Nitrogen and sulfur-codoped graphene quantum dot and preparation method thereof

A graphene quantum dot, nitrogen-sulfur technology, applied in the field of graphene, can solve the problems of limiting the wide application of nitrogen-sulfur co-doped graphene quantum dots, difficulty in obtaining raw materials, troublesome and time-consuming operation, etc., and achieves excellent photocatalytic effect, excellent Optical performance, low equipment requirements

Inactive Publication Date: 2016-05-11
GUILIN UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

[0004] The object of the present invention is to provide a nitrogen-sulfur co-doped graphene quantum dot and its preparation method, aiming at solving the problems of expensive equipment, cumbersome and time-consuming operation, cumbersome proce

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  • Nitrogen and sulfur-codoped graphene quantum dot and preparation method thereof
  • Nitrogen and sulfur-codoped graphene quantum dot and preparation method thereof
  • Nitrogen and sulfur-codoped graphene quantum dot and preparation method thereof

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preparation example Construction

[0036] Such as figure 1 As shown, the preparation method of the nitrogen-sulfur co-doped graphene quantum dots of the embodiment of the present invention comprises the following steps:

[0037] 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 filtering and removing acid, add an appropriate amount of NaOH to adjust the pH value, use 300W ultrasonic dispersion treatment, transfer it to a polytetrafluoroethylene tank, and conduct a hydrothermal reaction at a temperature of 180-200°C for 10-12h, and take out the reactant after natural cooling for filtration and dialysis After drying at 70°C, graphene quantum dots with rich groups on the surface and excellent optical properties are obtained.

[0038] S102: One-step synthesis of nitrogen-sulfur co-doped graphene qua...

Embodiment 1

[0041] 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;

[0042]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;

[0043] 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;

[0044] 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;

[0045] 5) Take out the reactant prepared in step 4, evaporate and dry at 70° C., and finally obtain graphene quantum dots.

Embodiment 2

[0047] 1) Take by weighing 0.1g of graphene quantum dots prepared in Example 1, add 100ml of deionized water, degrade 10min with ultrasonic wave 300W to make graphene quantum dots fully dissolve in deionized water, then slowly add 100ml of ammonia water, under magnetic stirring conditions Slowly add 0.25g of sublimed sulfur according to the ratio of the reactants, and stir for 30min to fully disperse the sublimed sulfur in the mixture;

[0048] 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;

[0049] 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;

[0050] 4) Take out the reactant prepared in step 3, evaporate and dry at 70° C., and finally obtain nitrogen-sulfur co-doped g...

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Abstract

The invention discloses a nitrogen and sulfur-codoped graphene quantum dot and a preparation method thereof. The preparation method comprises the steps that after a precursor pyrene is mixed with 80-100 ml of fuming nitric acid, refluxing and stirring are performed, nitro functionalizing treatment is performed on the surfaces of pyrene grains, a reactant is taken out, filtered and deacidified, an appropriate amount of NaOH is added to regulate the PH value, dispersion treatment is performed by adopting 300-W ultrasonic waves, the reactant is transferred into a polytetrafluoroethylene tank for a hydrothermal reaction, and after natural cooling is performed, a reactant is taken out, filtered, dialyzed and then dried; after a graphene quantum dot is dissolved into an appropriate amount of deionized water, an appropriate amount of ammonia water is added according to the proportion of the reactant, uniform mixing is performed, the mixture and an appropriate amount of sublimed sulfur are fully mixed to be uniform through stirring, the mixture is transferred into a polytetrafluoroethylene tank, a hydrothermal reaction is performed for 24 h by keeping the temperature of 180 DEG C-200 DEG C, and after cooling is performed, a reactant is taken out, filtered and dialysed to obtain the nitrogen and sulfur-codoped graphene quantum dot. The preparation method is simple in synthesis process, high in yield and finished product rate, environmentally friendly, poisonless, few in impurity and capable of easily obtaining the raw materials.

Description

technical field [0001] The invention belongs to the technical field of graphene, in particular to a nitrogen-sulfur co-doped graphene quantum dot and a preparation method thereof. Background technique [0002] Graphene is made of sp 2 A two-dimensional honeycomb crystal composed of hybridized carbon atoms. Because of its unique structure and properties, graphene material has quickly become the most eye-catching newcomer of carbon materials after carbon nanotubes since it was discovered in 2004. In 2010, the Nobel Prize in Physics was awarded to graphene discoverers to promote this research hotspot. Toward a new climax, high-quality graphene materials and their applications have become another scientific and technological commanding height for scientists from all over the world to compete. With the continuous development of graphene, graphene quantum dots have unique advantages in biological imaging due to their good biocompatibility and extremely stable optical properties,...

Claims

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Application Information

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IPC IPC(8): C09K11/65B01J27/24C02F1/30C02F101/38
CPCB01J27/24C02F1/30C02F2101/40C02F2305/10C09K11/65
Inventor 李明骆毅文剑锋唐涛李新宇肖剑荣
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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