CN115650807A - Preparation method of composite material of graphene loaded with nitrogen-containing compound - Google Patents
Preparation method of composite material of graphene loaded with nitrogen-containing compound Download PDFInfo
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- CN115650807A CN115650807A CN202211188348.9A CN202211188348A CN115650807A CN 115650807 A CN115650807 A CN 115650807A CN 202211188348 A CN202211188348 A CN 202211188348A CN 115650807 A CN115650807 A CN 115650807A
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- -1 nitrogen-containing compound Chemical class 0.000 title claims abstract description 26
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- 238000000034 method Methods 0.000 claims abstract description 10
- WUPZAQSKRMYJNB-MDZDMXLPSA-N 1,1'-azobis-1,2,3-triazole Chemical compound N1=NC=CN1\N=N\N1N=NC=C1 WUPZAQSKRMYJNB-MDZDMXLPSA-N 0.000 claims description 45
- ULRPISSMEBPJLN-UHFFFAOYSA-N 2h-tetrazol-5-amine Chemical compound NC1=NN=NN1 ULRPISSMEBPJLN-UHFFFAOYSA-N 0.000 claims description 22
- KLSJWNVTNUYHDU-UHFFFAOYSA-N Amitrole Chemical compound NC1=NC=NN1 KLSJWNVTNUYHDU-UHFFFAOYSA-N 0.000 claims description 22
- 239000013078 crystal Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 19
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- 239000000203 mixture Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- QWENRTYMTSOGBR-UHFFFAOYSA-N 1H-1,2,3-Triazole Chemical compound C=1C=NNN=1 QWENRTYMTSOGBR-UHFFFAOYSA-N 0.000 claims description 2
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 2
- YZEUHQHUFTYLPH-UHFFFAOYSA-N 2-nitroimidazole Chemical compound [O-][N+](=O)C1=NC=CN1 YZEUHQHUFTYLPH-UHFFFAOYSA-N 0.000 claims description 2
- MZRUFMBFIKGOAL-UHFFFAOYSA-N 5-nitro-1h-pyrazole Chemical compound [O-][N+](=O)C1=CC=NN1 MZRUFMBFIKGOAL-UHFFFAOYSA-N 0.000 claims description 2
- NDYLCHGXSQOGMS-UHFFFAOYSA-N CL-20 Chemical compound [O-][N+](=O)N1C2N([N+]([O-])=O)C3N([N+](=O)[O-])C2N([N+]([O-])=O)C2N([N+]([O-])=O)C3N([N+]([O-])=O)C21 NDYLCHGXSQOGMS-UHFFFAOYSA-N 0.000 claims description 2
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- UZGLIIJVICEWHF-UHFFFAOYSA-N octogen Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)CN([N+]([O-])=O)C1 UZGLIIJVICEWHF-UHFFFAOYSA-N 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 33
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- KUEFXPHXHHANKS-UHFFFAOYSA-N 5-nitro-1h-1,2,4-triazole Chemical compound [O-][N+](=O)C1=NC=NN1 KUEFXPHXHHANKS-UHFFFAOYSA-N 0.000 description 5
- 238000000113 differential scanning calorimetry Methods 0.000 description 5
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- FLDSOXFRYVOGFK-UHFFFAOYSA-N 2,5-dinitro-1h-imidazole Chemical compound [O-][N+](=O)C1=CN=C([N+]([O-])=O)N1 FLDSOXFRYVOGFK-UHFFFAOYSA-N 0.000 description 3
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- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- AUOVJYKEYXOIJD-UHFFFAOYSA-N 5-nitro-1H-1,2,4-triazole Chemical compound [N+](=O)([O-])C1=NNC=N1.[N+](=O)([O-])C1=NNC=N1 AUOVJYKEYXOIJD-UHFFFAOYSA-N 0.000 description 1
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Images
Abstract
The invention relates to a preparation method of a composite material of graphene loaded with a nitrogen-containing compound, belonging to the technical field of preparation of energy-containing composite materials. According to the invention, the surface affinity of graphene is improved by using the change of temperature, and the interaction between the desensitizer and the energetic material is enhanced by using the nano-size effect of the graphene, so that the mechanical sensitivity of the energetic material is favorably reduced; the invention is suitable for most energetic materials which are not easy to dissolve in water, and has strong universality; the preparation method has simple process, only needs to stir in the dispersed preparation solution, can realize large-scale batch preparation, and has better application prospect.
Description
Technical Field
The invention relates to a preparation method of a composite material of graphene loaded with a nitrogen-containing compound, belonging to the technical field of preparation of energy-containing composite materials.
Background
The energetic material is used as an indispensable power and power energy source of various weapon systems in a military national defense system, and can be widely used for various strategic and tactical weapon systems. The high energy of energetic materials is an important performance parameter, and the safety performance is one of the restriction factors of the preparation and the application of the energetic materials. Therefore, balancing the high energy level and the high safety performance of the energetic material, especially reducing the mechanical sensitivity of the energetic material, becomes an important research target in design and preparation experiments of the energetic material. At present, one of the methods commonly used in the prior art to reduce the mechanical sensitivity of energetic materials is to introduce a desensitizer into the energetic materials, so as to effectively reduce the sensitivity of the materials and improve the safety performance. Based on the situation, the effective desensitizer is developed, so that the comprehensive properties of energetic materials such as energy, process, sensitivity and the like are improved, the high energy and safety of the energetic materials can be balanced, the energetic materials can be applied to weapon systems more efficiently and more safely, and the important significance on the safe development of the energetic materials is realized.
Since the desensitizer added to energetic materials generally requires a large heat capacity and a small thermal conductivity, scientists generally use wax, graphite, polymer or low-sensitive energetic materials as the desensitizer. For example, wax-type phlegmatizers can produce strong endothermic effects, thereby reducing the sensitivity of nitramine-type explosives; the graphite insensitive agent can generate buffering mechanical energy and lubricating effect, thereby effectively reducing the impact sensitivity and the friction sensitivity of the energetic material. At present, due to the advantages of a lamellar structure with a large specific surface area, good electric and thermal conductivity, good mechanical properties and the like, the graphene and the derivatives thereof can be used for improving the thermal stability and the mechanical sensitivity of the energetic material. When the graphene and the derivatives thereof are used as an energetic material desensitizer, attention is paid to the existence of the graphene and the derivatives thereof, for example, a flaky fold structure influences the bulk density of crystals of an energetic material or an agglomeration effect causes the addition amount of the crystals to be increased, and the energy density of the energetic material is negatively influenced. Therefore, the reasonable introduction of the graphene and the derivatives thereof is beneficial to playing a larger role as a desensitizer at a lower dosage and avoiding the influence on the energy of the energetic material.
Disclosure of Invention
The invention aims to solve the problem that the addition of graphene serving as a desensitizer influences the bulk density of crystals of an energetic material, and provides a preparation method of a composite material with graphene loaded with a nitrogen-containing compound. The composite material is prepared by adopting a temperature auxiliary solution mixing method, the surface affinity of the graphene is improved by utilizing the change of temperature, and the interaction between the insensitive agent and the energetic material is enhanced by utilizing the nano-size effect of the graphene, so that the molecular accumulation of the energetic material is more regular, the higher energy density is kept, and the mechanical sensitivity of the energetic material is reduced.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a nitrogen-containing compound loaded graphene composite material comprises the following steps:
step one, dispersing graphene powder with a certain mass in 5mL of water, stirring, and performing ultrasonic treatment to uniformly disperse the graphene powder to obtain a solution A.
And step two, dispersing a certain mass of nitrogen-containing compound in a corresponding good solvent, and stirring to dissolve the nitrogen-containing compound to obtain a solution B.
And step three, heating the solution B to a certain temperature, adding the solution A into the solution B, stirring for a certain time, and stopping heating.
And step four, standing the mixed solution at room temperature for a period of time until crystals are separated out, and centrifuging, washing and freeze-drying to obtain the graphene-loaded nitrogen-containing compound composite material.
Wherein the water is water with the purity of deionized water or more, and the solvent is a good solvent of the nitrogen-containing compound.
Preferably, the graphene in the preparation process is any one or a mixture of more of graphene oxide and reduced graphene oxide; the mass taken is 0mg-1000mg.
Preferably, the nitrogen-containing compound in the preparation process comprises one or more of azotriazole, 5-aminotetrazole, 2-methylimidazole, 2-nitroimidazole, 3-nitropyrazole, 1,2, 3-triazole, 3-amino-1, 2,4-triazole, pyrazole, CL-20, HMX and the like.
Preferably, the mass of the nitrogen-containing compound in the step two in the preparation process is 0mg-1000mg.
Preferably, the mass percentage of the nitrogen-containing compound to the graphene in the preparation process is 0-100%.
Preferably, the reaction heating temperature of the step (3) is 40-100 ℃, and the stirring time is 1-6h.
Preferably, the reaction stirring speed of the steps (1), (2) and (3) is 500-800rpm.
Preferably, the standing time of the mixed solution in the step (4) is 8-48h.
Preferably, the centrifugal rotation speed of the step (4) is 3000-10000 r/min, and the centrifugal time is 5-20 min; the washing is carried out for 3 to 5 times by using deionized water; the drying is freeze drying.
Advantageous effects
According to the invention, the surface affinity of graphene is improved by using the change of temperature, and the interaction between the insensitive agent and the energetic material is enhanced by using the nano-size effect of the graphene, so that the molecular accumulation of the energetic material is more regular, the higher energy density is kept, and the mechanical sensitivity of the energetic material is favorably reduced; the invention is suitable for most energetic materials which are not easy to dissolve in water, and has strong universality; the preparation method has simple process, only needs to stir in the dispersed preparation solution, can be used for large-scale batch preparation, and has better application prospect.
Drawings
Fig. 1 is a transmission electron microscope picture of Graphene Oxide (GO).
FIG. 2 is X-ray diffraction patterns of raw material Graphene Oxide (GO), reduced Graphene Oxide (RGO), 3-amino-1, 2,4-triazole (AT), products AT-GO (10), AT-RGO (10) and control group products AT/GO mix and AT/RGO mix.
FIG. 3 shows X-ray diffraction patterns of Graphene Oxide (GO), azotriazole (ATRZ), ATRZ-GO, and control ATRZ/GO mixure, ATRZ @ GO.
Fig. 4 is an optical microscope bright field picture of a composite material ATRZ-GO obtained by loading Azotriazole (ATRZ) on Graphene Oxide (GO).
Fig. 5 is a Scanning Electron Microscope (SEM) picture of a composite material ATRZ-GO obtained by loading Azotriazole (ATRZ) on Graphene Oxide (GO).
FIG. 6 is a DSC characterization of Graphene Oxide (GO) loaded Azotriazole (ATRZ) resulting composite ATRZ-GO.
FIG. 7 is an X-ray diffraction spectrum of a graphene oxide supported 5-aminotetrazole composite material 5-ATZ-GO (10).
FIG. 8 is an X-ray diffraction pattern of graphene oxide supported 5-aminotetrazole composite 5-ATZ-GO (20.
FIG. 9 is an X-ray diffraction pattern of 3-Nitro-1,2,4-triazole composite material 3-Nitro-1,2,4-triazole loaded with graphene oxide.
FIG. 10 is an X-ray diffraction pattern of graphene oxide-supported 2,4-Dinitroimidazole composite material 2,4-Dinitroimidazole-GO.
FIG. 11 is a light-field image of an optical microscope of the obtained ATRZ crystal.
FIG. 12 is a DSC characterization of Azotriazole (ATRZ) crystals.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
(1) 42mg of Graphene Oxide (GO) is dispersed in 5mL of water, and is uniformly dispersed by stirring and ultrasonic treatment to obtain a solution A.
(2) 420mg of 3-amino-1, 2,4-triazole (AT) was dispersed in 10mL of water and dissolved by stirring to obtain a solution B.
(3) Heating the solution B to 50 ℃, adding the solution A into the solution B, stirring for 2 hours, and stopping heating.
(4) Standing the mixed solution AT room temperature for a period of time until crystals are separated out, and centrifuging, washing and freeze-drying to obtain the graphene oxide loaded 3-amino-1, 2,4-triazole composite material AT-GO (10.
(5) Fig. 1 is a transmission electron microscope picture of Graphene Oxide (GO); fig. 2 is an X-ray diffraction spectrum of the raw material Graphene Oxide (GO), 3-amino-1, 2,4-triazole (AT), and the product AT-GO (10).
Example 2
(1) And reducing the graphene oxide by sodium borohydride to obtain Reduced Graphene Oxide (RGO).
(2) And dispersing 42mg of the reduced graphene oxide obtained in the step (A) in 5mL of water, stirring and performing ultrasonic treatment to uniformly disperse the reduced graphene oxide to obtain a solution A. The rest of the experimental steps are the same as those in example 1, so that the composite material AT-RGO (10.
(3) FIG. 2 shows the X-ray diffraction patterns of Reduced Graphene Oxide (RGO), 3-amino-1, 2,4-triazole (AT) and the product AT-RGO (10).
Example 3
(1) Dispersing 200mg of Graphene Oxide (GO) in 5mL of water, stirring and ultrasonically dispersing uniformly to obtain a solution A.
(2) 82mg of Azotriazole (ATRZ) was dispersed in 10mL of water and dissolved by heating to obtain solution B.
(3) Heating the solution B to 80 ℃, adding the solution A into the solution B, stirring for 2 hours, and stopping heating.
(4) Standing the mixed solution at room temperature for a period of time until crystals are separated out, and centrifuging, washing and freeze-drying to obtain the graphene oxide loaded azotriazole composite material ATRZ-GO.
(5) The decomposition temperature of the Graphene Oxide (GO) loaded Azotriazole (ATRZ) composite material ATRZ-GO is measured through Differential Scanning Calorimetry (DSC), and the result shows that the thermal decomposition temperature of the ATRZ crystal is reduced due to the doping of the Graphene Oxide (GO), because the graphene oxide is a high-thermal-conductivity material and the crystal is more prone to thermal decomposition due to the faster thermal-conductivity speed.
(6) Fig. 3 shows X-ray diffraction spectra of Graphene Oxide (GO), azotriazole (ATRZ) and the product ATRZ-GO in this example. Fig. 4 is an optical microscope bright field image of the composite material ATRZ-GO obtained by loading Azotriazole (ATRZ) with Graphene Oxide (GO) in this example. Fig. 5 is a Scanning Electron Microscope (SEM) image of a composite material ATRZ-GO obtained by loading Azotriazole (ATRZ) with Graphene Oxide (GO) in this example. FIG. 6 is a DSC representation of the composite ATRZ-GO obtained by loading Azotriazole (ATRZ) with Graphene Oxide (GO) in this example.
Example 4
(1) 42mg of Graphene Oxide (GO) is dispersed in 5mL of water, and is uniformly dispersed by stirring and ultrasonic treatment to obtain a solution A.
(2) 420mg of 5-Aminotetrazole (5-Aminotetrazole, 5-ATZ) was dispersed in 10mL of water and dissolved by stirring to obtain solution B.
(3) Heating the solution B to 80 ℃, adding the solution A into the solution B, stirring for 2 hours, and stopping heating.
(4) Standing the mixed solution at room temperature for a period of time until crystals are separated out, and centrifuging, washing and freeze-drying to obtain the graphene oxide loaded 5-aminotetrazole composite material 5-ATZ-GO (10.
(5) 420mg of 5-aminotetrazole (5-ATZ) was ground to obtain a solid powder, and 42mg of Graphene Oxide (GO) was added and ground to mix well to obtain a solid mixture 5-ATZ/GO mixture as a control.
(6) Fig. 7 is an X-ray diffraction spectrum of a composite material 5-ATZ-GO (10) of graphene oxide supported 5-aminotetrazole, raw materials Graphene Oxide (GO), 5-aminotetrazole (5-ATZ), and a solid mixture 5-ATZ/GO mixture as a control group. The result shows that the 5-ATZ crystallization is influenced by adding excessive Graphene Oxide (GO), so that the graphene can be reasonably introduced to play the optimal role as a desensitizer, and the energy effect of an energy-containing compound is prevented from being weakened.
Example 5
(1) Dispersing 21mg of Graphene Oxide (GO) in 5mL of water, stirring and performing ultrasonic treatment to uniformly disperse the Graphene Oxide (GO) to obtain a solution A.
(2) 420mg of 5-Aminotetrazole (5-Aminotetrazole, 5-ATZ) was dispersed in 10mL of water and dissolved by stirring to obtain a solution B.
(3) Heating the solution B to 80 ℃, adding the solution A into the solution B, stirring for 2 hours, and stopping heating.
(4) Standing the mixed solution at room temperature for a period of time until crystals are separated out, and centrifuging, washing and freeze-drying to obtain the graphene oxide loaded 5-aminotetrazole composite material 5-ATZ-GO (20.
(5) FIG. 8 is an X-ray diffraction pattern of graphene oxide supported 5-aminotetrazole composite 5-ATZ-GO (20. The results show that the addition of graphene oxide makes the intra-crystalline molecular arrangement of 5-ATZ more dense.
Example 6
(1) Dispersing 21mg of Graphene Oxide (GO) in 5mL of water, stirring and performing ultrasonic treatment to uniformly disperse the Graphene Oxide (GO) to obtain a solution A.
(2) 420mg of 3-Nitro-1,2,4-triazole (3-Nitro-1, 2, 4-triazole) was dispersed in 10mL of water and dissolved by stirring to obtain a solution B.
(3) Heating the solution B to 80 ℃, adding the solution A into the solution B, stirring for 2 hours, and stopping heating.
(4) Standing the mixed solution at room temperature for a period of time until crystals are separated out, centrifuging, washing, and freeze-drying to obtain the graphene oxide loaded 3-Nitro-1,2,4-triazole composite material 3-Nitro-1,2,4-triazole-GO.
(5) FIG. 9 is an X-ray diffraction pattern of 3-Nitro-1,2,4-triazole composite material 3-Nitro-1,2,4-triazole loaded with graphene oxide.
Example 7
(1) Dispersing 21mg of Graphene Oxide (GO) in 5mL of water, stirring and performing ultrasonic treatment to uniformly disperse the Graphene Oxide (GO) to obtain a solution A.
(2) 420mg of 2,4-Dinitroimidazole (2, 4-Dinitroimidazole) was dispersed in 10mL of water and dissolved by stirring to obtain a solution B.
(3) Heating the solution B to 80 ℃, adding the solution A into the solution B, stirring for 2 hours, and stopping heating.
(4) Standing the mixed solution at room temperature for a period of time until crystals are separated out, centrifuging, washing, and freeze-drying to obtain the graphene oxide loaded 2,4-Dinitroimidazole composite material 2,4-Dinitroimidazole-GO.
(5) FIG. 10 is an X-ray diffraction pattern of graphene oxide-supported 2,4-Dinitroimidazole composite material 2,4-Dinitroimidazole-GO.
(1) Grinding 420mg of 3-amino-1, 2,4-triazole (AT) to obtain solid powder, adding 42mg of Graphene Oxide (GO) and grinding to mix uniformly to obtain a solid mixture AT/GO mixture.
(2) And reducing the graphene oxide by sodium borohydride reduction to obtain Reduced Graphene Oxide (RGO). 420mg of 3-amino-1, 2,4-triazole (AT) was ground to obtain a solid powder, and 42mg of Reduced Graphene Oxide (RGO) was added thereto and ground to mix them uniformly to obtain a solid mixture AT/RGO mix.
(3) In FIG. 2, AT/GO texture and AT/RGO texture are X-ray diffraction patterns of the solid mixture obtained in the present control group.
(1) And dispersing 200mg of Graphene Oxide (GO) in 5mL of water, stirring and performing ultrasonic treatment to uniformly disperse the Graphene Oxide (GO) to obtain a solution A.
(2) 82mg of Azotriazole (ATRZ) was dispersed in 10mL of water and dissolved by heating to obtain solution B.
(3) Adding the solution A into the solution B, stirring and mixing, immediately standing for a period of time until crystals are separated out, and centrifuging, washing and freeze-drying to obtain the Graphene Oxide (GO) and Azotriazole (ATRZ) crystals ATRZ @ GO.
(4) In FIG. 3, ATRZ @ GO is the X-ray diffraction spectrum of the crystal ATRZ @ GO of the Graphene Oxide (GO) composite Azotriazole (ATRZ) of the control group.
(1) 82mg of Azotriazole (ATRZ) is ground to obtain solid powder, and 200mg of Graphene Oxide (GO) is added and ground to be uniformly mixed to obtain a solid mixture ATRZ/GO mixture. ATRZ/GO mix in FIG. 3 is the X-ray diffraction pattern of the resulting solid mixture.
(2) 82mg of Azotriazole (ATRZ) was dispersed in 10mL of water, heated to dissolve it, immediately allowed to stand for a while until crystals precipitated, and centrifuged, washed, and dried to obtain Azotriazole (ATRZ) crystals. FIG. 11 is a light-field image of an optical microscope of the obtained ATRZ crystal. FIG. 12 is a DSC characterization of Azotriazole (ATRZ) crystals.
In summary, the invention includes but is not limited to the above embodiments, and any equivalent substitutions or partial modifications made under the spirit and principle of the invention are considered to be within the protection scope of the invention.
Claims (6)
1. A preparation method of a composite material of graphene loaded with nitrogen-containing compounds is characterized by comprising the following steps: the method comprises the following steps:
dispersing graphene powder in water, stirring and ultrasonically dispersing the graphene powder uniformly to obtain a solution A;
dispersing the nitrogen-containing compound in a corresponding good solvent, and completely dissolving to obtain a solution B;
and step three, heating the solution B, adding the solution A after the solution B reaches a certain temperature, stirring for a period of time, stopping heating, standing until crystals are separated out, and centrifuging, washing and freeze-drying to obtain the graphene nitrogen-containing compound loaded composite material.
2. The preparation method of the nitrogen-containing compound supported graphene composite material according to claim 1, wherein the nitrogen-containing compound is supported on the graphene: the graphene is any one or a mixture of more of graphene oxide and reduced graphene oxide; the mass taken is 0mg-1000mg.
3. The method for preparing the nitrogen-containing compound supported graphene composite material according to claim 1, wherein the method comprises the following steps: the nitrogen-containing compound comprises one or more of azotriazole, 5-aminotetrazole, 2-methylimidazole, 2-nitroimidazole, 3-nitropyrazole, 1,2, 3-triazole, 3-amino-1, 2,4-triazole, pyrazole, CL-20, HMX and the like; the mass taken is 0mg-1000mg.
4. The method for preparing the nitrogen-containing compound supported graphene composite material according to claim 1, wherein the method comprises the following steps: the mass percentage of the nitrogen-containing compound to the graphene is 0-100%.
5. The preparation method of the nitrogen-containing compound supported graphene composite material according to claim 1, wherein the nitrogen-containing compound is supported on the graphene: and step three, the certain temperature is 40-100 ℃, and the stirring time is 1-6h.
6. The preparation method of the nitrogen-containing compound supported graphene composite material according to claim 1, wherein the nitrogen-containing compound is supported on the graphene: the centrifugal rotating speed is 3000-10000 r/min, and the centrifugal time is 5-20 min; the washing is carried out for 3 to 5 times by using deionized water; the drying is freeze drying.
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