Nitrogen-doped graphene quantum dot and preparation method thereof

A technology of graphene quantum dots and nitrogen doping, which is applied in the field of graphene, can solve the problems of limiting the wide application of nitrogen doped graphene quantum dots, difficulty in obtaining raw materials, troublesome and time-consuming operation, etc., and achieves excellent photocatalytic performance and production The effect of low equipment requirements and less impurities

Inactive Publication Date: 2016-07-27
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a nitrogen-doped graphene quantum dot and its preparation method, aiming to solve the difficulties in obtaining raw materials, expensive equipment, troublesome and time-consuming operation, and cumbersome process existing in the main methods of preparing nitrogen-doped graphene quantum dots at present. , low yield and many impurities limit the wide application of nitrogen-doped graphene quantum dots

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  • Nitrogen-doped graphene quantum dot and preparation method thereof
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  • Nitrogen-doped graphene quantum dot and preparation method thereof

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preparation example Construction

[0037] Such as figure 1 Shown, the preparation method of the nitrogen-doped graphene quantum dot of the embodiment of the present invention comprises the following steps:

[0038] S101: Preparation of graphene quantum dots: mix a certain amount of precursor pyrene with 80-100ml of fuming nitric acid, reflux and stir at a temperature of 80-100°C, perform nitro functional treatment on the surface of pyrene grains, and take out the reactants After filtration and removal of acid, add appropriate amount of NaOH to adjust the pH value to 7, use 300W ultrasonic dispersion treatment, transfer to a polytetrafluoroethylene tank, hydrothermally react at 180-200°C for 10-12h, and take out the reactant after natural cooling After filtration and dialysis, dry at 70°C to obtain graphene quantum dots with excellent optical properties;

[0039] S102: Preparation of nitrogen-doped graphene quantum dots with excellent optical properties: After stirring the prepared graphene quantum dots and amm...

Embodiment 1

[0042] 1) Weigh 1g of pyrene and 80ml of fuming nitric acid and stir slowly, stir at 80°C for 12h, and take out after natural cooling;

[0043] 2) Take out the reactant prepared in step 1, filter the waste liquid with a 0.22 μm microporous membrane, and wash the filtrate several times with deionized water;

[0044] 3) Add 0.4g NaOH to the reactant prepared in step 2, put it in 300W ultrasonic dispersion for 1h, then immediately put it into a high-temperature reactor, and react at a constant temperature of 180°C for 12h;

[0045] 4) After natural cooling, take out the reactant prepared in step 3, remove solid impurities with a 0.22 μm microporous membrane, and then dialyze with a 3500Da dialysis bag for 48 hours to remove excess ions in the reactant;

[0046] 5) Take out the reactant prepared in step 4, evaporate and dry at 70° C., and finally obtain graphene quantum dots.

Embodiment 2

[0048] 1) Weigh 0.1g of graphene quantum dots, add 100ml of deionized water, and use 300W ultrasonic wave to degrade for 10min to fully dissolve the graphene quantum dots in deionized water, then slowly add 100ml of ammonia water, and stir for 30min with a magnet to mix evenly;

[0049] 2) Transfer the mixture in step 1 to a polytetrafluoroethylene tank, and maintain a constant temperature hydrothermal reaction at 180°C for 24 hours in a high-temperature reactor;

[0050] 3) After natural cooling, take out the reactant prepared in step 2, remove solid impurities with a 0.22 μm microporous membrane, and then dialyze with a 3500Da dialysis bag for 48 hours to remove excess ions in the reactant;

[0051] 4) Take out the reactant prepared in step 3, evaporate and dry at 70° C., and finally obtain nitrogen-doped graphene quantum dots.

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Abstract

The invention discloses a nitrogen-doped graphene quantum dot and a preparation method thereof. The preparation method comprises the following steps: mixing a precursor pyrene with 80-100ml of fuming nitric acid, performing backflow stirring, performing nitro functional treatment on the surfaces of pyrene crystal grains, taking out the reactant, filtering to remove acid, adding a proper amount of NaOH, adjusting the pH value to 7, performing 300W ultrasonic dispersion treatment, transferring to a polytetrafluoroethylene tank, performing hydrothermal reaction, naturally cooling, taking out the reactant, filtering, dialyzing, and drying so as to obtain a graphene quantum dot; stirring the graphene quantum dot with ammonia water, sufficiently and uniformly mixing, transferring into a polytetrafluoroethylene tank, performing high-temperature high-pressure hydrothermal reaction, naturally cooling, taking out the reactant, and performing filtration dialysis, thereby obtaining the nitrogen-doped graphene quantum dot with excellent optical properties. The nitrogen-doped graphene quantum dot is simple in synthesis process step, high in yield, high in finished product rate and few in impurity. The nitrogen-doped graphene quantum dot disclosed by the invention can be stably dispersed in water, and is stable in structure, excellent in optical property and rich in group in surfaces.

Description

technical field [0001] The invention belongs to the technical field of graphene, in particular to a nitrogen-doped graphene quantum dot and a preparation method thereof. Background technique [0002] Since the discovery of single-layer graphene by Geim et al. at the University of Manchester in 2004, due to its unique and excellent physical and chemical properties, graphene has shown broad application prospects in research fields such as microelectronics, functional materials, and chemical sensing. Compared with graphene, graphene quantum dots exhibit stronger quantum confinement effects and boundary effects. In addition, graphene quantum dots also exhibit good biocompatibility, good water solubility, chemical stability, and low annihilation , stable optical properties, etc., so that it has a good application prospect in optoelectronic devices, sensors, and biological imaging. Due to the lack of an effective energy level structure and effective technical means for modulating...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01P2002/85C01P2004/04C01P2004/80
Inventor 李明骆毅唐涛李新宇文剑锋肖剑荣
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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