CN108889326B - Preparation method of three-dimensional network frame of molybdenum disulfide and graphite phase carbon nitride - Google Patents
Preparation method of three-dimensional network frame of molybdenum disulfide and graphite phase carbon nitride Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 44
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 17
- 239000010439 graphite Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 13
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 10
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- MZRVEZGGRBJDDB-UHFFFAOYSA-N n-Butyllithium Substances [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims description 4
- -1 n-butyl lithium modified molybdenum disulfide Chemical class 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 238000002390 rotary evaporation Methods 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011261 inert gas Substances 0.000 abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 239000011733 molybdenum Substances 0.000 abstract description 2
- 238000006068 polycondensation reaction Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 239000010406 cathode material Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 229910052961 molybdenite Inorganic materials 0.000 description 2
- 230000001443 photoexcitation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000002019 disulfides Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229960000789 guanidine hydrochloride Drugs 0.000 description 1
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920005553 polystyrene-acrylate Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
Abstract
The invention discloses a preparation method of a three-dimensional network frame of molybdenum disulfide and graphite-phase carbon nitride, belonging to the field of preparation of porous materials. Molybdenum disulfide, cyanuric acid and melamine are added into a reaction kettle which takes water as solvent, stirred and dried at a fixed temperature to obtain a precursor. And placing the precursor in a furnace body with the function of introducing gas, controlling the gas flow rate and the heating rate, and calcining to obtain the molybdenum disulfide and graphite phase carbon nitride layer-by-layer composite three-dimensional network frame material. The invention has the advantages that: the method is characterized in that melamine and cyanuric acid are self-assembled in a solution to form melamine cyanurate, the melamine cyanurate is intercalated between layers of molybdenum disulfide and then used as a carbon source and a nitrogen source of graphite-phase carbon nitride, the carbon source and the nitrogen source are calcined in inert gas to generate a thermal polycondensation reaction, the molybdenum disulfide-graphite-phase carbon nitride layer-by-layer composite material is prepared, the aperture of a three-dimensional network frame is controlled by a method capable of changing the mass ratio of raw materials, and the process is simple.
Description
Technical Field
The invention relates to a preparation method of a three-dimensional network frame of molybdenum disulfide and graphite-phase carbon nitride, belongs to the field of preparation of porous materials, and can be used in the field of photocatalysis and the field of lithium ion battery cathode materials.
Background
Molybdenum disulfide (molybdenum disulfide), abbreviated MoS2Transition metal disulfides are typical two-dimensional sheet materials. Single-layer MoS2Is a sandwich structure of two layers of sulfur atoms and one layer of molybdenum atoms, the layers are combined together by Van der Waals force, and the distance between each layer is about 0.65 nm. Molybdenum disulfide possesses an energy band gap of 1.8eV, has great development potential in a nano transistor, and can be used as a linear photoconductor and a semiconductor for displaying P-type or N-type conductivity. Graphite-phase carbon nitride (graphic carbon nitride), abbreviated as g-C3N4It is the most stable carbon nitride allotrope and a very promising non-metal catalyst. Has been widely applied to the fields of hydrogen production by photolysis, photocatalysis, and the like. Has received much attention because of its excellent properties.
At present, graphite-phase carbon nitride (adv.Funct.Mater.2013,23(29): 3661-3667.) can be effectively prepared by adopting the thermal polycondensation reaction of the melamine cyanurate supramolecular assembly under the high-temperature condition, and the lamellar structure of the graphite-phase carbon nitride can induce stronger light absorption, and the energy band gap can be effectively increased by 0.16 eV. The three-dimensional reticular framework structure has high specific surface area and rich pore channels, can expose more active point sites, and further improves the performance of application in catalytic reaction and the like and the mass transfer diffusion of reactants and products in multiphase reaction. Molybdenum disulfide is sufficiently contacted with graphite phase carbon nitride to form heterojunction, and because of the difference between conduction band and valence band, electrons or holes generated by graphite phase carbon nitride due to photoexcitation can be transferred into conduction band or valence band of the compound, so that electron-hole separation and recombination rate are reduced, and thus active particles generated by photoexcitation can be more effectively utilized, and the catalytic efficiency is improved (Chemical Reviews,2016,116(12): 7159-7329.). In the application aspect of the lithium ion battery cathode material, the graphite-phase carbon nitride can block the movement of the molybdenum disulfide sheet layer to prevent the molybdenum disulfide sheet layer from agglomerating, and relieve the mechanical stress caused by the volume change of the molybdenum disulfide sheet layer. The three-dimensional network frame can accelerate the diffusion of lithium ions, so that the lithium ions can be fully contacted with molybdenum disulfide, and the rapid charge and discharge of the material are facilitated (adv. Mater.2014,26, 964-969).
At present, the patents for preparing a network structure by molybdenum disulfide modification include: a three-dimensional porous network composite material of molybdenum disulfide and carbon and a preparation method (publication number: CN 104966817A, 2015, 10 months and 7 days, Tianjin university) are adopted, sodium chloride is used as a dispersing agent and a template, ammonium molybdate and sodium molybdate are adopted, thiourea is dissolved in ionized water and freeze-dried, and a mixture is calcined in a tubular furnace and washed with water to remove the sodium chloride, so that a product is obtained. The three-dimensional porous graphene-loaded molybdenum disulfide composite material and the preparation method (publication number: CN104966812A, 10 months and 7 days in 2015, Tianjin university) adopt sodium chloride as a dispersing agent and a template, fully dissolve and mix the sodium chloride with a molybdenum source, a sulfur source and an organic carbon source, freeze-dry and grind to obtain a mixture; and putting the mixture into a tubular furnace, and calcining under the protection of argon to obtain a calcined product, thereby obtaining the three-dimensional porous graphene-like molybdenum disulfide-loaded composite material.
Patents for the preparation of graphite phase carbon nitride include: a method for preparing graphite phase carbon nitride material (publication number: CN106540733A, 3 and 29 days in 2017, and university of Tai Yuan chemical) uses dicyandiamide and nano-silica as precursors, and prepares graphite-like carbon nitride with high specific surface area by microwave roasting and muffle furnace roasting. A process for synthesizing porous graphite-phase carbon nitride includes such steps as preparing the microemulsion of polystyrene or polymethyl methacrylate as hard template, preparing cyanamide, dicyandiamide or guanidine hydrochloride as precursor, direct mixing, drying and calcining in inert gas atmosphere.
Disclosure of Invention
The invention aims to provide a preparation method of a three-dimensional network frame of molybdenum disulfide and graphite phase carbon nitride. The composite material can be used as a porous material in the fields of photocatalysis and lithium ion battery cathode materials. Has wide application prospect, simple preparation method process and large-scale production.
The three-dimensional network frame is a three-dimensional network frame structure which is built by compounding flaky molybdenum disulfide nanosheets and graphite phase carbon nitride layers, the network aperture is 10-200nm, the total mass of the compound is 100%, the mass percentage of molybdenum disulfide is 50-95%, and the mass percentage of graphite phase carbon nitride is 5-50%.
The preparation method of the three-dimensional network frame of the molybdenum disulfide and graphite phase carbon nitride layer-by-layer composite material with the structure is characterized by comprising the following steps:
(1) adding molybdenum disulfide, melamine and cyanuric acid into a reaction kettle using water as a solvent, stirring for 4 hours at a fixed temperature, removing the solvent and drying to obtain a precursor. The molybdenum disulfide comprises n-butyllithium modified molybdenum disulfide, the precursor only comprises molybdenum disulfide and melamine cyanurate, and the mass ratio of the melamine cyanurate is 0.05-20 calculated by taking the mass of the molybdenum disulfide as 1. The melamine cyanurate is obtained by hydrogen bond self-assembly of equal mass of melamine and cyanuric acid in aqueous solution. The fixed temperature range of the reaction is between room temperature and 100 ℃, and the optimal temperature is 80 ℃.
(2) Will be described in detail(1) The prepared precursor is placed in a tubular furnace, a muffle furnace or other heatable furnace bodies with the function of gas introduction, protective gas is introduced into the furnace bodies at a certain gas flow rate, and the temperature is raised. And keeping the fixed gas flow and the heating rate, heating to a fixed temperature, keeping the temperature, and calcining for 30-200 minutes to obtain the three-dimensional network frame of the molybdenum disulfide and graphite phase carbon nitride layer-by-layer composite material. The protective gas is nitrogen (N)2) Argon (Ar) or helium (He). The gas flow is 100-400 ml/min, wherein the optimal gas flow is 200 ml/min. The heating rate is 1-50 ℃/min, and the optimal heating rate value is 10-30 ℃/min. The fixed temperature is 300-700 ℃.
The invention has the advantages and positive effects that: by adopting the technical scheme, the melamine and the cyanuric acid are self-assembled in hydrogen bonds between the molybdenum disulfide layers to form the melamine cyanurate, so that the effect of intercalation between the molybdenum disulfide layers is achieved. And then the melamine cyanurate is thermally condensed into graphite-phase carbon nitride under the protection of inert gas and heating at controlled temperature. The aperture size of the three-dimensional network frame is controlled by controlling the mass ratio of the molybdenum disulfide to the melamine cyanurate. The method has the advantages of low cost, simple reaction process and strong controllability.
Drawings
FIG. 1 is a scanning electron micrograph of a three-dimensional network framework of a layer-by-layer composite of molybdenum disulfide and graphite-phase carbon nitride obtained in example 3 of the present invention. The three-dimensional network framework structure of the material is evident from the figure.
Detailed Description
The invention is further illustrated by the following examples, which do not limit the scope of the invention. (all the raw materials are commercially available analytical pure)
Example 1
Weighing 0.517 g of molybdenum disulfide, 0.602 g of melamine and 0.602 g of cyanuric acid, adding the materials into a reaction kettle containing 1000ml of deionized water, heating to 95 ℃, stirring for 3h, filtering to obtain a precursor product, and drying in vacuum for 4h at 80 ℃. And (3) placing the precursor in a tube furnace, introducing argon gas with the gas flow rate of 500ml/min, heating to 550 ℃ at the heating rate of 2.3 ℃/min, and preserving heat for 1 h. And after the reaction is finished, cooling to room temperature under the protection of argon atmosphere to obtain a three-dimensional network frame of the molybdenum disulfide and graphite phase carbon nitride layer-by-layer composite material, and measuring the aperture of a product prepared by the formula to be 98 nm.
Example 2
Weighing 0.511 g of n-butyllithium modified molybdenum disulfide, 1.011 g of melamine and 1.089 g of cyanuric acid, adding the materials into a reaction kettle containing 1000ml of deionized water, heating to 80 ℃, stirring for 4 hours, and filtering to obtain a precursor product. And (3) placing the precursor in a tube furnace, introducing nitrogen gas with the gas flow rate of 300ml/min, heating to 650 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1 h. And after the reaction is finished, cooling to room temperature under the protection of nitrogen atmosphere to obtain a three-dimensional network frame of the molybdenum disulfide and graphite phase carbon nitride layer-by-layer composite material, and measuring the aperture of a product prepared by the formula to be 10 nm.
Example 3
Weighing 0.501 g of n-butyllithium modified molybdenum disulfide, 0.595 g of melamine and 0.612 g of cyanuric acid, adding the weighed materials into a reaction kettle containing 1000ml of deionized water, heating to 70 ℃, stirring for 4 hours, and filtering to obtain a precursor product. Placing the precursor in a tube furnace, introducing helium gas with the gas flow rate of 100ml/min, heating to 650 ℃ at the heating rate of 50 ℃/min, and preserving heat for 1 h. And after the reaction is finished, cooling to room temperature under the protection of helium atmosphere to obtain a three-dimensional network frame of the molybdenum disulfide and graphite phase carbon nitride layer-by-layer composite material, and measuring the aperture of a product prepared by the formula to be 27 nm.
Claims (11)
1. A preparation method of a three-dimensional network frame of molybdenum disulfide and graphite phase carbon nitride comprises the following steps: (1) adding molybdenum disulfide, melamine and cyanuric acid into a reaction kettle using water as a solvent, stirring for 4 hours at a fixed temperature, removing the solvent and drying to obtain a precursor; (2) placing the precursor prepared in the step (1) in a tubular furnace, a muffle furnace or other heatable furnace bodies with the function of introducing gas, introducing protective gas into the furnace bodies at a certain gas flow rate, and starting to heat; keeping the fixed gas flow and the heating rate, heating to a fixed temperature, keeping the temperature and calcining for a period of time to obtain the three-dimensional network frame of the molybdenum disulfide and graphite phase carbon nitride layer-by-layer composite material.
2. The method of claim 1, wherein the method comprises the steps of: the molybdenum disulfide used as the raw material is unmodified molybdenum disulfide or n-butyl lithium modified molybdenum disulfide.
3. The method of claim 1, wherein the method comprises the steps of: the precursor comprises molybdenum disulfide and melamine cyanurate, the mass ratio of the melamine cyanurate is 0.05-20 calculated by taking the mass of the molybdenum disulfide as 1, wherein the melamine cyanurate is obtained by self-assembling equal mass of melamine and cyanuric acid in hydrogen bonds in an aqueous solution.
4. The method of claim 1, wherein the method comprises the steps of: the fixed temperature range in the reaction process is room temperature-100 ℃.
5. The method of claim 1, wherein the method comprises the steps of: the solvent removing process comprises natural drying, suction filtration or vacuum rotary evaporation.
6. The method of claim 1, wherein the method comprises the steps of: and (3) placing the precursor in the step (1) in a furnace body of a tubular furnace, a muffle furnace or other furnace bodies with controllable heating rate and gas introduction functions.
7. The method of claim 1, wherein the method comprises the steps of: the protective gas introduced into the furnace body is nitrogen (N)2) Argon (Ar) orHelium (He).
8. The method of claim 1, wherein the method comprises the steps of: the gas flow rate of introducing the protective gas into the furnace body is 100-400 ml/min.
9. The method of claim 1, wherein the method comprises the steps of: the heating rate is 1-50 ℃/min in the heating process.
10. The method of claim 1, wherein the method comprises the steps of: the furnace body is heated to a fixed temperature, and the fixed temperature range is 300-700 ℃.
11. The method of claim 1, wherein the method comprises the steps of: the calcination time at a fixed temperature is 30-200 min.
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CN111111700B (en) * | 2020-01-22 | 2022-01-14 | 复旦大学 | Few-layer molybdenum disulfide/nitrogen-doped porous carbon composite catalyst and preparation method thereof |
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