CN108889326A - A kind of preparation method of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride - Google Patents
A kind of preparation method of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride Download PDFInfo
- Publication number
- CN108889326A CN108889326A CN201810738052.7A CN201810738052A CN108889326A CN 108889326 A CN108889326 A CN 108889326A CN 201810738052 A CN201810738052 A CN 201810738052A CN 108889326 A CN108889326 A CN 108889326A
- Authority
- CN
- China
- Prior art keywords
- molybdenum disulfide
- carbon nitride
- phase carbon
- dimensional network
- graphite phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 37
- 239000010439 graphite Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920000877 Melamine resin Polymers 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
- 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 10
- 238000000034 method Methods 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000001338 self-assembly Methods 0.000 claims abstract description 3
- 238000010792 warming Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- -1 n-BuLi modified molybdenum disulfide Chemical class 0.000 claims description 4
- MZRVEZGGRBJDDB-UHFFFAOYSA-N n-Butyllithium Substances [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001727 in vivo Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 238000002390 rotary evaporation Methods 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 19
- 239000002131 composite material Substances 0.000 abstract description 7
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000011229 interlayer Substances 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 239000011261 inert gas Substances 0.000 abstract description 3
- 238000006068 polycondensation reaction Methods 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 238000009830 intercalation Methods 0.000 abstract description 2
- 230000002687 intercalation Effects 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000005864 Sulphur Substances 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
- 238000004458 analytical method Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 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
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920002223 polystyrene 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
- 239000004065 semiconductor Substances 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
- 239000004575 stone Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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 the preparation methods of a kind of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride, belong to the preparation field of porous material.Molybdenum disulfide, cyanuric acid and melamine are added in the reaction kettle taken water as a solvent for invention, stir under fixed temperature and are dried to obtain presoma.Presoma is placed in have and is passed through in the furnace body of gas function, gas flow rate is controlled and heating rate is calcined, obtain molybdenum disulfide and graphite phase carbon nitride three-dimensional network frame material compound layer by layer.The invention has the advantages that：It is self-assembly of melamine cyanurate in the solution with melamine and cyanuric acid, and it is intercalation into molybdenum disulfide interlayer, then as the carbon source of graphite phase carbon nitride and nitrogen source, thermal polycondensation reaction is generated by calcining in inert gas, prepare molybdenum disulfide and graphite phase carbon nitride composite material layer by layer, and the method for the mass ratio of changeable raw material controls three-dimensional network frame aperture, process is simple.
Description
Technical field
The present invention relates to the preparation methods of a kind of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride, belong to porous
The preparation field of material can be used for photocatalysis field and lithium ion battery negative material field.
Background technique
Molybdenum disulfide (molybdenum disulfide), is abbreviated as MoS2, belong to transition metal dichalcogenide, be a kind of
Typical two-dimensional slice material.The MoS of single layer2It is that two layers of sulphur atom clips one layer of molybdenum atom " sandwich " interlayer structure, layer
It is combined together between layer by Van der Waals force, the distance between every layer about 0.65nm.Molybdenum disulfide possesses the energy band of 1.8eV
Gap possesses very big development potentiality in nano-transistor, can be used as linear photoconductor conductor and show p-type or N-type conductivity can
Semiconductor.Graphite phase carbon nitride (graphitic carbon nitride), is abbreviated as g-C3N4, it is carbonitride the most stable
Allotrope is a kind of very promising non-metallic catalyst.The hydrogen manufacturing of the photodegradation that has been widely used water, photocatalysis etc.
Field.It is received significant attention because it has excellent performance.
The lower thermal polycondensation reaction using melamine cyanurate super-molecule assembling body in hot conditions can effectively make at present
Obtain graphite phase carbon nitride (Adv.Funct.Mater.2013,23 (29):3661-3667.) it, can induce with its layer structure stronger
Light absorption, band gap can effectively increase 0.16eV.Three-dimensional netted frame structure has high-specific surface area and duct abundant, energy
More active points are exposed, reactant and product in the performances and heterogeneous reaction of applications such as catalysis reaction are then lifted at
Mass transfer diffusion.Molybdenum disulfide and graphite phase carbon nitride, which come into full contact with, can form hetero-junctions, because of the difference of its conduction band and valence band, stone
Black phase carbon nitride is since the electronics of light excitation generation or hole can be transferred in the conduction band or valence band of compound, electron hole point
From recombination rate reduces, and so as to the active particle for more efficiently utilizing light excitation to generate, improves catalytic efficiency (Chemical
Reviews,2016,116(12):7159-7329.).In lithium ion battery negative material application aspect, graphite phase carbon nitride can
Stop the movement of molybdenum disulfide lamella to prevent its reunion, alleviates mechanical stress caused by its volume change.And three-dimensional network frame can
The diffusion for accelerating lithium ion, is allowed to come into full contact with molybdenum disulfide, is conducive to the fast charging and discharging of material
(Adv.Mater.2014,26,964-969)。
Have at present for the patent of the modified preparation network structure of molybdenum disulfide：The three-dimensional porous network of molybdenum disulfide and carbon is multiple
Condensation material and preparation method (publication number：CN 104966817A, on October 7th, 2015, University Of Tianjin), it is dispersion with sodium chloride
Agent and template, using ammonium molybdate, sodium molybdate, thiocarbamide is dissolved and is freeze-dried in ionized water, and mixture is calcined in tube furnace
Washing removal sodium chloride afterwards, obtains product.The graphene-supported molybdenum disulfide composite material of three-dimensional porous class and preparation method are (open
Number：CN104966812A, on October 7th, 2015, University Of Tianjin), using sodium chloride as dispersing agent and template, by itself and molybdenum
Source, sulphur source and organic carbon source sufficiently dissolve mixing, are freeze-dried and finely ground, obtain mixture；Mixture is put into tube furnace, in
The lower calcining of argon gas protection, obtains calcined product, obtains the graphene-supported molybdenum disulfide composite material of three-dimensional porous class.
The patent of preparation graphite phase carbon nitride has：A kind of method (publication number preparing graphite phase carbon nitride material：CN
106540733A, on March 29th, 2017, Institutes Of Technology Of Taiyuan), it the use of dicyanodiamine and nano silica is presoma, with
The graphitic carbon nitride of high specific surface area is prepared in microwave calcining and Muffle furnace roasting.A kind of conjunction of porous graphite phase carbon nitride
At method (publication number：CN104843658A, on August 19th, 2015, Changzhou University), with polystyrene or poly-methyl methacrylate
Ester microemulsion is hard template, and cyanamide, dicyanodiamine or guanidine hydrochloride are presoma, dry by directly mixing, the gas of inert gas
Porous graphite phase carbon nitride can be obtained in roasting under atmosphere.
Summary of the invention
The object of the present invention is to provide the preparation methods of a kind of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride.
The composite material can be used for photocatalysis field and lithium ion battery negative material field as porous material.Application prospect is wide
It is wealthy, and preparation method process is simple, can be mass-produced.
The present invention is realized by following technological means, and a kind of molybdenum disulfide and graphite phase carbon nitride are compound layer by layer
The three-dimensional network frame of material, which is characterized in that the three-dimensional network frame is that flaky molybdenum disulfide nanometer sheet and graphite-phase nitrogenize
A kind of three-dimensional network frame structure that carbon-coating layer is compound and is built into, network aperture is 10-200nm, with the gross mass of compound
It is calculated for 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 molybdenum disulfide of above structure and graphite phase carbon nitride the three-dimensional network frame of composite material layer by layer,
Characterized by the following steps：
(1) molybdenum disulfide, melamine and cyanuric acid are added in the reaction kettle taken water as a solvent, stir 4 under fixed temperature
Hour, it removes solvent and is dried to obtain presoma.Wherein molybdenum disulfide includes n-BuLi modified molybdenum disulfide, and the presoma is only
It is 1 calculating, the quality of melamine cyanurate with the quality of molybdenum disulfide including molybdenum disulfide and melamine cyanurate
Ratio is 0.05~20.Melamine cyanurate by etc. amount of substance melamine and cyanuric acid in aqueous solution hydrogen bond from group
Dress obtains.The fixed temperature range of reaction is room temperature~100 DEG C, and Optimal Temperature is 80 DEG C.
(2) by presoma made from step (1) be placed in tube furnace, Muffle furnace or other have be passed through gas function can heating furnace
In vivo, protective gas is passed through with certain gas flow rate into furnace body and started to warm up.The gas flow and heating speed being kept fixed
Rate is warming up to fixed temperature, keeps the temperature and calcines 30~200 minutes, it is multiple layer by layer to obtain molybdenum disulfide and graphite phase carbon nitride
The three-dimensional network frame of condensation material.Protective gas is nitrogen (N2), argon gas (Ar) or helium (He).Gas flow be 100~
400ml/min, wherein optimal gas flow is 200ml/min.Heating rate is 1~50 DEG C/min, and optimal heating rate value is situated between
In 10~30 DEG C/min.Fixed temperature is 300~700 DEG C.
The invention has the advantages and positive effects that：Due to taking above-mentioned technical proposal, make melamine and cyanuric acid
Melamine cyanurate is formed in molybdenum disulfide piece interlayer H-bonding self-assembly, achievees the effect that intercalation enters molybdenum disulfide interlayer.
Melamine cyanurate thermal polycondensation graphite phase carbon nitride is made by inert gas shielding and temperature control heating again.Pass through control
The pore size of molybdenum disulfide and melamine cyanurate mass ratio control three-dimensional network frame.This method is low in cost,
Reaction process is simple, and controllability is strong.
Detailed description of the invention
Fig. 1 is the three-dimensional network frame of the composite material layer by layer of molybdenum disulfide and graphite phase carbon nitride made from present example 3
Frame electron scanning micrograph.From this view it is apparent that the material three-dimensional network frame structure.
Specific embodiment
Below by example, the invention will be further described, but embodiment is not intended to limit protection scope of the present invention.It is (each
Raw material is that commercially available analysis is pure)
Embodiment 1
0.517 gram of molybdenum disulfide is weighed, 0.602 gram of melamine, 0.602 gram of cyanuric acid, has been added to 1000ml milliliters
In the reaction kettle of deionized water, 95 DEG C of stirring 3h are warming up to, filter to obtain precursor product, 80 DEG C of vacuum drying 4h.By presoma
It is placed in tube furnace, is passed through gas flow rate and is the argon gas of 500ml/min, and be warming up to the heating rate of 2.3 DEG C/min
550 DEG C of temperature, keep the temperature 1h.It is cooled to room temperature under argon atmosphere protection after reaction, obtains molybdenum disulfide and graphite-phase nitrogen
The three-dimensional network frame for changing carbon-coating layer composite material, measuring product aperture made from the formula is 98nm.
Embodiment 2
0.511 gram of n-BuLi modified molybdenum disulfide is weighed, 1.011 grams of melamine, 1.089 grams of cyanuric acid, is added to
In the reaction kettle for there are 1000 ml deionized waters, 80 DEG C of stirring 4h are warming up to, precursor product is filtered to obtain.Presoma is placed in pipe
In formula furnace, it is passed through the nitrogen gas that gas flow rate is 300ml/min, is warming up to 650 DEG C of temperature with the heating rate of 10 DEG C/min,
Keep the temperature 1h.It is cooled to room temperature under nitrogen atmosphere protection after reaction, it is multiple layer by layer to obtain molybdenum disulfide and graphite phase carbon nitride
The three-dimensional network frame of condensation material, measuring product aperture made from the formula is 10nm.
Embodiment 3
0.501 gram of n-BuLi modified molybdenum disulfide is weighed, 0.595 gram of melamine, 0.612 gram of cyanuric acid, is added to
In the reaction kettle for there are 1000 ml deionized waters, 70 DEG C of stirring 4h are warming up to, precursor product is filtered to obtain.Presoma is placed in pipe
In formula furnace, it is passed through the helium atmosphere that gas flow rate is 100ml/min, is warming up to 650 DEG C of temperature with the heating rate of 50 DEG C/min,
Keep the temperature 1h.It is cooled to room temperature under helium atmosphere protection after reaction, it is multiple layer by layer to obtain molybdenum disulfide and graphite phase carbon nitride
The three-dimensional network frame of condensation material, measuring product aperture made from the formula is 27nm.
Claims (12)
1. the preparation method of a kind of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride, which includes following step
Suddenly：(1) molybdenum disulfide, melamine and cyanuric acid are added in the reaction kettle taken water as a solvent, it is small that 4 is stirred under fixed temperature
When, it removes solvent and is dried to obtain presoma.
2. the preparation method of a kind of molybdenum disulfide according to claim 1 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：The molybdenum disulfide that raw material uses is unmodified molybdenum disulfide or n-BuLi modified molybdenum disulfide.
3. the preparation method of a kind of molybdenum disulfide according to claim 1 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：The presoma includes molybdenum disulfide and melamine cyanurate, is calculated with the quality of molybdenum disulfide for 1, three
The mass ratio of poly cyanamid cyanurate be 0.05~20, wherein melamine cyanurate by etc. amount of substance melamine with
H-bonding self-assembly obtains cyanuric acid in aqueous solution.
4. the preparation method of a kind of molybdenum disulfide according to claim 1 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：The range of fixed temperature is room temperature~100 DEG C in reaction process, and Optimal Temperature is 80 DEG C.
5. the preparation method of a kind of molybdenum disulfide according to claim 1 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：Removing dissolving agent process includes natural drying, suction filtration or rotary evaporation in vacuo.
6. the preparation method of a kind of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride, which includes following step
Suddenly：(2) by presoma made from step (1) be placed in tube furnace, Muffle furnace or other have be passed through gas function can heating furnace
In vivo, protective gas is passed through with certain gas flow rate into furnace body and started to warm up；The gas flow and heating speed being kept fixed
Rate is warming up to fixed temperature, keeps the temperature and calcines a period of time, it is compound layer by layer with graphite phase carbon nitride to obtain molybdenum disulfide
The three-dimensional network frame of material.
7. the preparation method of a kind of molybdenum disulfide according to claim 6 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：Place step (1) presoma furnace body be tube furnace, Muffle furnace or other with controllable heating rate and can
It is passed through the furnace body of gas function.
8. the preparation method of a kind of molybdenum disulfide according to claim 6 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：The protective gas being passed through into furnace body is nitrogen (N2), argon gas (Ar) or helium (He).
9. the preparation method of a kind of molybdenum disulfide according to claim 6 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：The gas flow that protective gas is passed through into furnace body is 100~400ml/min, wherein optimal gas flow is
200ml/min。
10. the preparation method of a kind of molybdenum disulfide according to claim 6 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：Heating rate is 1~50 DEG C/min in temperature-rise period, and optimal heating rate value is between 10~30 DEG C/min.
11. the preparation method of a kind of molybdenum disulfide according to claim 6 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：Furnace body is warming up to fixed temperature, which is 300~700 DEG C.
12. the preparation method of a kind of molybdenum disulfide according to claim 6 and the three-dimensional network frame of graphite phase carbon nitride,
It is characterized in that：Calcination time under fixed temperature is 30~200min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810738052.7A CN108889326B (en) | 2018-07-02 | 2018-07-02 | Preparation method of three-dimensional network frame of molybdenum disulfide and graphite phase carbon nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810738052.7A CN108889326B (en) | 2018-07-02 | 2018-07-02 | Preparation method of three-dimensional network frame of molybdenum disulfide and graphite phase carbon nitride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108889326A true CN108889326A (en) | 2018-11-27 |
| CN108889326B CN108889326B (en) | 2021-01-19 |
Family
ID=64348478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810738052.7A Active CN108889326B (en) | 2018-07-02 | 2018-07-02 | Preparation method of three-dimensional network frame of molybdenum disulfide and graphite phase carbon nitride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108889326B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075901A (en) * | 2019-05-14 | 2019-08-02 | 东南大学 | Porous sulphur mixes the preparation of graphite phase carbon nitride-redox graphene nanometer sheet |
| CN111111700A (en) * | 2020-01-22 | 2020-05-08 | 复旦大学 | Few-layer molybdenum disulfide/nitrogen-doped porous carbon composite catalyst and preparation method thereof |
| WO2023104141A1 (en) * | 2021-12-09 | 2023-06-15 | 桂林理工大学 | N/o co-doped molybdenum sulfide@porous carbon composite electrode material and preparation method therefor, negative electrode material and preparation method therefor, and use thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829860A (en) * | 2015-05-29 | 2015-08-12 | 北京理工大学 | Melamine cyanurate and montmorillonite nano-composite and preparation method thereof |
| CN104891997A (en) * | 2015-05-27 | 2015-09-09 | 青岛大学 | Preparation method of graphite phase carbon nitride/molybdenum sulfide composite material |
| CN104966817A (en) * | 2014-12-01 | 2015-10-07 | 天津大学 | Molybdenum disulfide-carbon three-dimensional porous network composite and preparation method thereof |
| CN106587156A (en) * | 2016-12-07 | 2017-04-26 | 江苏大学 | Method for preparing g-C3N4/MoS2 nanocomposite with vulcanizing sintering method |
| CN106881136A (en) * | 2017-02-23 | 2017-06-23 | 江苏大学 | Metal phase molybdenum bisuphide/two dimension carbonitride catalysis material preparation method |
-
2018
- 2018-07-02 CN CN201810738052.7A patent/CN108889326B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104966817A (en) * | 2014-12-01 | 2015-10-07 | 天津大学 | Molybdenum disulfide-carbon three-dimensional porous network composite and preparation method thereof |
| CN104891997A (en) * | 2015-05-27 | 2015-09-09 | 青岛大学 | Preparation method of graphite phase carbon nitride/molybdenum sulfide composite material |
| CN104829860A (en) * | 2015-05-29 | 2015-08-12 | 北京理工大学 | Melamine cyanurate and montmorillonite nano-composite and preparation method thereof |
| CN106587156A (en) * | 2016-12-07 | 2017-04-26 | 江苏大学 | Method for preparing g-C3N4/MoS2 nanocomposite with vulcanizing sintering method |
| CN106881136A (en) * | 2017-02-23 | 2017-06-23 | 江苏大学 | Metal phase molybdenum bisuphide/two dimension carbonitride catalysis material preparation method |
Non-Patent Citations (2)
| Title |
|---|
| YOUNG-SI JUN ET AL.: "From Melamine-Cyanuric Acid Supramolecular Aggregates to Carbon Nitride Hollow Spheres", 《ADVANCED FUNCTIONAL MATERIALS》 * |
| YOUZHI CAO ET AL.: "Construction of acrossed-layer-structure MoS2/g-C3N4 heterojunction with enhanced photocatalytic performance", 《RSC ADVANCES》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075901A (en) * | 2019-05-14 | 2019-08-02 | 东南大学 | Porous sulphur mixes the preparation of graphite phase carbon nitride-redox graphene nanometer sheet |
| CN110075901B (en) * | 2019-05-14 | 2021-10-19 | 东南大学 | Preparation of porous sulfur-doped graphite phase carbon nitride-reduced graphene oxide nanosheet |
| CN111111700A (en) * | 2020-01-22 | 2020-05-08 | 复旦大学 | Few-layer molybdenum disulfide/nitrogen-doped porous carbon composite catalyst and preparation method thereof |
| 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 |
| WO2023104141A1 (en) * | 2021-12-09 | 2023-06-15 | 桂林理工大学 | N/o co-doped molybdenum sulfide@porous carbon composite electrode material and preparation method therefor, negative electrode material and preparation method therefor, and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108889326B (en) | 2021-01-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107442122B (en) | Cobalt-nitrogen-sulfur co-doped carbon-supported cobalt nanoparticle electrocatalyst and preparation method thereof | |
| Gao et al. | Synthesis, characterization and lithium-storage performance of MoO 2/carbon hybrid nanowires | |
| CN110853937A (en) | Preparation method of nickel-cobalt bimetallic selenide/carbon composite for supercapacitor | |
| CN108993563A (en) | A kind of preparation method of the three-dimensional network frame of montmorillonite and graphite phase carbon nitride | |
| CN102784648B (en) | Catalyst for growing three-dimensional carbon nanotube/grapheme composite material and preparation method of catalyst | |
| CN108889326A (en) | A kind of preparation method of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride | |
| CN102530931A (en) | Graphene-based nano composite material and preparation method thereof | |
| CN104986742A (en) | Bead-chain-like graphitized carbon nitride nano material and preparation method thereof | |
| CN108772092B (en) | Ag3PO4/g-C3N4 composite tubular nano powder and preparation method thereof | |
| CN102698666B (en) | Based on the preparation method of the graphene/nanometer particle composite material of infrared irridiation | |
| CN104401977A (en) | Preparation method of graphene aerogel and graphene-carbon nanotube aerogel | |
| CN109395764B (en) | Preparation method of phosphorus-doped carbon nitride, product and application thereof | |
| CN107876074B (en) | g-C3N4Preparation method of nanoparticle/flower-shaped BiOI composite material | |
| CN112569959A (en) | Preparation method of manganese-modified carbon nanotube-loaded cobalt oxide, product and application thereof | |
| CN102001651A (en) | Method for preparing graphene based on hydroxylamine reduction | |
| CN107808958A (en) | Preparation method of ferroso-ferric oxide/nitrogen-doped graphene composite and products thereof and application | |
| CN105688969A (en) | Preparation method of catalyst for photo-catalytically splitting water to produce hydrogen | |
| CN110416548A (en) | A kind of preparation method and applications of the two-dimensional structure of N doping porous carbon | |
| CN109650358A (en) | A method of quickly graphite phase carbon nitride nanometer rods are prepared without template | |
| CN109622003B (en) | g-C 3 N 4 @g-C 4 N 3 Composite photocatalyst, preparation method and application thereof | |
| Zhou et al. | Design of ap–n heterojunction in 0D/3D MoS 2/gC 3 N 4 composite for boosting the efficient separation of photogenerated carriers with enhanced visible-light-driven H 2 evolution | |
| CN108963215B (en) | N-doped graphene flexible substrate fixed porous MoS with three-dimensional structure2Nano material and preparation method and application thereof | |
| CN105967176B (en) | A kind of preparation method of cellular three-dimensional grapheme | |
| CN105834446A (en) | Synthetic method for ultrathin layered NiO-CoOx nanosheet loading NiCo nano particle composite | |
| CN109225268B (en) | Preparation method of honeycomb porous structure substrate-supported nano material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |