A preparation method of graphene quantum dots with controllable oxidation degree

A technology of graphene quantum dots and oxidation degree, applied in chemical instruments and methods, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problem of low yield, unfavorable large-scale preparation of graphene quantum dots, and impurity removal Low efficiency and other problems, to achieve the effect of large processing capacity, high yield, and simple preparation process

Active Publication Date: 2017-02-22
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, dialysis generally takes many times and a long time to meet the impurity removal requirements, and the impurity removal efficiency is low, which is not conducive to the large-scale preparation of graphene quantum dots
Chinese patent application number 201310740378.0 discloses the extraction of graphene quantum dots from graphene oxide aqueous solution to obtain high-purity graphene oxide powder, but the yield is low

Method used

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  • A preparation method of graphene quantum dots with controllable oxidation degree
  • A preparation method of graphene quantum dots with controllable oxidation degree
  • A preparation method of graphene quantum dots with controllable oxidation degree

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add ultra-fine graphite powder into 200 ml of distilled water, stir evenly, and then filter with ultrasonic treatment for 10 minutes, collect the graphite powder on the filter paper; disperse the above graphite powder in 200 ml of ethanol, stir well, and then ultrasonically treat for 10 minutes Suction filtration, collect the graphite powder on the filter paper, and dry at 50°C to obtain graphite powder with uniform particle size.

[0028] Take 1 gram of cleaned graphite powder and add it to 70 ml of a mixed solution of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 5:1, stir mechanically, and control the temperature at about 110 °C. After reacting for 24 hours, the heating was stopped, and after cooling to room temperature, 430 ml of distilled water was added while stirring to dilute the reactant. Sodium hydroxide was added while stirring until the reaction was neutral.

[0029] The solution was added to a 2 liter XDA-1 macroporous resi...

Embodiment 2

[0032] Take 1 gram of cleaned graphite powder and add it to 80 ml of a mixed solution of concentrated sulfuric acid and concentrated hydrochloric acid with a volume ratio of 5:1, stir mechanically, and control the temperature at about 130 °C. After reacting for 26 hours, the heating was stopped, and after cooling to room temperature, 420 ml of distilled water was added while stirring to dilute the reactant. Sodium hydroxide was added while stirring until the reaction was neutral.

[0033] The solution solution was added to a 2 liter XDA-1 macroporous resin column and adsorbed for 4 hours. After elution with distilled water until no chloride ions are detected by silver nitrate and no sulfate ions are detected by barium chloride, the eluate is collected. Elution was performed sequentially with 1000 ml of distilled water, 1200 ml of 50% ethanol and 1800 ml of 95% ethanol.

[0034] After drying the solutions eluted with distilled water, 50% ethanol and 95% ethanol, respectively,...

Embodiment 3

[0036] Take 1 gram of cleaned graphite powder and add it to 70 ml of a mixed solution of concentrated hydrochloric acid and concentrated nitric acid with a volume ratio of 6:1, stir mechanically, and control the temperature at about 150 °C. After reacting for 28 hours, the heating was stopped, and after cooling to room temperature, 430 ml of distilled water was added while stirring to dilute the reactant. Sodium hydroxide was added while stirring until the reaction was neutral.

[0037] The solution was added to a 2 liter XDA-1 macroporous resin column and adsorbed for 6 hours. After elution with distilled water until no chloride ions can be detected by silver nitrate, start to collect the eluate. Elution was carried out successively with 1000 ml of distilled water and 1500 ml of 95% ethanol.

[0038] After drying the solutions eluted with distilled water and 95% ethanol, respectively, 0.1561 g and 0.2517 g of graphene quantum dots were obtained, with a yield of 40.78%.

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Abstract

The invention relates to a method for preparing graphene quantum dots with controllable oxidation degrees. According to the method provided by the invention, graphene quantum dots with controllable particle sizes are prepared from ultrafine graphite powder which serves as a raw material, by a strong-acid oxidation method and are purified through macroporous resin, so that graphene quantum dots which are free of inorganic salt impurities and have different degrees of oxidation can be obtained. The method is simple in process, low in cost and relatively high in yield and is applicable to industrial large-scale production.

Description

technical field [0001] The invention relates to a preparation method of graphene quantum dots with controllable oxidation degree, belonging to the technical field of preparation of graphene quantum dots. Background technique [0002] Graphene quantum dots are an emerging zero-dimensional carbon material. Compared with conventional large-size two-dimensional graphene, graphene quantum dots have significant edge effects and quantum confinement effects, thus exhibiting excellent optical and electrical properties. At the same time, compared with traditional carbon quantum dots and rare earth metal oxide quantum dots, graphene quantum dots also have good water solubility, stable and adjustable fluorescence, low cytotoxicity and excellent biocompatibility. The performance advantages make graphene quantum dots have very broad application prospects in many fields such as optoelectronic materials and devices, electrocatalysis, electrochemical biosensing, and bioimaging. [0003] Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C09K11/65B82Y30/00
Inventor 赵亮董树清毕青孙亚明王利涛张霞张晓莉
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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