CN107601467B - Preparation method of oil-soluble graphene quantum dots - Google Patents
Preparation method of oil-soluble graphene quantum dots Download PDFInfo
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- CN107601467B CN107601467B CN201710946525.8A CN201710946525A CN107601467B CN 107601467 B CN107601467 B CN 107601467B CN 201710946525 A CN201710946525 A CN 201710946525A CN 107601467 B CN107601467 B CN 107601467B
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Abstract
The invention provides a preparation method of oil-soluble graphene quantum dots, and belongs to the technical field of nano material preparation. The method comprises the following steps: (1) placing citric acid in a container, heating and melting at the temperature of 180-250 ℃ until the citric acid becomes orange; (2) adding a proper amount of oleylamine into orange citric acid pyrolysis liquid, and reacting at the temperature of 180 ℃ and 250 ℃ for 3-8 min; (3) stopping heating, dropwise adding the reactants into toluene, and violently shaking until the reactants are completely mixed; (4) adding water into the uniformly mixed toluene solution, slowly shaking up, and standing until the solution is layered; (5) and (3) taking the upper toluene layer, and freeze-drying to obtain solid powder, namely the oil-soluble graphene quantum dots. The oil-soluble graphene quantum dots prepared by the method are high in purity; the method has the advantages of common and easily obtained reagents, simple method and easy large-scale preparation.
Description
Technical Field
The invention relates to preparation of a nano material, and particularly belongs to a preparation method of oil-soluble graphene quantum dots.
Background
Graphene quantum dots are graphene flakes less than 10nm in size. The graphene quantum dots have many excellent properties, such as large surface area, high mechanical properties, high electron mobility and high biocompatibility, so that the graphene quantum dots have important application prospects in the fields of biomedicine, electronic materials, optical materials, magnetic materials, environmental detection and the like.
The preparation methods of the graphene quantum dots are mainly divided into two types, namely a top-down method and a bottom-up method. The top-down method is to perform chemical or physical treatment on a graphene sheet to obtain graphene quantum dots, and specifically comprises an electrochemical method, a hydrothermal method, a chemical carbon fiber stripping method and the like; the bottom-up method is to obtain the graphene quantum dots by taking small molecules as reaction precursors and carrying out a series of chemical reaction steps, and specifically comprises a chemical vapor deposition method, a pyrolysis method, a microwave method and the like.
At present, the oil-soluble graphene quantum dots are generally synthesized firstly, and then are subjected to functional modification. But the steps of the implementation process are complicated and difficult to popularize. CN201710381811 discloses a melt preparation method of nitrogen-doped graphene quantum dots, which can obtain the nitrogen-doped graphene quantum dots under a melt condition. However, the graphene quantum dots prepared by the method are water-soluble and not oil-soluble. And the purity of the quantum dots prepared by the method is difficult to ensure.
Disclosure of Invention
The invention aims to provide a simple and effective preparation method of oil-soluble graphene quantum dots.
The invention provides a preparation method of oil-soluble graphene quantum dots, which comprises the following steps:
(1) placing citric acid in a container, heating and melting at the temperature of 180-250 ℃ until the citric acid becomes orange;
(2) adding a proper amount of oleylamine into orange citric acid pyrolysis liquid, and reacting at the temperature of 180 ℃ and 250 ℃ for 3-8 min;
(3) stopping heating, dropwise adding the reactants into toluene, and violently shaking until the reactants are completely mixed;
(4) adding water into the uniformly mixed toluene solution, slowly shaking up, and standing until the solution is layered;
(5) and (3) taking the upper toluene layer, and freeze-drying to obtain solid powder, namely the oil-soluble graphene quantum dots.
The citric acid in the step (1) is analytically pure citric acid with the purity of 99.5 percent; the oleylamine in the step (2) is analytically pure oleylamine; the toluene in the step (3) is analytically pure toluene; the water in the step (4) is deionized water.
Compared with the prior art, the invention has the following beneficial effects:
1. the oil-soluble graphene quantum dots prepared by the method can remove toluene and unreacted oleylamine thereof after freeze drying, so that the purity is high.
2. The method has the advantages of common and easily obtained reagents, simple method and easy large-scale preparation.
Drawings
FIG. 1 is a projection electron microscope image of oil-soluble graphene quantum dots prepared by the method.
Figure 2 shows the ultraviolet-visible spectrum of the toluene solution of oil-soluble graphene quantum dots prepared in the present invention.
FIG. 3 shows the fluorescence emission spectrum (excitation wavelength is 420 nm) of the toluene solution of the oil-soluble graphene quantum dots prepared by the present invention.
The specific implementation mode is as follows:
example 1
(1) Weighing 4g of citric acid, placing in a 25ml beaker, heating at 200 deg.C until the citric acid is melted and the pyrolysis solution turns orange (55 min);
(2) adding 0.5ml oleylamine into orange citric acid pyrolysis liquid, and reacting for 6min at 200 ℃;
(3) stopping heating, adding the citric acid and oleylamine reactant into 100ml of methylbenzene, and violently shaking until the reactants are completely mixed;
(4) adding 100ml of water into the solution, shaking up, and standing until the solution is clearly layered;
(5) and taking the upper toluene layer, and freeze-drying the toluene layer for 36 hours to obtain 0.08g of solid powder, namely the oil-soluble graphene quantum dots.
Example 2
(1) Weighing 4g of citric acid, placing in a 25ml beaker, heating at 220 deg.C until the citric acid is melted and the pyrolysis solution turns orange (43 min);
(2) adding 1ml oleylamine into orange citric acid pyrolysis liquid, and reacting for 8min at 220 ℃;
(3) stopping heating, adding the citric acid and oleylamine reactant into 100ml of methylbenzene, and violently shaking until the reactants are completely mixed;
(4) adding 100ml of water into the solution, shaking up, and standing until the solution is clearly layered;
(5) and taking the upper toluene layer, and freeze-drying the toluene layer for 36 hours to obtain 0.11g of solid powder, namely the oil-soluble graphene quantum dot.
Claims (2)
1. A preparation method of oil-soluble graphene quantum dots is characterized by comprising the following steps:
(1) placing citric acid in a container, heating and melting at the temperature of 180-250 ℃ until the citric acid becomes orange;
(2) adding a proper amount of oleylamine into orange citric acid pyrolysis liquid, and reacting at the temperature of 180 ℃ and 250 ℃ for 3-8 min;
(3) stopping heating, dropwise adding the reactants into toluene, and violently shaking until the reactants are completely mixed;
(4) adding water into the uniformly mixed toluene solution, slowly shaking up, and standing until the solution is layered;
(5) and (3) taking the upper toluene layer, and freeze-drying to obtain solid powder, namely the oil-soluble graphene quantum dots.
2. The method for preparing the oil-soluble graphene quantum dot according to claim 1, wherein the water in the step (4) is deionized water.
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| CN107601467B true CN107601467B (en) | 2020-04-17 |
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| CN115433573B (en) * | 2022-09-28 | 2023-06-20 | 山西大学 | Preparation method of oil-soluble carbon dots for detecting doxycycline hydrochloride |
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