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Preparation method of nitrogen-doped graphene quantum dot dispersion liquid

A graphene quantum dot and dispersion technology, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as unfavorable large-scale industrial production, high equipment requirements, limited output, etc., to achieve dangerous green environmental protection, monodispersity, etc. good, less dangerous effect

Inactive Publication Date: 2015-12-30
UNIV OF ELECTRONIC SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is a one-step method, and the solvothermal method involves the regulation of temperature and pressure, which requires high equipment and needs to be carried out in a closed container, which limits the output.
[0013] Existing processes generally require high temperature, high pressure and strong acid, as well as several hours to several days of reaction time. Some methods also need complex processes to first synthesize graphene, graphene oxide, etc., and multi-step synthesis is not conducive to large-scale Industrial production

Method used

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  • Preparation method of nitrogen-doped graphene quantum dot dispersion liquid
  • Preparation method of nitrogen-doped graphene quantum dot dispersion liquid
  • Preparation method of nitrogen-doped graphene quantum dot dispersion liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Weigh 10g of glucose, dissolve it in 500ml of pure water, add 5ml of ammonia water to make a mixed solution;

[0035] (2) Transfer the mixed solution to a glass non-airtight container, and carry out microwave irradiation reaction, the microwave power is 450W, and the irradiation time is 5min;

[0036] figure 1 It is a schematic diagram of the mechanism for preparing nitrogen-doped graphene quantum dots in the present invention. Under the action of ammonia water and microwave irradiation, glucose forms a compound with pyridine nitrogen and pyrrole nitrogen under a series of actions such as dehydration condensation, small molecule polymerization, doping, and carbonization. Two forms of doped graphene quantum dots.

[0037] (3) heat the liquid obtained from the above reaction at 40° C., stir and heat for 1 hour, and remove excess ammonia;

[0038]The boiling point of ammonia water is about 36°C, and keeping the liquid at 40°C is very suitable for the present inventio...

Embodiment 2

[0041] (1) Weigh 10g of glucose, dissolve it in 100ml of pure water, add 5ml of ammonia water to make a mixed solution;

[0042] (2) Transfer the mixed solution to a polypropylene plastic non-airtight container, and carry out microwave irradiation reaction, the microwave power is 720W, and the irradiation time is 2min;

[0043] (3) heat the liquid obtained from the above reaction at 40° C., stir and heat for 1 hour, and remove excess ammonia;

[0044] (4) Put the liquid obtained from the above treatment into a dialysis bag with a molecular weight cut-off of 500 Da, and perform centrifugal dialysis for 20 min at a speed of 8000 rpm to obtain a nitrogen-doped graphene quantum dot dispersion.

[0045] figure 2 The transmission electron microscope figure of the nitrogen-doped graphene quantum dot prepared for the present invention, as can be seen from the figure, the nitrogen-doped graphene quantum dot prepared by this method has excellent monodispersity, the size is about 5nm, ...

Embodiment 3

[0047] (1) Weigh 10g of glucose, dissolve it in 10ml of pure water, add 1ml of ammonia water to make a mixed solution;

[0048] (2) Transfer the mixed solution to a polypropylene plastic non-airtight container, and carry out microwave irradiation reaction, the microwave power is 450W, and the irradiation time is 2min;

[0049] (3) heat the liquid obtained from the above reaction at 40° C., stir and heat for 1 hour, and remove excess ammonia;

[0050] (4) Put the liquid obtained from the above-mentioned treatment into a dialysis bag with a molecular weight cut-off of 1000 Da, and perform centrifugal dialysis for 20 min at a speed of 8000 rpm to obtain a nitrogen-doped graphene quantum dot dispersion.

[0051] image 3 For the X-ray photoelectron energy spectrum of the nitrogen-doped graphene quantum dot prepared by the present invention, as can be seen from the figure, the graphene quantum dot prepared by this method has successfully carried out nitrogen doping (N1s peak), and...

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Abstract

The invention provides a preparation method of nitrogen-doped graphene quantum dot dispersion liquid. The preparation method comprises the following steps: placing a glucose-ammonium water mixed solution in a microwave-resisting non-sealed container, and carrying out the microwave radiation reaction; stirring the liquid obtained in the reaction at a low temperature, heating to remove excessive ammonium water, placing the liquid into a dialysis bag, centrifuging to accelerate the dialysis purification to obtain the nitrogen-doped graphene quantum dot dispersion liquid. According to the preparation method, a one-step synthetic method is adopted, the glucose is used as a carbon source, ammonium water is used as a nitrogen source and a drive agent, the microwave radiation is used as assistance, and the synthetic rate from the polymerization of glucose, nitrogen doping, carbonization to the formation of nitrogen-doped graphene quantum dots is extremely increased; the method is simple in process, easy for obtaining raw materials, rapid in reaction and environment-friendly; the prepared nitrogen-doped graphene quantum dot is good in monodispersity, high and adjustable in photoluminescent properties, excellent in solubility, good in application prospect in the fields of biological imaging, fluorescent probes and the like, and suitable for industrialized mass production after being amplified in the pilot test.

Description

technical field [0001] The invention relates to the field of nanomaterial preparation, in particular to a one-step preparation method of nitrogen-doped graphene quantum dot dispersion liquid. Background technique [0002] Graphene is a carbon atom with sp 2 The hexagonal two-dimensional material with a honeycomb lattice formed by hybridization, the special and perfect structure contains rich and peculiar physical phenomena, so that graphene exhibits many excellent mechanical, thermal, optical and electrical properties, and is used in radio frequency transistors. , sensors, flexible transparent conductive films, lithium-ion batteries, and supercapacitors have broad application prospects and have attracted great attention from the scientific community. [0003] However, for graphene with a complete lattice structure, graphene is a semiconductor with zero band gap, and its conduction band and valence band intersect at the Dirac point. In order to realize the application of gr...

Claims

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Application Information

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IPC IPC(8): C01B31/04C09K11/65
Inventor 陈远富郑斌杰李萍剑戚飞刘竞博贺加瑞张万里
Owner UNIV OF ELECTRONIC SCI & TECH OF CHINA
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