CN112607727B - Preparation method of high-nitrogen-content doped graphene quantum dot - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000002096 quantum dot Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- -1 amino graphene Chemical compound 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 37
- 239000000243 solution Substances 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 15
- 238000000502 dialysis Methods 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 39
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 20
- 125000000524 functional group Chemical group 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000007787 solid Substances 0.000 description 6
- 238000004020 luminiscence type Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 238000005576 amination reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
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- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- QVYARBLCAHCSFJ-UHFFFAOYSA-N butane-1,1-diamine Chemical compound CCCC(N)N QVYARBLCAHCSFJ-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses a preparation method of a high-nitrogen-content doped graphene quantum dot, and belongs to the technical field of graphene quantum dots. The method comprises the following steps: dispersing amino graphene in a strong acid solution to obtain a product A; heating the product A for reaction to obtain a product B; removing strong acid in the product B to obtain a product C; dispersing the product C in ammonia water to obtain a product D; heating and pressurizing the product D to react to obtain a product E; and purifying and drying the product E to obtain the high-nitrogen-content doped graphene quantum dot. The preparation method is simple and controllable in production process, and the prepared high-nitrogen-content doped graphene quantum dot is uniform in size, high in yield, high in nitrogen content, rich in functional groups on the surface, good in dispersibility in water and other organic solvents, and excellent in optical performance.
Description
Technical Field
The invention belongs to the technical field of graphene quantum dots, and particularly relates to a preparation method of a high-nitrogen-content doped graphene quantum dot.
Background
The graphene quantum dot is derived from physical research of graphene, has a similar carbon structure as graphene, and is another novel zero-dimensional carbon nanomaterial found after carbon nanomaterial such as zero-dimensional fullerene, one-dimensional carbon nanotube and two-dimensional graphene is reported. From the appearance, the graphene quantum dot has strong quantum confinement effect and edge effect, and the effect is more obvious when the size is smaller. The graphene quantum dots have abundant surface functional groups, so that the graphene quantum dots have excellent water-dispersing properties. Meanwhile, the graphene quantum dot has the advantages of conductivity, luminescence, innocuity, low preparation cost and the like, and is widely applied to the fields of photoelectricity, catalysis, biological medicine and the like.
At present, the preparation of graphene quantum dots mainly comprises a top-down method and a bottom-up method, wherein the top-down method takes carbon materials with larger sizes such as graphite as raw materials, the graphene quantum dots are obtained through cutting, stripping or decomposing by a physical and chemical method, and the physical and chemical degradation of the graphite is usually carried out by a hydrothermal method, a solvothermal method, a hydrazine hydrate reduction method, an electrochemical method and the like. The bottom-up method is to use small molecules as precursors and finally obtain the graphene quantum dots through a series of chemical reactions.
However, the commonly synthesized graphene quantum dots often have the defects of single surface functional group, low fluorescence quantum yield and the like, and limit the application of the graphene quantum dots in a plurality of fields. In recent years, researchers find that doping heteroatoms in the quantum dots can effectively regulate the structure and performance of graphene quantum dots. Among them, nitrogen doped graphene quantum dots are receiving a great deal of attention due to their unique photoelectric and catalytic properties. Since the nitrogen element and the carbon element are positioned in the same period of the periodic table, the atomic radius is close, so that the doping is relatively easy to realize. And the nitrogen atoms have strong electron-withdrawing induction effect, and can change the density of pi electron cloud so as to change the band gap width of the graphene quantum dot, thereby changing the property of the graphene quantum dot.
The Chinese patent 2019103475382 with publication date of 2019, 6 and 28 discloses a method for preparing nitrogen-doped graphene quantum dots by a hydrothermal method, which comprises the steps of adding butanediamine and hydrogen peroxide, and cutting graphene oxide by the hydrothermal method to obtain the nitrogen-doped graphene quantum dots, wherein the nitrogen-doped graphene quantum dots are good in dispersibility and uniform in particles. However, in the method disclosed by the patent, the graphene quantum dots are prepared by adopting a hydrothermal method, graphene oxide and reduction products thereof are adopted as raw materials, a large amount of reagents are required to be added in the reduction process, and the time consumption is long.
The Chinese patent 2017114945611 with publication date of 2018, 4 and 6 discloses a preparation method of a nitrogen-doped graphene quantum dot material, which comprises the steps of dispersing reduced graphene oxide in concentrated nitric acid, heating a magnetic stirring oil bath to 140-160 ℃, performing constant temperature reaction for 12-18 hours under condensation of circulating water, evaporating a solvent, and dialyzing to obtain the nitrogen-doped graphene quantum dot, so that the luminescence stability of the nitrogen-doped graphene quantum dot is improved to a certain extent. However, the preparation process of the nitrogen-doped graphene quantum dot obtained by the method is complex, the time consumption is long, and the nitrogen content is low.
Disclosure of Invention
Aiming at the problems of low yield, low nitrogen content, more impurities and complex preparation of graphene quantum dots in the prior art, the invention aims to provide a preparation method of graphene quantum dots doped with high nitrogen content, which comprises the steps of functionalizing graphene oxide amino groups and preparing nitrogen-doped graphene quantum dots from amino functionalized graphene.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of high-nitrogen-content doped graphene quantum dots comprises the following steps:
step 1, dispersing amino graphene in a strong acid solution to obtain a product A;
step 2, heating the product A for reaction to obtain a product B;
step 3, removing strong acid in the product B to obtain a product C;
step 4, dispersing the product C in ammonia water to obtain a product D;
step 5, heating and pressurizing the product D to react to obtain a product E;
and 6, purifying and drying the product E to obtain the high-nitrogen-content doped graphene quantum dot.
Further, the strong acid is nitric acid.
Further, the strong acid solution is a strong acid aqueous solution with the concentration of 3-8 mol/L.
Further, the amino graphene is prepared by adopting a method of China patent 2018102122660.
Further, in the step 1, the concentration of the amino graphene in the strong acid solution is 2% -5%.
Further, in the step 1, the amino graphene is dispersed in a strong acid solution in an ultrasonic mode, the ultrasonic power is 100W, and the ultrasonic time is 0.1-1 hour.
Further, in the step 2, the heating reaction condition is that the reaction is carried out for 6 to 10 hours at the temperature of 60 to 80 ℃.
Further, in step 4, the method of dispersing the product C in ammonia water is as follows: dispersing the product C in water, and then adding ammonia water to adjust the pH to 8-9.
Further, in step 5, the method for heating and pressurizing the product D to react is as follows: transferring the product D into a reaction kettle, setting the reaction temperature to be 160-220 ℃ and the reaction time to be 6-12 hours.
Further, in step 6, the method for purifying the product E comprises the following steps: and (3) carrying out suction filtration on the product E by using a microporous filter membrane, collecting filtrate, and then putting the collected filtrate into a dialysis bag for dialysis to obtain dialysis filtrate, thus finishing the purification of the product E.
Compared with the prior art, the invention has the beneficial effects that:
the high-nitrogen-content doped graphene quantum dot prepared by the method is simple and controllable in production process, and the nitrogen content is improved while the introduction of other impurity ions is avoided by selecting the amino graphene with rich nitrogen content as a carbon source, preferably nitric acid as a strong oxidant and ammonia water as a nitrogen source. The prepared high-nitrogen-content doped graphene quantum dot has uniform size, high yield, high nitrogen content, no other impurity ions, rich functional groups on the surface, good dispersibility in water and other organic solvents, and excellent optical performance, and can emit bright green fluorescence under 365nm ultraviolet irradiation.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of a high nitrogen doped graphene quantum dot according to the present invention;
FIG. 2 is an infrared spectrum of a nitrogen-doped graphene quantum dot of example 1;
fig. 3 is an atomic force picture of the nitrogen-doped graphene quantum dot of example 1;
FIG. 4 is a photograph of a nitrogen-doped graphene quantum dot of example 1 under a 365nm ultraviolet lamp;
fig. 5 is a photograph of comparative example 1 nitrogen doped graphene quantum dots under a 365nm uv lamp.
Detailed Description
The invention is further described below in connection with specific embodiments.
The aminographene used in the following examples was prepared according to example 1 of chinese patent 2018102122660.
The rest raw materials are all commercial products.
Example 1
Referring to the schematic flow chart shown in fig. 1, the preparation method of the high-nitrogen doped graphene quantum dot in this embodiment is as follows:
1. 205mL of deionized water was taken in a beaker, and then HNO with a content of 65% -68% was weighed 3 45mL of the solution is added into deionized water, stirred while being reversed, and prepared into 250mL of 4mol/L nitric acid aqueous solution;
2. dispersing 1g of amino graphene powder in the prepared solution, uniformly dispersing by ultrasonic, wherein the ultrasonic power is 100W, and the ultrasonic time is 0.5 hour;
3. transferring the solution with uniform ultrasonic dispersion into an oil bath, heating to 60 ℃, condensing and refluxing for 10 hours;
4. after the reaction is finished, taking out the reaction solution, and heating and steaming to remove the nitric acid solution in the product to obtain a tan solid;
5. the obtained tan solid is dispersed in 100mL deionized water by ultrasonic, the ultrasonic power is 100W, the ultrasonic time is 0.5 hour, and then ammonia water (25% -28%) is added to adjust the pH to 8.03;
6. transferring the solution with the pH value regulated to a reaction kettle, and reacting for 12 hours at 160 ℃;
7. cooling to room temperature after the reaction is finished, carrying out suction filtration by using a microporous filter membrane with the diameter of 0.22 mu m, and collecting filtrate;
8. dialyzing the collected filtrate in a dialysis bag with molecular weight cut-off of 3500 and dialysis times of 5 times for 2 hours each time;
9. and (3) carrying out vacuum drying on the obtained filtrate, and obtaining a dried powdery sample which is the high-nitrogen-content doped graphene quantum dot.
The obtained nitrogen content doped graphene quantum dot can emit bright green fluorescence under 365nm ultraviolet irradiation.
Example 2
Referring to fig. 1, the preparation method of the high nitrogen doped graphene quantum dot of the present embodiment is as follows:
1. 185mL of deionized water is taken in a beaker, and HNO with the content of 65 to 68 percent is then weighed 3 65mL of the aqueous solution is added into deionized water, stirred while being reversed, and prepared into 250mL of 6mol/L nitric acid aqueous solution;
2. dispersing 1g of amino graphene powder in the prepared solution, uniformly dispersing by ultrasonic, wherein the ultrasonic power is 100W, and the ultrasonic time is 0.5 hour;
3. transferring the solution with uniform ultrasonic dispersion into an oil bath, heating to 70 ℃, condensing and refluxing for 8 hours;
4. after the reaction is finished, taking out the reaction solution, heating and steaming to remove the nitric acid solution in the product to obtain a tan solid;
5. the obtained tan solid is dispersed in 100mL deionized water by ultrasonic, the ultrasonic power is 100W, the ultrasonic time is 0.5 hour, and ammonia water (25% -28%) is added to adjust the pH to 8.56;
6. transferring the solution with the pH value regulated to a reaction kettle, and reacting for 10 hours at 180 ℃;
7. cooling to room temperature after the reaction is finished, carrying out suction filtration by using a microporous filter membrane with the diameter of 0.22 mu m, and collecting filtrate;
8. dialyzing the collected filtrate in a dialysis bag with molecular weight cut-off of 3500 and dialysis times of 5 times for 2 hours each time;
9. and (3) carrying out vacuum drying on filtrate obtained by dialysis, wherein a dried powdery sample is the high-nitrogen-content doped graphene quantum dot.
The obtained nitrogen content doped graphene quantum dot can emit bright green fluorescence under 365nm ultraviolet irradiation.
Example 3
1. 160mL of deionized water is taken in a beaker, and then HNO with the content of 65 to 68 percent is weighed 3 90mL of the aqueous solution is added into deionized water, stirred while being reversed, and prepared into 250mL of 8mol/L nitric acid aqueous solution;
2. dispersing 1g of amino graphene powder in the prepared solution, uniformly dispersing by ultrasonic, wherein the ultrasonic power is 100W, and the ultrasonic time is 0.5 hour;
3. transferring the solution with uniform ultrasonic dispersion into an oil bath, heating to 80 ℃, condensing and refluxing for 6 hours;
4. after the reaction is finished, taking out the reaction solution, heating and steaming to remove the nitric acid solution in the product to obtain a tan solid;
5. the obtained tan solid is dispersed in 100mL deionized water by ultrasonic, the ultrasonic power is 100W, the ultrasonic time is 0.5 hour, and ammonia water (25% -28%) is added to adjust the pH to 8.93;
6. transferring the solution with the pH value regulated to a reaction kettle, and reacting for 8 hours at the temperature of 200 ℃;
7. cooling to room temperature after the reaction is finished, carrying out suction filtration by using a microporous filter membrane with the diameter of 0.22 mu m, and collecting filtrate;
8. dialyzing the collected filtrate in a dialysis bag with molecular weight cut-off of 3500 and dialysis times of 5 times for 2 hours each time;
9. and (3) carrying out vacuum drying on the filtrate obtained by dialysis, wherein a dried powdery sample is the high-nitrogen-content doped graphene quantum dot.
The obtained nitrogen content doped graphene quantum dot can emit bright green fluorescence under 365nm ultraviolet irradiation.
Comparative example 1
The preparation method of the nitrogen-doped graphene quantum dot of the comparative example is basically the same as that of example 1, except that the comparative example 1 directly uses graphene oxide as a raw material for reaction, and does not undergo amination reaction.
Comparative example 2
This comparative example is substantially the same as example 1, except that graphene is directly reacted as a raw material, and no amination reaction is performed.
Fig. 2 is an infrared spectrum of a nitrogen-doped graphene quantum dot of example 1. As can be seen from the figure, 3342.9cm -1 Is NH stretching vibration peak 1486.77cm -1 For OH bending vibration peak, 1352.79cm -1 Is C-N telescopic vibration peak of 1003.35cm -1 Is C-C telescopic vibration peak of 695.20cm -1 Is NH 2 The out-of-plane rocking peak proves that the surface of the material is rich in functional groups and has good dispersibility in water and other organic solvents.
Fig. 3 is an atomic force picture of the nitrogen-doped graphene quantum dot of example 1, and as can be seen from fig. 3, the prepared nitrogen-doped graphene quantum dot has uniform distribution and small particle size, and is beneficial to fluorescence luminescence stability.
Fig. 4 is a photograph of the nitrogen-doped graphene quantum dot of example 1 under a 365nm ultraviolet lamp.
Fig. 5 is a photograph of the nitrogen-doped graphene quantum dot of comparative example 1 under a 365nm ultraviolet lamp.
As can be seen from comparison between fig. 4 and fig. 5, the fluorescence luminescence intensity of the nitrogen doped graphene quantum dot prepared by the method is higher than that of the graphene quantum dot prepared by graphene without amination reaction under a 365nm ultraviolet lamp.
The nitrogen content of the nitrogen-doped graphene quantum dots obtained in each of the examples and comparative examples was tested, and the results are shown in table 1.
As can be seen from Table 1, the nitrogen content of the nitrogen-doped graphene quantum dots prepared by the method is obviously improved compared with the graphene quantum dots prepared by directly using graphite oxide and graphene, and the nitrogen-doped graphene quantum dots are favorable for fluorescence luminescence stability.
Table 1N content test for different examples and comparative examples
Sample of | N content (%) |
Example 1 | 6.86 |
Example 2 | 6.55 |
Example 3 | 6.32 |
Comparative example 1 | 3.21 |
Comparative example 2 | 2.32 |
Claims (6)
1. The preparation method of the high-nitrogen-content doped graphene quantum dot is characterized by comprising the following steps of:
step 1, dispersing amino graphene in a strong acid solution to obtain a product A;
step 2, heating and reacting the product A at 60-80 ℃ for 6-10 hours to obtain a product B;
step 3, removing strong acid in the product B to obtain a product C;
step 4, dispersing the product C in ammonia water to obtain a product D;
step 5, transferring the product D into a reaction kettle, setting the reaction temperature to 160-220 ℃ and the reaction time to 6-12 hours to obtain a product E;
step 6, purifying and drying the product E to obtain the high-nitrogen-content doped graphene quantum dot;
the strong acid is nitric acid.
2. The preparation method of the high-nitrogen-content doped graphene quantum dot according to claim 1, wherein the strong acid solution is a strong acid aqueous solution with the concentration of 3-8 mol/L.
3. The method for preparing the high-nitrogen-content doped graphene quantum dots according to claim 1, wherein in the step 1, the concentration of the amino graphene in a strong acid solution is 2% -5%.
4. The preparation method of the high-nitrogen-content doped graphene quantum dot is characterized in that in the step 1, the amino graphene is dispersed in a strong acid solution in an ultrasonic mode, the ultrasonic power is 100W, and the ultrasonic time is 0.1-1 hour.
5. The method for preparing the high-nitrogen-content doped graphene quantum dot according to claim 1, wherein in the step 4, the method for dispersing the product C in ammonia water is as follows: dispersing the product C in water, and then adding ammonia water to adjust the pH to 8-9.
6. The method for preparing the high-nitrogen-content doped graphene quantum dot according to claim 1, wherein in the step 6, the method for purifying the product E is as follows: and (3) carrying out suction filtration on the product E by using a microporous filter membrane, collecting filtrate, and then putting the collected filtrate into a dialysis bag for dialysis to obtain dialysis filtrate, thus finishing the purification of the product E.
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