CN114806551A - Graphene fluorescent nano material and preparation method and application thereof - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 96
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 230000004913 activation Effects 0.000 claims abstract description 9
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N ethyl acetate Substances CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- 238000012984 biological imaging Methods 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000012216 imaging agent Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- 239000007850 fluorescent dye Substances 0.000 abstract description 2
- 238000001215 fluorescent labelling Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class 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
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 229910021387 carbon allotrope Inorganic materials 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0013—Luminescence
- A61K49/0017—Fluorescence in vivo
- A61K49/0019—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01B32/194—After-treatment
- C01B32/196—Purification
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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Abstract
The invention discloses a graphene fluorescent nano material, which is prepared by dispersing graphene in a dispersion liquid, and then adding N-hydroxysuccinimide and N, N-dimethyldodecylamine into a solvent for activation; adding activated graphene into a trivalent ferric salt, ethylene glycol, nitric acid and sulfuric acid, performing ultrasonic dispersion, performing high-temperature reaction, washing with water and ethanol, filtering and separating a graphene material, and drying to obtain the graphene fluorescent nano material. After the graphene is subjected to dispersion activation, the graphene material obtained by the subsequent reaction has good dispersibility and good length uniformity; through repeated reaction for many times, the prepared graphene fluorescent nano material has high purity, good fluorescent labeling effect and good biological compatibility; the graphene fluorescent nano material has low overall reaction conditions, relatively simple preparation process and low manufacturing cost.
Description
Technical Field
The invention relates to the technical field of graphene materials, in particular to a graphene fluorescent nano material and a preparation method thereof.
Background
The carbon material is a common and special material on the earth, and with the development of nanotechnology, the carbon nanomaterial has become the leading field of technological innovation in recent 20 years. Due to the special performance of the material expressed on the nanometer size, a new way is provided for the research of the behaviors and the interaction mechanism of cells, subcells and single molecule atoms. However, due to the characteristics of low water solubility and low activity of the carbon nanomaterial, the application of the carbon nanomaterial in a plurality of research fields such as analytical chemistry, material science and biotechnology is limited.
Graphene is the basic building block for some carbon allotropes, including graphite, carbon nanotubes, and fullerenes. The functionalization of graphene and the application of graphene in chemical modification electrodes, chemical power sources, catalysts, gas sensors and the like are researched more. However, the low water solubility and poor biocompatibility of ordinary graphene limit its biological and medical applications.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, an object of the present invention is to provide a graphene fluorescent nanomaterial and a preparation method thereof, which solve the problems of low water solubility and poor biocompatibility of graphene.
According to the graphene fluorescent nano material provided by the invention, graphene is dispersed in dispersion liquid, and then N-hydroxysuccinimide and N, N-dimethyldodecylamine are added into a solvent for activation; adding activated graphene into a trivalent ferric salt, ethylene glycol, nitric acid and sulfuric acid, performing ultrasonic dispersion, performing high-temperature reaction, washing with water and ethanol, filtering and separating a graphene material, and drying to obtain the graphene fluorescent nano material.
In some embodiments of the invention, the graphene is graphene oxide or graphene fluoride.
In other embodiments of the present invention, the dispersion is one of a silicon nitride-ethyl acetate solution or a boron nitride solution.
In other embodiments of the present invention, the graphene fluorescent nanomaterial may be reacted through the above steps for a plurality of times to improve the purity of the graphene fluorescent nanomaterial.
In other embodiments of the present invention, the graphene fluorescent nanomaterial has a size of 10-15 nm.
In other embodiments of the present invention, the mass ratio of the graphene, the ferric salt, the glycol, the nitric acid and the sulfuric acid is 1: 0.5-1.5:2-2.5: 1.2-1.5: 1.0-1.2.
A preparation method of a graphene fluorescent nano material comprises the following specific steps:
s1: dissolving a dispersing agent in deionized water by ultrasonic oscillation to prepare a dispersion liquid, wherein the molar concentration of the dispersion liquid is 1.0-2.5 moL/L;
s2: slowly adding graphene into the dispersion liquid, and ultrasonically vibrating, wherein the vibration dissolution frequency is 1.0-2.5KHz, and the vibration time is 10-15 min;
s3: n-hydroxysuccinimide and N, N-dimethyldodecylamine are added in a ratio of 1: preparing 1.5-2.5mol/l solution according to the molar concentration ratio, adding the vibrated and dispersed graphene into the solution for activation for 1-3 h;
s4: the activated graphene, a ferric iron salt, ethylene glycol, nitric acid and sulfuric acid are mixed according to a mass ratio of 1: 0.5-1.5:2-2.5: 1.2-1.5: 1.0-1.2, performing ultrasonic dispersion reaction, firstly performing ultrasonic dispersion for 10-20min, then performing reaction for 5-10h in a reaction kettle at the temperature of 180-220 ℃, cooling to room temperature after complete reaction, repeatedly washing reacted graphene with water and absolute ethyl alcohol, then drying the separated graphene material, and finally obtaining the primary graphene fluorescent nanomaterial;
s5: and (5) repeating the steps S2-S4 by using the initial graphene fluorescent nano material obtained in the step S4 to perform 3-5 operations, so as to obtain the graphene fluorescent nano material.
In other embodiments of the present invention, the reaction kettle of step S4 is reacted under nitrogen protection.
The graphene fluorescent nano material can be applied to biological imaging agents, tracing agents and the field of medicines.
According to the invention, graphene is subjected to dispersion activation, and then the graphene material obtained by the subsequent reaction has good dispersibility and good length uniformity.
The graphene fluorescent nano material prepared by repeated reaction (3-5 times) has high purity, good fluorescent labeling effect and good biological compatibility.
The graphene fluorescent nano material has low overall reaction conditions, relatively simple preparation process and low manufacturing cost.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
The invention provides a preparation method of a graphene fluorescent nano material, which comprises the following specific steps:
s1: dissolving a dispersing agent (silicon nitride-ethyl acetate) in deionized water by ultrasonic oscillation to prepare a dispersion liquid, wherein the molar concentration of the dispersion liquid is 1.0 moL/L;
s2: slowly adding graphene into the dispersion liquid, and ultrasonically vibrating, wherein the vibration dissolution frequency is 1.0KHz, and the vibration time is 10 min;
s3: n-hydroxysuccinimide and N, N-dimethyldodecylamine are added in a ratio of 1: preparing 1.5mol/l solution according to a molar concentration ratio, adding the graphene subjected to vibration dispersion into the solution for activation, and activating for 3 hours;
s4: the activated graphene, a ferric iron salt, ethylene glycol, nitric acid and sulfuric acid are mixed according to a mass ratio of 1: 0.5:2: 1.2: 1.0, performing ultrasonic dispersion reaction, namely performing ultrasonic dispersion for 10min, reacting for 5h in a reaction kettle at 180 ℃ under the protection of nitrogen, cooling to room temperature after complete reaction, repeatedly washing reacted graphene with water and absolute ethyl alcohol, drying the separated graphene material, and finally obtaining the primary graphene fluorescent nano material;
s5: and (5) repeating the steps S2-S4 by using the initial graphene fluorescent nano-material obtained in the step S4 to perform 3 operations, so as to obtain the graphene fluorescent nano-material.
Example 2
The invention provides a preparation method of a graphene fluorescent nano material, which comprises the following specific steps:
s1: dissolving a dispersing agent (boron nitride) in deionized water by ultrasonic oscillation to prepare a dispersion liquid, wherein the molar concentration of the dispersion liquid is 2.0 moL/L;
s2: slowly adding graphene into the dispersion liquid, and ultrasonically vibrating, wherein the vibration dissolution frequency is 1.8KHz, and the vibration time is 12 min;
s3: n-hydroxysuccinimide and N, N-dimethyldodecylamine are added in a ratio of 1: preparing a solution with the molar concentration ratio of 1 into 2.0mol/l, adding the graphene subjected to vibration dispersion into the solution for activation for 2 hours;
s4: the activated graphene, a ferric iron salt, ethylene glycol, nitric acid and sulfuric acid are mixed according to a mass ratio of 1: 1.0:2.2: 1.4: 1.1, performing ultrasonic dispersion reaction, namely performing ultrasonic dispersion for 15min, reacting for 8h in a reaction kettle at the temperature of 200 ℃ under the protection of nitrogen, cooling to room temperature after complete reaction, repeatedly washing reacted graphene with water and absolute ethyl alcohol, drying the separated graphene material, and finally obtaining a primary graphene fluorescent nano material;
s5: and (5) repeating the steps S2-S4 by using the initial graphene fluorescent nano-material obtained in the step S4 to perform 4 operations, so as to obtain the graphene fluorescent nano-material.
Example 3
The invention provides a preparation method of a graphene fluorescent nano material, which comprises the following specific steps:
s1: dissolving a dispersing agent (silicon nitride-ethyl acetate) in deionized water by ultrasonic oscillation to prepare a dispersion liquid, wherein the molar concentration of the dispersion liquid is 2.5 moL/L;
s2: slowly adding graphene into the dispersion liquid, and ultrasonically vibrating, wherein the vibration dissolution frequency is 2.5KHz, and the vibration time is 15 min;
s3: n-hydroxysuccinimide and N, N-dimethyldodecylamine are prepared by reacting a mixture of 1: preparing 1.5-2.5mol/l solution according to the molar concentration ratio, adding the vibrated and dispersed graphene into the solution for activation for 1 h;
s4: the activated graphene, a ferric iron salt, ethylene glycol, nitric acid and sulfuric acid are mixed according to a mass ratio of 1: 1.5:2.5: 1.5: 1.2, carrying out ultrasonic dispersion reaction, firstly carrying out ultrasonic dispersion for 20min, reacting for 10h in a reaction kettle at 220 ℃ under the protection of nitrogen, cooling to room temperature after complete reaction, repeatedly washing reacted graphene with water and absolute ethyl alcohol, then drying the separated graphene material, and finally obtaining the primary graphene fluorescent nano material;
s5: and (5) repeating the steps S2-S4 by using the initial graphene fluorescent nano-material obtained in the step S4 to obtain the graphene fluorescent nano-material.
According to the method, graphite powder is used as a raw material, graphene powder is dispersed and activated in a solution phase, and is subjected to cyclic alkylation modification, and the modified graphene has good dispersibility in an aqueous solution or a common organic solvent due to alkyl functional groups on the graphene, so that the agglomeration of the graphene is effectively avoided. The graphene fluorescent nano material prepared by the invention can emit bright fluorescence.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A graphene fluorescent nanomaterial is characterized in that: dispersing graphene in dispersion liquid, and then adding N-hydroxysuccinimide and N, N-dimethyldodecylamine to activate in a solvent; adding activated graphene into a trivalent ferric salt, ethylene glycol, nitric acid and sulfuric acid, performing ultrasonic dispersion, performing high-temperature reaction, washing with water and ethanol, filtering and separating a graphene material, and drying to obtain the graphene fluorescent nano material.
2. The graphene fluorescent nanomaterial according to claim 1, wherein: the graphene is graphene oxide or fluorinated graphene.
3. The graphene fluorescent nanomaterial according to claim 1, wherein: the dispersion liquid is one of a silicon nitride-ethyl acetate solution or a boron nitride solution.
4. The graphene fluorescent nanomaterial according to claim 1, wherein: the graphene fluorescent nano material can be subjected to the reaction of the steps for multiple times so as to improve the purity of the graphene fluorescent nano material.
5. The graphene fluorescent nanomaterial according to claim 1, wherein: the size of the graphene fluorescent nano material is 10-15 nm.
6. The graphene fluorescent nanomaterial according to claim 1, wherein: the mass ratio of the graphene to the ferric iron salt to the glycol to the nitric acid to the sulfuric acid is 1: 0.5-1.5:2-2.5: 1.2-1.5: 1.0-1.2.
7. A preparation method of a graphene fluorescent nano material is characterized by comprising the following steps: the method comprises the following specific steps:
s1: dissolving a dispersing agent in deionized water by ultrasonic oscillation to prepare a dispersion liquid, wherein the molar concentration of the dispersion liquid is 1.0-2.5 moL/L;
s2: slowly adding graphene into the dispersion liquid, and ultrasonically vibrating, wherein the vibration dissolution frequency is 1.0-2.5KHz, and the vibration time is 10-15 min;
s3: n-hydroxysuccinimide and N, N-dimethyldodecylamine are added in a ratio of 1: preparing 1.5-2.5mol/l solution according to the molar concentration ratio, adding the vibrated and dispersed graphene into the solution for activation for 1-3 h;
s4: the activated graphene, a ferric iron salt, ethylene glycol, nitric acid and sulfuric acid are mixed according to a mass ratio of 1: 0.5-1.5:2-2.5: 1.2-1.5: 1.0-1.2, performing ultrasonic dispersion reaction, firstly performing ultrasonic dispersion for 10-20min, then performing reaction for 5-10h in a reaction kettle at the temperature of 180-220 ℃, cooling to room temperature after complete reaction, repeatedly washing reacted graphene with water and absolute ethyl alcohol, then drying the separated graphene material, and finally obtaining the primary graphene fluorescent nanomaterial;
s5: and (5) repeating the steps S2-S4 by using the initial graphene fluorescent nano material obtained in the step S4 to perform 3-5 operations, so as to obtain the graphene fluorescent nano material.
8. The preparation method of the graphene fluorescent nanomaterial according to claim 7, characterized in that: and (4) reacting in the reaction kettle of the step S4 under the protection of nitrogen.
9. The graphene fluorescent nanomaterial according to any one of claims 1 to 6, wherein the graphene fluorescent nanomaterial is used in biological imaging agents, tracers and medical fields.
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