CN107829106A - Preparation method of molybdenum sulfide/nitridation carbon composite and products thereof and application - Google Patents
Preparation method of molybdenum sulfide/nitridation carbon composite and products thereof and application Download PDFInfo
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- CN107829106A CN107829106A CN201711056790.5A CN201711056790A CN107829106A CN 107829106 A CN107829106 A CN 107829106A CN 201711056790 A CN201711056790 A CN 201711056790A CN 107829106 A CN107829106 A CN 107829106A
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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 preparation method of a kind of molybdenum sulfide/nitridation carbon composite and products thereof and application; cyanamide coats the preparation of molybdenum sulfide intermediate; the molybdenum sulfide intermediate that cyanamide coats is placed under the protection of nitrogen and calcined; control calcining heat; calcining 4 hours, last natural cooling can obtain molybdenum sulfide/nitridation carbon composite of 3D structures.This method realizes a kind of preparation of the molybdenum sulfide with heterojunction structure/nitridation carbon composite using the mode of growth in situ and calcining, and resulting molybdenum sulfide is the dendritic dimensional structures 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 new molybdenum sulfide/nitridation carbon composite, it is able to ensure that electronics fast transferring between interface, therefore prepared composite 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 field, and in particular to a kind of molybdenum sulfide/carbonitride composite wood
Preparation method of material and products thereof and application.
Background technology
Hydrogen Energy is considered as the efficient substitute of 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 catalyst of catalyzing manufacturing of hydrogen best results, it is used for hydrogen production reaction coated on electrode surface extensively by people.However, noble metal
Pt fancy prices and the rare of resource seriously hinder its large-scale industrialization application.Therefore, it is cheap to seek 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 new non-precious metal catalyst and urged
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 turn into the study hotspot of electro-catalysis hydrogen preparation field.
Recent document and theoretical study results show, MoS2Electro-catalysis hydrogen production activity and its two-dimensional layered structure edge
Active site it is relevant, design the two-dimentional MoS of nanostructured2Thin 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,
Molybdenum sulfide and the interface resistance of azotized carbon nano structure can be substantially reduced, significantly improves electro-catalysis hydrogen production reaction efficiency, on the one hand
MoS in carbon nitride material2Nanometer sheet surface can form many small crackles, be effectively increased the edge catalytic active site of material
Point；The pore structure of another aspect carbonitride can guarantee that electronics in MoS2The high efficiency of transmission between carbon base body, make catalysate hydrogen
Gas is easy to diffuse out from electrode.
The preparation method of molybdenum disulfide/nitridation carbon composite mainly includes in situ hybridization, Physical etc. at present.Ge
Et al. prepare molybdenum disulfide and carbon nitride material respectively（J. Hydrogen. Energy 2013, 38, 6960）, Ran Houjin
Row is baking mixed, so as to obtain molybdenum disulfide/nitridation carbon composite；Li et al. is then by the molybdenum disulfide prepared and carbonitride
Material is put to be mixed in ethanol（Langmuir, 2014, 30, 8965）, molybdenum disulfide/nitrogen is prepared by sonochemical method
Change carbon composite；Patent of invention CN201510278920.4 was once reported MoS2It is well mixed, grinds with nitrogen source precursor material
Calcining finally gives molybdenum disulfide/nitridation carbon composite after mill.Above-mentioned method is prepared using two-step method or multistep processes more,
Synthetic method is relatively complicated, and process is cumbersome, and time-consuming, low yield, and composite does not have certain 3D structure structures
Type.
It is necessary to develop controllable and reproducible method at this stage, to prepare molybdenum disulfide/nitridation carbon composite；Together
When the composite prepared can keep good nanometer configuration.It is multiple that the present invention proposes a kind of new molybdenum sulfide/carbonitride
The preparation method of condensation material, the material molybdenum sulfide with 3D dendritic structures is prepared, 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.
The content of the invention
For overcome the deficiencies in the prior art, present invention aims at：It is proposed a kind of system of molybdenum sulfide/nitridation carbon composite
Preparation Method.
Another object of the present invention is：It is proposed product prepared by a kind of above method.
A further object of the present invention is：The application of the said goods is provided.
This method.Heterojunction structure can be produced between the molybdenum sulfide and carbonitride of the composite, unique structure can be true
Fast transferring of the electronics between interface is protected, therefore prepared composite shows excellent electro-catalysis H2-producing capacity.
Purpose of the present invention problem is achieved through the following technical solutions：
A kind of preparation method of molybdenum sulfide/nitridation carbon composite, using cellulosic material as substrate, certain cyanamide is added,
Using sulphur ammonium molybdate as sulphur source and molybdenum source, using 1- imidazoles -4- formic acid as ligand framework, among solvent-thermal process molybdenum sulfide
Body material, then calcining obtain molybdenum sulfide/nitridation carbon composite of 3D dendritic structures, comprised the following steps：
A, the preparation of cyanamide cladding molybdenum sulfide intermediate：Weigh a certain amount of 1- imidazoles -4- formic acid to be dissolved in acetonitrile solution, formed
Homogeneous ligand solution；Sulphur ammonium molybdate is dissolved in dimethylformamide according to a certain percentage, is slowly added into ligand solution body
In system, sulphur ammonium molybdate is substantially dissolved in ligand solution by stirring, while add cellulose, and add a certain amount of cyanamide
Coated；Above-mentioned mixed liquor is sealed in ptfe autoclave, by the hydro-thermal of certain time, washing, drying
Processing, 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 calcined, control calcining heat, calcining 4 hours, most
Natural cooling can obtain molybdenum sulfide/nitridation carbon composite of 3D structures afterwards.
Cellulose used is bacteria cellulose in the preparation process of described cyanamide cladding molybdenum sulfide intermediate, hemicellulose
Element, lignin or pectin, cyanamide are cyanamide, dicyandiamide, one kind in melamine or cyanuric acid.
With cellulose and cyanamide be raw material in the preparation process of described cyanamide cladding molybdenum sulfide intermediate, by cellulose and
Cyanamide in mass ratio 10:1~1:10 mixing.
Described sulphur ammonium molybdate solution concentration is between 0.1 ~ 10 mol/L.
Described 1- imidazoles -4- formic acid solutions concentration is between 0.1 ~ 1 mol/L.
The solvent of described solvent thermal reaction is non-polar solven, selected from ethanol, ethylene glycol, and acetonitrile, dimethylformamide,
Toluene or chloroform.
The reaction time of preferable solvent thermal reaction is 1-72 hours, and the reaction temperature of solvent thermal reaction is 100~200oC。
Preferable calcining heat is 800 ~ 1200oC。
The present invention provides a kind of molybdenum sulfide/nitridation carbon composite, it is characterised in that according to any of the above-described methods described system
It is standby to obtain.
The present invention also provides a kind of molybdenum sulfide/nitridation carbon composite answering as water electrolysis hydrogen production catalytic electrode material
With.
The present invention relates to a kind of preparation method and molybdenum sulfide/nitrogen of 3D dendritic structures molybdenum sulfide/nitridation carbon composite
Change carbon composite.Cellulosic material will be tieed up 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/nitridation of heterojunction structure as ligand framework by the method for solvent heat and calcination processing
Carbon composite；Dendroid pattern is presented in the molybdenum sulfide of 3D structures, is mostly 5 ~ 7 Rotating fields, can be effective with carbon nitride material
With reference to being a kind of efficient water electrolysis hydrogen production catalytic electrode material.
Brief description of the drawings
Fig. 1 is the TEM figures for molybdenum sulfide/nitridation carbon composite that the embodiment of the present invention 1 synthesizes.
Fig. 2 is the high-resolution TEM figures for molybdenum sulfide/nitridation carbon composite that the embodiment of the present invention 1 synthesizes.
Embodiment
The present embodiment is implemented under premised on technical solution 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：
0.2 gram of 1- imidazoles -4- formic acid is weighed first to be dissolved in acetonitrile solution, forms 0.1 mol/L homogeneous ligand solution；Claim
Take 0.1 gram of sulphur ammonium molybdate to be dissolved in dimethylformamide, form 0.1 mol/L uniform solution, it is then that sulphur ammonium molybdate is molten
Liquid is slowly added into 1- imidazoles -4- formic acid solutions, is allowed to fully dissolve by stirring；The bacterial fibers of 0.1 gram of addition simultaneously
Element, and the urea for weighing 1.0 grams carries out cladding processing；Above-mentioned mixed liquor is sealed in ptfe autoclave, 170oSolvent thermal reaction 48 hours at a temperature of C, are then washed, drying process, obtain solid powder.The cyanamide of gained is coated
Molybdenum sulfide intermediary material be placed in tube furnace, nitrogen protection under with 3oC/min heating rate is raised to 800oC, 800oKept for 4 hours at a temperature of C, Temperature fall, you can to obtain the molybdenum sulfide of 3D structures/nitridation carbon composite.Fig. 1 is to be closed
Into molybdenum sulfide/carbonitride composite material transmission electron microscope picture, from figure, it can be seen that it has the dendritic structures of 3D,
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 spectrograms
Further illustrate that the material molybdenum sulfide of 3D dendritic structures is made up of 5 ~ 7 synusia layer materials, carbon nitride material is as substrate, vulcanization
Molybdenum is then covered in the surface of carbonitride, forms special heterojunction structure.
Embodiment 2：
0.2 gram of 1- imidazoles -4- formic acid is weighed first to be dissolved in acetonitrile solution, forms 0.1 mol/L homogeneous ligand solution；Claim
Take 1.0 grams of sulphur ammonium molybdate to be dissolved in dimethylformamide, form 1.0 mol/L uniform solution, it is then that sulphur ammonium molybdate is molten
Liquid is slowly added into 1- imidazoles -4- formic acid solutions, is allowed to fully dissolve by stirring；Add 0.1 gram thin in proportion simultaneously
Fungin and 0.1 gram of cyanamide；Above-mentioned mixed liquor is sealed in ptfe autoclave, 170oAt a temperature of C
Solvent thermal reaction 48 hours, is then washed, drying process, obtains solid powder.The molybdenum sulfide that the cyanamide of gained is coated
Intermediary material is placed in tube furnace, with 3 under nitrogen protectionoC/min heating rate is raised to 800oC, 800oAt a temperature of C
Kept for 4 hours, Temperature fall, you can to obtain the molybdenum sulfide of 3D structures/nitridation carbon composite.
Embodiment 3：
0.2 gram of 1- imidazoles -4- formic acid is weighed first to be dissolved in acetonitrile solution, forms 1.0 mol/L homogeneous ligand solution；Claim
Take 1.0 grams of sulphur ammonium molybdate to be dissolved in dimethylformamide, form 1.0 mol/L uniform solution, it is then that sulphur ammonium molybdate is molten
Liquid is slowly added into 1- imidazoles -4- formic acid solutions, is allowed to fully dissolve by stirring；Add 0.1 gram thin in proportion simultaneously
Fungin and 1.0 grams of dicyandiamide；Above-mentioned mixed liquor is sealed in ptfe autoclave, 170oAt a temperature of C
Solvent thermal reaction 48 hours, is then washed, drying process, obtains solid powder.The molybdenum sulfide that the cyanamide of gained is coated
Intermediary material is placed in tube furnace, with 3 under nitrogen protectionoC/min heating rate is raised to 800oC, 800oAt a temperature of C
Kept for 4 hours, Temperature fall, you can to obtain the molybdenum sulfide of 3D structures/nitridation carbon composite.
Embodiment 4：
0.2 gram of 1- imidazoles -4- formic acid is weighed first to be dissolved in acetonitrile solution, forms 0.1 mol/L homogeneous ligand solution；Claim
Take 0.1 gram of sulphur ammonium molybdate to be dissolved in dimethylformamide, form 0.1 mol/L uniform solution, it is then that sulphur ammonium molybdate is molten
Liquid is slowly added into 1- imidazoles -4- formic acid solutions, is allowed to fully dissolve by stirring；Ratio adds 0.1 gram of bacterium simultaneously
Cellulose and 1.0 grams of dicyandiamide；Above-mentioned mixed liquor is sealed in ptfe autoclave, 190oIt is molten at a temperature of C
Agent thermal response 24 hours, is then washed, drying process, obtains solid powder.In the molybdenum sulfide that the cyanamide of gained is coated
Mesosome material is placed in tube furnace, 900oC temperature lower calcinations 4 hours, Temperature fall, you can to obtain the vulcanization of 3D structures
Molybdenum/nitridation carbon composite.
Claims (10)
1. the preparation method of a kind of molybdenum sulfide/nitridation carbon composite, it is characterised 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, pass through solvent-thermal process sulphur
Change molybdenum intermediary material, then calcining obtains molybdenum sulfide/nitridation carbon composite of 3D dendritic structures, comprises the following steps：
A, the preparation of cyanamide cladding molybdenum sulfide intermediate：Weigh a certain amount of 1- imidazoles -4- formic acid to be dissolved in acetonitrile solution, formed
Homogeneous ligand solution；Sulphur ammonium molybdate is dissolved in dimethylformamide according to a certain percentage, is slowly added into ligand solution body
In system, sulphur ammonium molybdate is substantially dissolved in ligand solution by stirring, while add cellulose, and add a certain amount of cyanamide
Coated；Above-mentioned mixed liquor is sealed in ptfe autoclave, by the hydro-thermal of certain time, washing, drying
Processing, obtains solid powder, and 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 calcined, calcined 4 hours, last natural cooling
To obtain the molybdenum sulfide of 3D structures/nitridation carbon composite.
2. the preparation method of molybdenum sulfide/nitridation carbon composite according to claim 1, it is characterised in that described cyanamide bag
It is bacteria cellulose, hemicellulose, lignin or pectin to cover cellulose used in the preparation process of molybdenum sulfide intermediate；Cyanamide
For cyanamide, dicyandiamide, one kind in melamine or cyanuric acid.
3. the preparation method of molybdenum sulfide according to claim 1 or claim 2/nitridation carbon composite, it is characterised in that described cyanogen
With cellulose and cyanamide it is raw material in the preparation process of amine cladding molybdenum sulfide intermediate, by cellulose and cyanamide in mass ratio 10:
1~1:10 mixing.
4. the preparation method of molybdenum sulfide/nitridation carbon composite according to claim 1, it is characterised in that described sulphur molybdic acid
Ammonium salt solution concentration is between 0.1 ~ 10 mol/L.
5. the preparation method of molybdenum sulfide/nitridation carbon composite according to claim 1, it is characterised in that described 1- miaows
Azoles -4- formic acid solutions concentration is between 0.1 ~ 1 mol/L.
6. the preparation method of molybdenum sulfide/nitridation carbon composite according to claim 1, it is characterised in that described solvent heat
The solvent of reaction is non-polar solven, selected from ethanol, ethylene glycol, acetonitrile, dimethylformamide, toluene or chloroform.
7. the preparation method of molybdenum sulfide/nitridation carbon composite according to claim 1, it is characterised in that preferable solvent heat
The reaction time of reaction is 1-72 hours, and the reaction temperature of solvent thermal reaction is 100~200oC。
8. the preparation method of molybdenum sulfide/nitridation carbon composite according to claim 1, it is characterised in that preferable calcining temperature
Spend for 800 ~ 1200oC。
9. a kind of molybdenum sulfide/nitridation carbon composite, it is characterised in that be prepared into according to any methods describeds of claim 1-8
Arrive.
10. molybdenum sulfide/nitridation carbon composite answering as water electrolysis hydrogen production catalytic electrode material according to claim 9
With.
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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 |
| 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 |
| CN110697794A (en) * | 2019-11-01 | 2020-01-17 | 宁波大学 | Cobalt sulfide/g-C with two-dimensional hollow nanosheet structure3N4Composite electrode material and preparation method thereof |
| CN111286752A (en) * | 2018-12-10 | 2020-06-16 | 南京理工大学 | Nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and preparation method thereof |
| CN111905767A (en) * | 2020-07-29 | 2020-11-10 | 华南农业大学 | Nano pompon-shaped molybdenum sulfide/wood-based carbon porous electrode material and preparation method and application thereof |
| CN112642462A (en) * | 2020-12-30 | 2021-04-13 | 山东科技大学 | Molybdenum trisulfide rhenium nanosheet/graphite phase carbon nitride nanotube heterostructure photocatalyst and preparation method thereof |
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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 |
| CN111286752A (en) * | 2018-12-10 | 2020-06-16 | 南京理工大学 | Nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material 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 |
| CN110697794A (en) * | 2019-11-01 | 2020-01-17 | 宁波大学 | Cobalt sulfide/g-C with two-dimensional hollow nanosheet structure3N4Composite electrode material and preparation method 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 |
| CN111905767A (en) * | 2020-07-29 | 2020-11-10 | 华南农业大学 | Nano pompon-shaped molybdenum sulfide/wood-based carbon porous electrode material and preparation method and application 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 |
| CN112642462A (en) * | 2020-12-30 | 2021-04-13 | 山东科技大学 | Molybdenum trisulfide rhenium nanosheet/graphite phase carbon nitride nanotube heterostructure photocatalyst and preparation method thereof |
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