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Large-scale preparation method for graphene quantum dots

A large-scale preparation technology of graphene quantum dots, applied in the direction of graphene, chemical instruments and methods, luminescent materials, etc., can solve the problems of complex steps, complex processes, low yield, etc., achieve large reaction volume, simple process, cost reduction effect

Active Publication Date: 2014-05-14
湖北高地石墨烯科技有限公司
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Problems solved by technology

Among them, the secondary oxidation method needs to prepare high-quality graphene materials before the subsequent oxidation steps can be carried out, which is costly and not conducive to industrialization; the process involved in the organic synthesis method is complicated and cumbersome, which is not conducive to industrial production; The method of electron or ion beam etching has the problem of low yield and cannot be mass-produced; the method of microscopically cutting carbon materials also has the defects of complicated steps and low yield

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  • Large-scale preparation method for graphene quantum dots
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[0033] see figure 1 , a method for large-scale preparation of graphene quantum dots in an embodiment, comprising the following steps S110 to S140.

[0034] Step S110: adding graphene oxide into the first solvent, uniformly dispersing to obtain a first dispersion liquid, adding a reducing agent to the first dispersion liquid, and uniformly dispersing to obtain a mixed liquid.

[0035] Graphene oxide is preferably monolayer graphene oxide prepared by a modified Hummers' chemical method.

[0036] The first solvent is at least one selected from water, dimethoxyethane, polyvinyl alcohol aqueous solution, glycerol, diethylene glycol and N-methylpyrrolidone. The boiling points of these solvents are relatively high, and the high-boiling-point solvents can provide a sufficiently high ambient temperature for the deoxygenation and reduction of graphene oxide, and the above-mentioned high-boiling-point solvents have no adverse reaction with graphene oxide.

[0037] Preferably, the first...

Embodiment 1

[0079] Preparation of graphene quantum dots

[0080] 1. Provide single-layer graphene oxide prepared by improving Hummers' chemical method, disperse single-layer graphene oxide in dimethoxyethane, and uniformly disperse to obtain the first monolayer graphene oxide concentration of 2mg / mL Dispersion liquid, adding oxalic acid to the first dispersion liquid, uniformly dispersed to obtain a mixed liquid; wherein, the mass ratio of single-layer graphene oxide to oxalic acid is 1:3;

[0081]2. The mixture was ultrasonically dispersed in a 120W ultrasonic environment for 4 hours, then placed in a closed reaction container, and reacted in a 500W microwave environment for 30 minutes; take out and add dimethoxyethane, and the added dimethoxy The volume of ethane is 15% of the volume of the initial dimethoxyethane in the first dispersion liquid; continue to react in the microwave environment of 500W for 10min, after the reaction finishes, wait for the reaction liquid to cool down, add t...

Embodiment 2

[0086] Preparation of graphene quantum dots

[0087] 1. Provide single-layer graphene oxide prepared by improving Hummers’ chemical method, disperse single-layer graphene oxide in a mixed solvent of triethylene glycol and N-methylpyrrolidone with a volume ratio of 1:1, and disperse evenly Obtaining the concentration of monolayer graphene oxide is the first dispersion liquid of 6mg / mL, sodium oxalate is added in the first dispersion liquid, evenly dispersed to obtain mixed solution; Wherein, the mass ratio of monolayer graphene oxide and sodium oxalate is 1: 8;

[0088] 2. Ultrasonically disperse the mixed solution for 1 hour in a 150W ultrasonic environment, put it into a closed reaction container, and react in a 700W microwave environment for 20 minutes; take out and add diethylene glycol and N at a volume ratio of 1:1 -The mixed solvent of methylpyrrolidone, the volume ratio of the mixed solvent of diethylene glycol and N-methylpyrrolidone added is that the volume ratio of ...

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Abstract

The invention provides a large-scale preparation method for graphene quantum dots. The large-scale preparation method comprises the following steps: adding graphene oxide into a first solvent to obtain a first solvent to obtain a first dispersion solution; adding a reducing agent into the first dispersion solution to obtain a mixed solution; reacting the mixed solution in a microwave environment of 500-800W for 10-60 minutes; cooling and carrying out solid-liquid separation and taking solids to obtain a rough product; mixing one of reductive polyhydroxy aldehyde and an organic acid with the rough product; adding Lewis acid and uniformly mixing to obtain a mixture; adding the mixture into a second solvent to obtain a second dispersion solution; reacting the second dispersion solution in the microwave environment of 500-800W for 0.2-1 hour; then stripping in the microwave environment of 120-300W for 2-3 hours; separating and purifying to obtain the graphene quantum dots. The large-scale preparation is finished by a microwave-solvothermal method; the process is simple and the utilization rate of the graphene oxide is high; the yield is high.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a large-scale preparation method of graphene quantum dots. Background technique [0002] Since Andre Geim and Konstantin Novoselof of the University of Manchester successfully stripped pyrolytic graphite and observed graphene for the first time in 2004, the enthusiasm for research on new carbon materials in the academic community has not subsided. The successful separation of graphene means that the theoretical prediction of the thermodynamic instability of two-dimensional crystals has been broken, and it has brought the possibility of many new fields of research. [0003] Perfect graphene has an ideal two-dimensional structure, which is composed of a hexagonal lattice. Each carbon atom is combined with three other carbon atoms in the direction of the lattice plane through a σ bond, and the electrons that do not form a σ bond act as π Electrons form a π orbital ...

Claims

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Application Information

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IPC IPC(8): C01B31/04C09K11/65C01B32/184
Inventor 张明东张麟德
Owner 湖北高地石墨烯科技有限公司
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