking nitrogen-doped In the case of heterogeneous 3D graphene loaded with a mass ratio of 10% noble metal Pt, efficient eosin Y-sensitized photolysis of water for hydrogen production can be achieved

Method used

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  • Anti-stacking nitrogen doped three-dimensional graphene and preparation method thereof
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  • Anti-stacking nitrogen doped three-dimensional graphene and preparation method thereof

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Effect test

Embodiment 1

[0028] Add 80 mL of 1 mg / mL graphene oxide aqueous solution into the reactor, then heat it in water at 180 °C for 10 h, then centrifuge and wash the obtained solid three times, and dry it at 60 °C for 12 h to obtain stacked graphene;

[0029] Take 10 mg of stacked graphene and 40 mg of Eosin Y solid into 70 mL of aqueous solution, sonicate for 30 min, add 0.50 mL of 10 mM H 2 PtCl 6 and 10 mL of triethanolamine, and degas the reaction system while maintaining a constant temperature of 5 °C. Then, the reaction system was irradiated with visible light with a wavelength greater than 420 nm for 30 min. Afterwards, the system was degassed to keep the system in a vacuum state. The reaction system was irradiated with visible light with a wavelength greater than 420 nm, and the hydrogen production was detected online by gas chromatography, with argon as the carrier gas. After 2 h of light irradiation, the hydrogen production in the system was detected.

Embodiment 2

[0031] Add 15 mL of 10 mg / mL graphene oxide aqueous solution into the reaction kettle, and then hydroheat at 180 °C for 10 h, and then freeze-dry the obtained columnar graphene to obtain 3D graphene;

[0032] Take 10 mg of prepared 3D graphene and 40 mg of Eosin Y solid into 70 mL solution, sonicate for 30 min, add 0.50 mL of 10mM H 2 PtCl 6 and 10 mL of triethanolamine, and degas the reaction system while maintaining a constant temperature of 5 °C. Then, the reaction system was irradiated with visible light with a wavelength greater than 420 nm for 30 min. Afterwards, the system was degassed to keep the system in a vacuum state. The reaction system was irradiated with visible light with a wavelength greater than 420 nm, and the hydrogen production was detected online by gas chromatography, with argon as the carrier gas. After 2 h of light irradiation, the hydrogen production in the system was detected.

Embodiment 3

[0034] Add 350 mg melamine and 1.5 mL 37wt% formaldehyde to 15 mL 10 mg / mL graphene oxide aqueous solution, heat at 180 °C for 10 h, then centrifuge, wash, and dry to obtain stack-resistant graphene oxide. Put anti-stacking graphene oxide into a tube furnace, calcined at 750 °C for 5 h under the protection of nitrogen atmosphere (heating rate is 5 °C per minute), and then cool down naturally to obtain anti-stacking nitrogen-doped 3D graphene;

[0035] Take 10 mg of anti-stacking nitrogen-doped 3D graphene and 40 mg of Eosin Y solid into 70 mL of solution, sonicate for 30 min, add 0.50 mL of 10mM H 2 PtCl 6 and 10 mL of triethanolamine, and degas the reaction system while maintaining a constant temperature of 5 °C. Then, the reaction system was irradiated with visible light with a wavelength greater than 420 nm for 30 min. Afterwards, the system was degassed to keep the system in a vacuum state. The reaction system was irradiated with visible light with a wavelength greater ...

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Abstract

The invention discloses anti-stacking nitrogen doped three-dimensional graphene and a preparation method thereof. The preparation method comprises the following steps: hydrothermally preparing anti-stacking graphene oxide by using melamine, a formaldehyde aqueous solution with a concentration of 37wt% and a graphene oxide aqueous solution; and calcining the prepared anti-stacking graphene oxide under a nitrogen atmosphere so as to be able to obtain the anti-stacking nitrogen doped three-dimensional graphene. According to the invention, the catalyst has good eosin Y sensitized photocatalytic water-splitting hydrogen production activity after loaded with precious metal PT with a mass ratio of 10% under illumination of visible light; and the preparation method is simple and practicable, and the catalyst is cheap and can be conveniently recycled, so the composite photocatalic material has extensive practicable values and application prospects in the technical files of material preparation and the field of photocatalytic water-splitting hydrogen production.

Description

technical field [0001] The invention belongs to the field of photocatalytic material preparation and photocatalytic technology, and in particular relates to a three-dimensional graphene resistant to stacking nitrogen doping and a preparation method thereof. Background technique [0002] In recent years, graphene, a material with unique two-dimensional morphology, excellent electrical conductivity and large theoretical specific surface area, has received extensive attention and applications in the field of photocatalysis. In the field of photocatalysis, the commonly used preparation method of graphene is the modified Hummers method. The experimental operation of this graphene preparation method is relatively simple, and the output of graphene is relatively high, and a certain amount of oxygen-containing functional groups can be introduced on the surface of graphene, which is conducive to increasing the stability of graphene in different solvents (aqueous and organic phases). ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J21/18B01J23/42C01B3/04
CPCC01B3/042B01J21/18B01J23/42B01J27/24C01B2203/0277C01B2203/107B01J35/39Y02E60/36
Inventor 徐艺军翁波
Owner FUZHOU UNIV
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