CN107829106B - Molybdenum sulfide/nitridation carbon composite preparation method and products thereof and application - Google Patents
Molybdenum sulfide/nitridation carbon composite preparation method and products thereof and application Download PDFInfo
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- CN107829106B CN107829106B CN201711056790.5A CN201711056790A CN107829106B CN 107829106 B CN107829106 B CN 107829106B CN 201711056790 A CN201711056790 A CN 201711056790A CN 107829106 B CN107829106 B CN 107829106B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a kind of molybdenum sulfide/nitridation carbon composite preparation methods and products thereof and application; the preparation of cyanamide cladding molybdenum sulfide intermediate; the molybdenum sulfide intermediate that cyanamide coats is placed under the protection of nitrogen and is calcined; control calcination temperature; calcining 4 hours, last natural cooling can obtain molybdenum sulfide/nitridation carbon composite of 3D structure.This method realizes a kind of preparation of the molybdenum sulfide with heterojunction structure/nitridation carbon composite in the way of growth in situ and calcining, and obtained molybdenum sulfide is the dendritic dimensional structure of 3D, is wrapped in the inside of carbon nitride material.Due to the presence of heterojunction structure between molybdenum sulfide and carbonitride in this novel molybdenum sulfide/nitridation carbon composite, it can ensure electronics fast transferring between interface, therefore prepared composite material shows excellent electro-catalysis H2-producing capacity, there is very big application potential in terms of water electrolysis hydrogen production field.
Description
Technical field
The invention belongs to inorganic nano nonmetallic materials preparation fields, and in particular to a kind of molybdenum sulfide/carbonitride composite wood
Preparation method of material and products thereof and application.
Background technique
Hydrogen Energy is considered as the efficient substitute of the following traditional fossil energy.In numerous Hydrogen Energy production ways, electricity is urged
Change the hydrogen gas production mode that hydrogen production reaction is a kind of efficient green.So far, precious metals pt base catalyst is considered as electricity
The optimal catalyst of catalyzing manufacturing of hydrogen effect is coated on electrode surface for hydrogen production reaction extensively by people.However, noble metal
Pt fancy price and the rare of resource seriously hinder its large-scale industrialization application.Therefore, seek low in cost, property
The catalyst for preparing hydrogen electrode of energy high-efficient and lasting is the key that hydrogen energy source utilizes, and also complies with 21st century green energy resource and sustainable development
The requirement of exhibition.In recent years, transient metal sulfide shows efficient electricity as a kind of novel non-precious metal catalyst and urges
Change hydrogen production efficiency.In numerous transient metal sulfides, platelike molybdenumdisulfide (MoS2) two dimensional crystal material is due to its abundance
Height, the advantages such as price is low become the research hotspot of electro-catalysis hydrogen preparation field.
Recent document and theoretical study results shows MoS2Electro-catalysis hydrogen production activity and its two-dimensional layered structure edge
Active site it is related, design the two-dimentional MoS of nanostructure2Thin layer simultaneously maximumlly exposes its edge catalytic active site
Point quantity is to improve the effective way of its electro-catalysis hydrogen production activity.By two-dimentional MoS2Thin layer is effectively compound in carbon nitride material,
It can be substantially reduced the interface resistance of molybdenum sulfide Yu azotized carbon nano structure, significantly improve electro-catalysis hydrogen production reaction efficiency, on the one hand
MoS in carbon nitride material2Nanometer sheet surface will form many small crackles, effectively increase the edge catalytic active site of material
Point；The pore structure of another aspect carbonitride can guarantee electronics in MoS2The high efficiency of transmission between carbon base body makes catalysate hydrogen
Gas is easy to diffuse out from electrode.
Molybdenum disulfide/nitridation carbon composite preparation method mainly includes in situ hybridization, physical method etc. at present.Ge
Et al. prepare molybdenum disulfide and carbon nitride material (J. Hydrogen. Energy 2013,38,6960) respectively, then into
Row is baking mixed, to obtain molybdenum disulfide/nitridation carbon composite；Li et al. people is then by the molybdenum disulfide prepared and carbonitride
Material puts mixing (Langmuir, 2014,30,8965) in ethanol, prepares molybdenum disulfide/nitrogen by sonochemical method
Change carbon composite；Patent of invention CN201510278920.4 was once reported MoS2It is uniformly mixed, grinds with nitrogen source precursor material
Calcining finally obtains molybdenum disulfide/nitridation carbon composite after mill.Above-mentioned method mostly uses two-step method or multistep processes to prepare,
Synthetic method is relatively complicated, and process is cumbersome, and time-consuming, low yield, and composite material does not have certain 3D structure structure
Type.
At this stage it is necessary to develop controllable and reproducible method, to prepare molybdenum disulfide/nitridation carbon composite；Together
When the composite material prepared be able to maintain good nanometer configuration.The invention proposes a kind of new molybdenum sulfide/carbonitride is multiple
The preparation method of condensation material prepares the material molybdenum sulfide with 3D dendritic structure, and can be effective with nitridation carbon substrate
It is compound, specific heterojunction structure is formd, is had broad application prospects in electro-catalysis hydrogen preparation field.
Summary of the invention
In order to overcome the deficiencies of the prior art, present invention aims at: propose a kind of system of molybdenum sulfide/nitridation carbon composite
Preparation Method.
Another object of the present invention is: proposing a kind of product of above method preparation.
Another object of the present invention is to: the application of the said goods is provided.
Heterojunction structure can be generated between the molybdenum sulfide and carbonitride of the composite material, unique structure can ensure electricity
Fast transferring of the son between interface, therefore prepared composite material shows excellent electro-catalysis H2-producing capacity.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of molybdenum sulfide/nitridation carbon composite adds certain cyanogen using cellulosic material as substrate
Amine, using 1- imidazoles -4- formic acid as ligand framework, passes through solvent-thermal process molybdenum sulfide using sulphur ammonium molybdate as sulphur source and molybdenum source
Intermediary material, then calcining obtains molybdenum sulfide/nitridation carbon composite of 3D dendritic structure, includes the following steps:
A, the preparation of cyanamide cladding molybdenum sulfide intermediate: weighing a certain amount of 1- imidazoles -4- formic acid and be dissolved in acetonitrile solution,
Form uniform ligand solution；Sulphur ammonium molybdate is dissolved in dimethylformamide according to a certain percentage, it is molten to be slowly added into ligand
In liquid system, it is substantially dissolved in sulphur ammonium molybdate in ligand solution by stirring, while adding cellulose, and add a certain amount of
Cyanamide is coated；Above-mentioned mixed liquor is sealed in ptfe autoclave, by the hydro-thermal of certain time, washing,
It is dried, obtains solid powder.Hydrothermal temperature control is 170 ~ 200oC, hydro-thermal time are 24 ~ 48 hours；
B, the molybdenum sulfide intermediate that cyanamide coats is placed under the protection of nitrogen and is calcined, control calcination temperature, calcining 4 is small
When, last natural cooling can obtain molybdenum sulfide/nitridation carbon composite of 3D structure.
Cellulose used in the preparation process of the cyanamide cladding molybdenum sulfide intermediate is bacteria cellulose, hemicellulose
Element, lignin or pectin, cyanamide are cyanamide, dicyandiamide, one of melamine or cyanuric acid.
With cellulose and cyanamide be raw material in the preparation process of the described cyanamide cladding molybdenum sulfide intermediate, by cellulose and
Cyanamide 10: 1~1:10 in mass ratio mixing.
The sulphur ammonium molybdate solution concentration is between 0.1 ~ 10 mol/L.
1- imidazoles -4- formic acid solution the concentration is between 0.1 ~ 1 mol/L.
The solvent of the solvent thermal reaction be nonpolar solvent, be selected from ethyl alcohol, ethylene glycol, acetonitrile, dimethylformamide,
Toluene or chloroform.
The reaction time of preferred solvent thermal reaction is 1-72 hours, and the reaction temperature of solvent thermal reaction is 100~200
℃。
Preferred calcination temperature is 800 ~ 1200 DEG C.
The present invention provides a kind of molybdenum sulfide/nitridation carbon composite, it is characterised in that according to any of the above-described the method system
It is standby to obtain.
The present invention also provides a kind of molybdenum sulfide/nitridation carbon composites to answer as water electrolysis hydrogen production catalytic electrode material
With.
The present invention relates to the preparation methods and molybdenum sulfide/nitrogen of a kind of 3D dendritic structure molybdenum sulfide/nitridation carbon composite
Change carbon composite.Using cellulosic material as carbon substrate, cyanamide is as nitrogen source, using sulphur ammonium molybdate as sulphur source and molybdenum source, with
1- imidazoles -4- formic acid obtains molybdenum sulfide/nitrogen of heterojunction structure as ligand framework, by the method for solvent heat and calcination processing
Change carbon composite；Dendroid pattern is presented in the molybdenum sulfide of 3D structure, is mostly 5 ~ 7 layers of structure, can have with carbon nitride material
Effect combines, and is a kind of efficient water electrolysis hydrogen production catalytic electrode material.
Detailed description of the invention
Fig. 1 is molybdenum sulfide/nitridation carbon composite TEM figure that the embodiment of the present invention 1 synthesizes；
Fig. 2 is molybdenum sulfide/nitridation carbon composite high-resolution TEM figure that the embodiment of the present invention 1 synthesizes.
Specific embodiment
The present embodiment is implemented under the premise of the technical scheme of the present invention, gives detailed embodiment and specific
Operating process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1:
It weighs 0.2 gram of 1- imidazoles -4- formic acid first to be dissolved in acetonitrile solution, the uniform ligand for forming 0.1 mol/L is molten
Liquid；It weighs 0.1 gram of sulphur ammonium molybdate to be dissolved in dimethylformamide, the uniform solution of 0.1 mol/L is formed, then by sulphur molybdic acid
Ammonium salt solution is slowly added into 1- imidazoles -4- formic acid solution, is allowed to sufficiently dissolve by stirring；The bacterium of 0.1 gram of addition simultaneously
Cellulose, and the urea for weighing 1.0 grams carries out cladding processing；Above-mentioned mixed liquor is sealed in ptfe autoclave,
Solvent thermal reaction 48 hours, is then washed, is dried, obtain solid powder at a temperature of 170 DEG C.By resulting cyanamide
The molybdenum sulfide intermediary material of cladding is placed in tube furnace, is raised to 800 DEG C under nitrogen protection with the heating rate of 3 DEG C/min, In
It is kept for 4 hours at a temperature of 800 DEG C, Temperature fall, it can obtain molybdenum sulfide/nitridation carbon composite of 3D structure.Fig. 1 is institute
The molybdenum sulfide of synthesis/carbonitride composite material material transmission electron microscope picture, from figure, it can be seen that it has the dendritic knot of 3D
Structure, mean size is between 10 ~ 25 nm；Molybdenum sulfide is coated in one layer of soft carbon nitride material.Fig. 2 high resolution electron microscopy spectrum
Figure further illustrates that the material molybdenum sulfide of 3D dendritic structure is made of 5 ~ 7 synusia layer materials, and carbon nitride material is as substrate, sulphur
Change the surface that molybdenum is then covered on carbonitride, forms special heterojunction structure.
Embodiment 2:
It weighs 0.2 gram of 1- imidazoles -4- formic acid first to be dissolved in acetonitrile solution, the uniform ligand for forming 0.1 mol/L is molten
Liquid；It weighs 1.0 grams of sulphur ammonium molybdate to be dissolved in dimethylformamide, the uniform solution of 1.0 mol/L is formed, then by sulphur molybdic acid
Ammonium salt solution is slowly added into 1- imidazoles -4- formic acid solution, is allowed to sufficiently dissolve by stirring；Add 0.1 gram in proportion simultaneously
Bacteria cellulose and 0.1 gram of cyanamide；Above-mentioned mixed liquor is sealed in ptfe autoclave, in 170 DEG C of temperature
Solvent thermal reaction 48 hours, is then washed, is dried, obtain solid powder under spending.The sulphur that resulting cyanamide is coated
Change molybdenum intermediary material to be placed in tube furnace, 800 DEG C is raised under nitrogen protection with the heating rate of 3 DEG C/min, in 800 DEG C of temperature
It is lower to be kept for 4 hours, Temperature fall, it can obtain molybdenum sulfide/nitridation carbon composite of 3D structure.
Embodiment 3:
It weighs 0.2 gram of 1- imidazoles -4- formic acid first to be dissolved in acetonitrile solution, the uniform ligand for forming 1.0 mol/L is molten
Liquid；It weighs 1.0 grams of sulphur ammonium molybdate to be dissolved in dimethylformamide, the uniform solution of 1.0 mol/L is formed, then by sulphur molybdic acid
Ammonium salt solution is slowly added into 1- imidazoles -4- formic acid solution, is allowed to sufficiently dissolve by stirring；Add 0.1 gram in proportion simultaneously
Bacteria cellulose and 1.0 grams of dicyandiamide；Above-mentioned mixed liquor is sealed in ptfe autoclave, in 170 DEG C of temperature
Solvent thermal reaction 48 hours, is then washed, is dried, obtain solid powder under spending.The sulphur that resulting cyanamide is coated
Change molybdenum intermediary material to be placed in tube furnace, 800 DEG C is raised under nitrogen protection with the heating rate of 3 DEG C/min, in 800 DEG C of temperature
It is lower to be kept for 4 hours, Temperature fall, it can obtain molybdenum sulfide/nitridation carbon composite of 3D structure.
Embodiment 4:
It weighs 0.2 gram of 1- imidazoles -4- formic acid first to be dissolved in acetonitrile solution, the uniform ligand for forming 0.1 mol/L is molten
Liquid；It weighs 0.1 gram of sulphur ammonium molybdate to be dissolved in dimethylformamide, the uniform solution of 0.1 mol/L is formed, then by sulphur molybdic acid
Ammonium salt solution is slowly added into 1- imidazoles -4- formic acid solution, is allowed to sufficiently dissolve by stirring；Ratio adds 0.1 gram simultaneously
Bacteria cellulose and 1.0 grams of dicyandiamide；Above-mentioned mixed liquor is sealed in ptfe autoclave, in 190 DEG C of temperature
Lower solvent thermal reaction 24 hours, is then washed, is dried, obtain solid powder.The vulcanization that resulting cyanamide is coated
Molybdenum intermediary material is placed in tube furnace, 900 DEG C temperature lower calcination 4 hours, Temperature fall, it can obtain the sulphur of 3D structure
Change molybdenum/nitridation carbon composite.
Claims (6)
1. a kind of molybdenum sulfide/nitridation carbon composite preparation method, which is characterized in that using cellulosic material as substrate, add
Add cyanamide, using sulphur ammonium molybdate as sulphur source and molybdenum source, using 1- imidazoles -4- formic acid as ligand framework, passes through solvent-thermal process sulphur
Change molybdenum intermediary material, then calcining obtains molybdenum sulfide/nitridation carbon composite of 3D dendritic structure, includes the following steps:
A, it the preparation of cyanamide cladding molybdenum sulfide intermediate: weighs a certain amount of 1- imidazoles -4- formic acid and is dissolved in acetonitrile solution, formed
Uniform ligand solution；Sulphur ammonium molybdate is dissolved in dimethylformamide according to a certain percentage, is slowly added into ligand solution body
In system, it is substantially dissolved in sulphur ammonium molybdate in ligand solution by stirring, while adding cellulose, and add a certain amount of cyanamide
It is coated；Above-mentioned mixed liquor is sealed in ptfe autoclave, by the solvent thermal reaction of certain time, then
It washed, be dried, obtain solid powder, the control of solvent heat temperature is 170 ~ 200 DEG C, the solvent heat time is 24 ~
48 hours；
B, the molybdenum sulfide intermediate that cyanamide coats is placed under the protection of nitrogen and is calcined, calcined 4 hours, last natural cooling
To obtain molybdenum sulfide/nitridation carbon composite of 3D structure.
2. molybdenum sulfide/nitridation carbon composite preparation method according to claim 1, it is characterised in that the cyanamide packet
Covering cellulose used in the preparation process of molybdenum sulfide intermediate is bacteria cellulose.
3. molybdenum sulfide according to claim 1 or claim 2/nitridation carbon composite preparation method, it is characterised in that the cyanogen
It with cellulose and cyanamide is raw material that amine, which coats in the preparation process of molybdenum sulfide intermediate, by cellulose and cyanamide in mass ratio 10:
1~1:10 mixing.
4. molybdenum sulfide/nitridation carbon composite preparation method according to claim 1, it is characterised in that the sulphur molybdic acid
Ammonium salt solution concentration is between 0.1 ~ 10 mol/L.
5. molybdenum sulfide/nitridation carbon composite preparation method according to claim 1, it is characterised in that the 1- miaow
Azoles -4- formic acid solution concentration is between 0.1 ~ 1 mol/L.
6. molybdenum sulfide/nitridation carbon composite preparation method according to claim 1, it is characterised in that preferred calcining temperature
Degree is 800 ~ 1200 DEG C.
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| CN109225296A (en) * | 2018-08-31 | 2019-01-18 | 中国环境科学研究院 | A kind of visible light-responded photochemical catalyst and preparation method thereof |
| CN111286752B (en) * | 2018-12-10 | 2021-11-09 | 南京理工大学 | Nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and preparation method thereof |
| CN109876869A (en) * | 2019-01-26 | 2019-06-14 | 南开大学 | Titanium diboride surface cladding functional film material of core-shell structure and the preparation method and application thereof |
| CN110697794B (en) * | 2019-11-01 | 2022-04-01 | 宁波大学 | Cobalt sulfide/g-C with two-dimensional hollow nanosheet structure3N4Composite electrode material and preparation method thereof |
| CN111905767B (en) * | 2020-07-29 | 2021-11-26 | 华南农业大学 | Nano pompon-shaped molybdenum sulfide/wood-based carbon porous electrode material and preparation method and application thereof |
| CN112642462B (en) * | 2020-12-30 | 2022-10-18 | 山东科技大学 | Molybdenum-rhenium trisulfide nanosheet/graphite-phase carbon nitride nanotube heterostructure photocatalyst and preparation method thereof |
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