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Coal-based graphene quantum dot and preparation method thereof

A graphene quantum dot, coal-based technology, applied in the direction of graphene, chemical instruments and methods, nano-carbon, etc., can solve the problems of expensive raw materials, complicated process, high production cost, etc., to shorten the reaction time, reduce the severity, reduce the The effect of production costs

Active Publication Date: 2022-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of these methods are that the raw materials are expensive, the process is complicated, and the preparation cost is high, which limits the low-cost preparation of GQDs.
[0005] RuquanYe and others chose coal rich in energy and mineral resources in the world as raw materials, and prepared graphene quantum dots by reflux treatment at 100-120°C for 24 hours by the mixed acid oxidation method of concentrated sulfuric acid and concentrated nitric acid; Yongqiang Dong et al. Coal is used as a raw material, and graphene compounds such as graphene quantum dots are prepared through nitric acid oxidation reaction at 130°C for 24 hours. This kind of reaction at a higher temperature for a longer time causes many safety hazards in the entire preparation process.

Method used

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  • Coal-based graphene quantum dot and preparation method thereof
  • Coal-based graphene quantum dot and preparation method thereof
  • Coal-based graphene quantum dot and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Weigh bituminous coal (the average particle size is 70-80 μm, and the ash content of the bituminous coal after deashing is 0.61% by weight) and nitric acid (concentration is 68% by weight) by acid washing and deashing with a weight ratio of 1:8, followed by Put it into the sample tube, react at 25°C for 1 hour, put the sample tube into the microwave digestion instrument, react at the infrared limit temperature of 125°C for 30 minutes, and then carry out microwave digestion to remove the acid for 20 minutes to obtain the solid oxidation product. Dissolve the solid oxidation product in water, after filtration, adjust the pH value of the filtrate with ammonia solution to 7, obtain the coal-based graphene quantum dots after the obtained solution is freeze-dried, and test the particle size range of the coal-based graphene quantum dots by TEM 5-25nm, see figure 1 .

Embodiment 2

[0052] Weigh anthracite (average particle size 70-80 μm, deashed by acid washing, the ash content of anthracite after deashing is 0.91% by weight) and nitric acid with a weight ratio of 1:8, add them to the sample tube in turn, and heat at 25°C After reacting for 1 hour, put the sample tube into a microwave digestion apparatus, react at an infrared limit temperature of 125°C for 30 minutes, and then carry out microwave digestion to remove acid for 20 minutes to obtain a solid oxidation product. The solid oxidation product is dissolved in water, after filtration, the pH of the filtrate is adjusted to 7 with ammonia solution, and the obtained solution is freeze-dried to obtain coal-based graphene quantum dots. The particle size range of coal-based graphene quantum dots tested by TEM is 8-28nm, see figure 2 .

Embodiment 3

[0054] Weigh lignite (average particle size is 60-90 μm, deashed by acid washing, the ash content of lignite after deashing is 0.40% by weight) and nitric acid with a weight ratio of 1:12, add to the sample tube in turn, and react at room temperature After 2 hours, put the sample tube into a microwave digestion apparatus, react at an infrared limit temperature of 150°C for 30 minutes, and then perform microwave digestion to remove acid for 30 minutes to obtain a solid oxidation product. Dissolve the solid oxidation product in water, after filtration, adjust the pH value of the filtrate with ammonia solution to 7, obtain the coal-based graphene quantum dots after the obtained solution is freeze-dried, and test the particle size range of the coal-based graphene quantum dots by TEM 10-35nm, see image 3 .

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Abstract

The invention relates to a coal-based graphene quantum dot and a preparation method thereof.The method comprises the steps that a coal-based raw material and excessive nitric acid are mixed, the obtained mixture is subjected to a pre-oxidation reaction, and a pre-oxidation reaction mixture is obtained; carrying out microwave digestion treatment on the pre-oxidation reaction mixture to obtain an oxidation reaction product; and removing nitric acid in the oxidation reaction product, and washing and drying the obtained solid. The conditions of the method provided by the invention can reduce the severity of graphene quantum dots prepared by oxidation reaction, shorten the reaction time, and facilitate high-valued utilization of coal-based raw materials.

Description

technical field [0001] The invention relates to a coal-based graphene quantum dot and a preparation method thereof. Background technique [0002] Graphene quantum dots (GQDs), as an emerging nanomaterial, not only has the excellent properties of graphene, but also has good chemical inertness, biocompatibility, low toxicity, photoluminescence and upconversion luminescence The application in various fields such as biological imaging, disease detection, drug delivery, photoelectric devices, Raman enhancement, catalysts, sensors, etc. has gradually become a research hotspot, and has attracted extensive attention of scientists in various fields such as chemistry, physics, materials, and biology. [0003] The preparation methods of GQDs mainly include hydrothermal method, electrochemical method, mixed acid oxidation method, ultrasonic method, microwave method and electron beam etching method, etc. The disadvantages of these methods are that the raw materials are expensive, the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184
CPCC01B32/184C01B2204/32
Inventor 黄玉萍韩江华王树青高秀枝
Owner CHINA PETROLEUM & CHEM CORP
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