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Mass preparation method and device of graphene quantum dots

A graphene quantum dot, large-scale preparation technology, applied in graphene, nano-carbon and other directions, can solve the problems of low yield and low purity of graphene quantum dots

Inactive Publication Date: 2016-01-13
NANJING UNIV
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  • Description
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Problems solved by technology

However, the yield of graphene quantum dots prepared by these methods is usually very low, and because a large amount of strong alkali is used to neutralize the remaining strong acid solution in the preparation process, the obtained samples usually contain a relatively high content of salt, that is, Its purity is low

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  • Mass preparation method and device of graphene quantum dots
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  • Mass preparation method and device of graphene quantum dots

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Embodiment Construction

[0030] The following are examples of the present invention, and the reagents used in the examples are chemically pure.

[0031] Design a condensing tube with a switch and an oval drop recovery device by yourself, use XC-72 carbon black as the raw material, and use concentrated nitric acid as the oxidant; put 1.6g of carbon black and 300ml of concentrated nitric acid in a triangular round bottom flask , and put in a magnetic stirrer at the same time; install the water droplet recovery device on the middle neck of the Erlenmeyer flask, then install the condenser tube on the water droplet recovery device, and use the iron stand and clips to fix the condenser tube and the triangular round bottom flask at the same time; Put the mixed solution of ethylene glycol and water cooled by the low-temperature constant temperature bath device into the tube; place the triangular round bottom flask in the oil bath, raise the temperature of the oil bath to 135°C, under magnetic stirring, at 135°...

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Abstract

The invention relates to a mass preparation method and a mass preparation device of graphene quantum dots. According to the invention, conductive carbon black is adopted as a raw material and concentrated nitric acid is adopted as an oxidant; conductive carbon black and concentrated nitric acid are placed in a flask, and a magnetic stirrer is also placed in the flask; the flask is provided with a reflux device, and one section of the pipe in the reflux device is a condenser pipe; the flask is placed in an oil bath pot, and the oil bath pot is heated to a temperature of 135+ / -2 DEG C; under the stirring of the magnetic stirrer, a reflux reaction is carried out for 24+ / -6h under a temperature of 135 DEG C; a low-temperature thermostat bath device is turned off, and the oil bath pot is heated to a temperature of 180+ / -2 DEG C; argon is delivered to the bottom of the flask, and concentrated nitric acid evaporation is carried out for 10+ / -2h under the temperature of 180+ / -2 DEG C; an obtained solid sample is dissolved in deionized water, and the mixture is centrifuged with a high-speed centrifuge; an upper-layer suspension liquid is fetched after centrifugation, and is respectively filtered with a 220nm filter membrane and a 25nm filter membrane; unoxidized carbon black or large particles are removed; a graphene quantum dot solution obtained after suction filtration is collected, and is subjected to rotary evaporation under a temperature of 40-80 DEG C with a rotary evaporator; and an obtained concentrated graphene quantum dot solution is subjected to freezing and drying with a vacuum freeze-drying machine.

Description

technical field [0001] The invention relates to a method and device for large-scale preparation of graphene quantum dots, especially the oxidation of carbon black and the removal of nitric acid can be realized under in-situ conditions, and graphite can be realized in an environmentally friendly way under a closed experimental device. Large-scale preparation of ene quantum dots. Background technique [0002] Due to its large specific surface area, low toxicity, good water solubility, significant quantum effects and boundary effects, graphene quantum dots have attracted widespread attention and research in the fields of nanoscience and nanotechnology. And it has been widely used in supercapacitors, solar cells, biological calibration and imaging, ultrasensitive sensors and detectors, fluorescent probes, etc. The preparation methods of graphene quantum dots reported so far generally include: microwave-assisted method, hydrothermal method, electrochemical and other methods. Ho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 刘富池孙媛媛汤怒江钟伟都有为
Owner NANJING UNIV
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