Highly-efficient preparation method for strong-fluorescence graphene quantum dot

A technology of graphene quantum dots and fluorescence, which is applied in the field of nano-fluorescent materials, can solve the problems of complex synthesis mechanism, harsh reaction conditions, and low synthesis yield, and achieve the effect of simple synthesis operation process, wide process window, and mild reaction

Pending Publication Date: 2019-05-03
QUANZHOU NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

From top to bottom, the C=C bond is destroyed by chemical or physical means, and the large-sized carbon source precursor is cut into small-sized quantum dots. Common methods include hydrothermal method, electrochemical method, chemical exfoliation method, and acid oxidation. The advantage is that the selected raw materials are low in price and suitable for large-scale preparation. The disadvantages are harsh reaction conditions, long preparation cycle, low yield, difficult contro...

Method used

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  • Highly-efficient preparation method for strong-fluorescence graphene quantum dot
  • Highly-efficient preparation method for strong-fluorescence graphene quantum dot
  • Highly-efficient preparation method for strong-fluorescence graphene quantum dot

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 40g of pyrene and put it into a 5L water-bath reactor, then add 3.2L of concentrated nitric acid with a concentration of 67wt%, slowly adjust the stirring speed to 150r / min, and set the temperature of the water bath at 60-80°C to make the reaction solution react at a constant temperature in a swirl state After cooling to room temperature for 10-24 hours, add 5-10 times the volume of deionized water to dilute, then perform suction filtration, rinse and dry to obtain about 64.5 g of surface nitro-functionalized intermediate product 1,3,6-trinitropyrene. Using ethanol as a solvent, measure 20ml of hydrazine hydrate and 980ml of ethanol to prepare an alkaline solution with a concentration of 2% by volume, then weigh 5g of 1,3,6-trinitropyrene solid and disperse it in the solution, and ultrasonicate under the condition of power 300W Pulverize for 1 hour to obtain a 1,3,6-trinitropyrene suspension with a concentration of 5 mg / ml. The above suspension was transferred to ...

Embodiment 2

[0029] Configure 980ml of mixed solvents with a volume ratio of pure water and ethanol of 1:1, then add 20ml of hydrazine hydrate to configure an alkaline solution with a volume percentage concentration of 2%, then weigh 5g of the 1,3,6-trinitrogen prepared in Example 1 The pyrene solid was dispersed in the solution and ultrasonically pulverized for 1 hour at a power of 300W to obtain a suspension with a 1,3,6-trinitropyrene concentration of 5 mg / ml. The above suspension was transferred to a 5L high-pressure polytetrafluoroethylene reactor, sealed, and hydrothermally reacted in an oven at 200°C for 10 hours. After cooling, a tan solution with a graphene quantum dot content of about 1.45g was obtained. After the reaction, the solution was suction-filtered, and 5ml of the filtrate sample was taken for a fluorescence comparison test, and the remaining solution was dried to obtain graphene quantum dot powder.

[0030] The parameters of the fluorescence spectrometer were fixed, and...

Embodiment 3

[0032] Using ethanol as a solvent, measure 20ml of hydrazine hydrate and 980ml of ethanol to configure an alkaline solution with a concentration of 2% by volume, then weigh 15g of the 1,3,6-trinitropyrene solid prepared in Example 1 and disperse it in the solution Ultrasonic pulverization for 1 hour under the condition of power 300W to obtain a suspension with a concentration of 15 mg / ml of 1,3,6-trinitropyrene. Transfer the suspension to a 5L high-pressure polytetrafluoroethylene reactor, seal it, and react it hydrothermally in an oven at 200°C for 10 hours. After cooling, the content of graphene quantum dots is about 8.7g. volume mean) black solution. After the reaction, the solution was suction-filtered, and 5ml of the filtrate sample was taken for a fluorescence comparison test, and the remaining solution was dried to obtain graphene quantum dot powder.

[0033] The parameters of the fluorescence spectrometer were fixed, and it was found through testing that the fluoresce...

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Abstract

The invention discloses a highly-efficient preparation method for a strong-fluorescence graphene quantum dot. The highly-efficient preparation method comprises the following steps: with pyrene as a reactant precursor and concentrated nitric acid as a nitrating agent, mixing the pyrene with the concentrated nitric acid in proportion, subjecting a mixed solution to water-bath heating to a constant low temperature of 60 to 80 DEG C under a reflux state, and carrying out a nitration reaction so as to obtain an intermediate product namely 1,3,6-trinitropyrene; and dissolving the intermediate product and an alkaline substance namely hydrazine hydrate into a solvent in a certain proportion, carrying out ultrasonic crushing so as to obtain an ultrasonically-crushed suspension, then transferring the suspension to a high-pressure-resistant reaction kettle, carrying out a hydrothermal reaction so as to synthesize a graphene quantum dot solution with high quantum efficiency, and carrying out vacuum filtering, drying and collection so as to obtain a graphene quantum dot powder. The method provided by the invention has the advantages of simple and highly-efficient preparation process, low cost,high quantum efficiency, environmental protection, no generation of harmful wastes and convenience in large-scale production, and facilitates promotion of graphene quantum dot application.

Description

technical field [0001] The invention belongs to the technical field of nano fluorescent materials, and in particular relates to a high-efficiency preparation method of strongly fluorescent graphene quantum dots. Background technique [0002] Graphene quantum dots (GQDs) are quasi-zero-dimensional materials that can reach the thickness of a single atom. Due to the remarkable quantum confinement effect and edge effect presented by its quasi-zero-dimensional characteristics, it has many unique thermal, electrical and Optical properties have attracted extensive attention of many domestic and foreign researchers in the past ten years. Compared with traditional fluorescent materials and other semiconductor quantum dots, GQDS has the advantages of abundant raw materials, low price, low toxicity, stable structure, easy surface functionalization, adjustable bandgap width range, good biocompatibility, and superior fluorescence performance. . These characteristics make GQDS have grea...

Claims

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Application Information

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IPC IPC(8): C01B32/184C09K11/65B82Y20/00
Inventor 颜少彬廖廷俤郑玲玲张璐吴琦朱星群崔旭东向斌
Owner QUANZHOU NORMAL UNIV
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