CN107381515A - A kind of preparation method and product of vanadium nitride elctro-catalyst - Google Patents
A kind of preparation method and product of vanadium nitride elctro-catalyst Download PDFInfo
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- CN107381515A CN107381515A CN201710669800.6A CN201710669800A CN107381515A CN 107381515 A CN107381515 A CN 107381515A CN 201710669800 A CN201710669800 A CN 201710669800A CN 107381515 A CN107381515 A CN 107381515A
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- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000003054 catalyst Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 11
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000013049 sediment Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000000376 reactant Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract 3
- 235000021110 pickles Nutrition 0.000 claims abstract 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000004570 mortar (masonry) Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000000643 oven drying Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 description 7
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 7
- 229910052573 porcelain Inorganic materials 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0617—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
-
- 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
-
- B01J35/33—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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
-
- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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 preparation method and product of vanadium nitride elctro-catalyst, comprise the following steps：1）Urea, ammonium metavanadate, cabaltous nitrate hexahydrate are sufficiently mixed according to formula rate, are fully ground, obtains reactant feed；2）Reactant feed prepared by the step 1 pyroreaction under atmosphere protection, 700 900 DEG C of reaction temperature, the 5h of reaction time 2, the powder obtained after cooling go the removal of impurity with pickle, wash lower sediment, drying precipitated, are fully ground, obtain vanadium nitride elctro-catalyst.Vanadium nitride elctro-catalyst prepared by the present invention, it is high to have the characteristics that technical process is simple, reaction time is short, materials chemistry forms homogeneous, the uniform electro catalytic activity of appearance and size, stability.
Description
Technical field
The present invention relates to vanadium nitride nano powder body preparing technical field, and in particular to a kind of preparation of vanadium nitride elctro-catalyst
Method and product.
Background technology
With the rapid growth of global economy, energy problem and problem of environmental pollution deeply annoying human lives, people
It is badly in need of finding cleaning sustainable energy to solve this two large problems, and Hydrogen Energy is as green sustainable energy of new generation, people
It is placed high hopes.Water-splitting technology is to realize one of sustainable effective way for preparing hydrogen, and the key problem of the technology is
Develop efficient, cheap water-splitting catalyst.At present, noble metal-based catalysts（Such as Pt, Ru or Ir oxide）It is catalysis
The best water-splitting catalyst of performance, still, it is expensive, reserves are low the shortcomings that significantly limit the extensive of such catalyst
Using therefore, it is current study hotspot to develop the High-efficient Water catalyst for cracking being made up of the cheap element of earth's crust rich content.
Vanadium nitride（VN）With higher mechanical strength, electron conductivity is corrosion-resistant, and stability is high, in physics, chemistry, Material Field
Have a wide range of applications, be very promising electrocatalysis material, and vanadium nitride yet there are no report in electro-catalysis field using the country
Lead, therefore prepare nano vanadium nitride powder-body and have great importance applied to electro-catalysis field.
A kind of Application No. CN101717076A Chinese patent " preparation method of vanadium nitride " is by vanadium-containing compound with having
Machine nitride mixes, and is calcined in nitrogenous gas, obtains vanadium nitride.The process that this method raw material prepares is more complicated, preparation process
Need the parameter that controls more, applied to super capacitor material preparation field.
A kind of Application No. CN104016314A Chinese patent " preparation method of vanadium nitride " uses the hot method of liquid phase solvent
Prepare vanadium nitride, liquid phase uses the aqueous solution or alcohols solvent, vanadium source be divalence, trivalent or the tetravalence chloride of vanadium, sulfate,
Nitrate and acetate, nitrogen source are ammonia, urea, nitrile, ammonium chloride, ammonium carbonate, ammonium acetate, ammonium sulfate.This method obtains
Vanadium nitride nano powder body, preparation technology is more complicated, applied to the ferrous materials additive in technical field of metal material.
The content of the invention
It is an object of the invention to provide a kind of preparation method and product of vanadium nitride elctro-catalyst, to overcome prior art
Existing complex process, vanadium nitride powder-body size are big, the defects of seldom is applied in electro-catalysis field.The present invention is sintered by one-step method
Obtain that technical process is simple, reaction time is short, homogeneous, the uniform electro catalytic activity of appearance and size of materials chemistry composition, stability
High vanadium nitride elctro-catalyst.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of vanadium nitride elctro-catalyst, comprises the following steps：
Step 1：Urea, ammonium metavanadate, cabaltous nitrate hexahydrate are sufficiently mixed according to a certain percentage, three's mass ratio is 10：
(1-2)：2,20~50min is ground in mortar, obtains reactant feed；
Step 2：Reactant feed prepared by step 1 is transferred in porcelain boat, reacted under certain atmosphere in tube furnace, temperature
Scope is 700-900 DEG C, soaking time 2-5h, and heating rate is 5-10 DEG C/min, and the powder obtained after cooling is with 0.5M's
H2SO4Solution soaks 10-20h（Remove the impurity such as cobalt oxide）, lower sediment is washed alternately totally six times by washing alcohol, in 60 DEG C of bakings
After case dries 6-10 h, 20~50min is ground in mortar, obtains vanadium nitride elctro-catalyst.
Certain atmosphere in above-mentioned steps two refers to any one in argon gas, nitrogen, vacuum.
And a kind of vanadium nitride elctro-catalyst prepared by the above method, vanadium nitride elctro-catalyst chi prepared by the present invention
Very little to be less than 25nm, pattern is uniform, good dispersion.
Compared with prior art, the present invention has technique effect beneficial below：
1）Step sintering process used in the present invention, technique is simple, time-consuming short, and it is cumbersome to overcome the precursor process being widely used
The defects of；
2）The introducing of cabaltous nitrate hexahydrate promotes the low temperature synthesis of pure phase vanadium nitride；
3）The reactivity of each raw material is high, improves reaction efficiency；
4）Obtained nano vanadium nitride powder-body size 20nm or so is reacted, much smaller than vanadium carbide powder chi on the document reported
It is very little, and its pattern is uniform, good dispersion；
5）Nano vanadium nitride powder-body prepared by this method can be applied to the water-splitting production hydrogen elctro-catalyst in electro-catalysis field.
Brief description of the drawings
Fig. 1 is the XRD of the nano vanadium nitride prepared in embodiment 1；
Fig. 2 is the nano vanadium nitride SEM figures prepared in embodiment 4；
Fig. 3 is the nano vanadium nitride LSV curve maps prepared in embodiment 5.
Embodiment
Below in conjunction with the accompanying drawings and embodiment is described in further detail to the present invention, it should be appreciated that these embodiments are only used
In explanation rather than limitation the scope of the present invention.Here it will be understood that this area after the content of the invention authorized has been read
Technical staff can make any change or modification to the present invention, and these equivalences equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
Step 1：1.5g urea is weighed, 0.3g ammonium metavanadates, 0.3g cabaltous nitrate hexahydrates, is sufficiently mixed grinding 20min；
Step 2：Raw material obtained by step 1 is put into porcelain boat, reacted in using argon gas as the tube furnace of atmosphere, heating rate is
5 DEG C/min, holding temperature is 700 DEG C, soaking time 2h, the powder 0.5M obtained after cooling H2SO4Solution soaks 10h
（Remove the impurity such as cobalt oxide）, lower sediment process washing alcohol, which is washed, to replace six times totally, after 60 DEG C of oven drying 6h, is ground in mortar
20min is ground, obtains vanadium nitride elctro-catalyst.
Fig. 1 is the XRD spectrum of the nano vanadium nitride prepared by the present embodiment, as can be seen from the figure standard corresponding to sample
PDF card numbers are 78-1315, and diffraction maximum is sharp, and intensity is high, illustrate the vanadium nitride nano powder body crystallization that the embodiment obtains
Property is fine.
Embodiment 2
Step 1：1.5g urea is weighed, 0.3g ammonium metavanadates, 0.3g cabaltous nitrate hexahydrates, is sufficiently mixed grinding 40min；
Step 2：Raw material obtained by step 1 is put into porcelain boat, reacted in using nitrogen as the tube furnace of atmosphere, heating rate is
8 DEG C/min, holding temperature is 800 DEG C, soaking time 5h, the powder 0.5M obtained after cooling H2SO4Solution soaks 15h
（Remove the impurity such as cobalt oxide）, lower sediment washes alternating totally six times by washing isopropanol, after 60 DEG C of oven drying 8h, mortar
Middle grinding 30min, obtains vanadium nitride elctro-catalyst.
Embodiment 3
Step 1：1.5g urea is weighed, 0.2g ammonium metavanadates, 0.3g cabaltous nitrate hexahydrates, is sufficiently mixed grinding 20min；
Step 2：Raw material obtained by step 1 is put into porcelain boat, reacted in using argon gas as the tube furnace of atmosphere, heating rate is
10 DEG C/min, holding temperature is 900 DEG C, soaking time 5h, the powder 0.5M obtained after cooling H2SO4Solution soaks 20h
（Remove the impurity such as cobalt oxide）, lower sediment washes alternating totally six times by washing methanol, after 60 DEG C of h of oven drying 6, mortar
Middle grinding 40min, obtains vanadium nitride elctro-catalyst.
Embodiment 4
Step 1：1.5g urea is weighed, 0.2g ammonium metavanadates, 0.3g cabaltous nitrate hexahydrates, is sufficiently mixed grinding 20min；
Step 2：Raw material obtained by step 1 is put into porcelain boat, reacted in using vacuum as the tube furnace of atmosphere, heating rate is
8 DEG C/min, holding temperature is 900 DEG C, soaking time 4h, the powder 0.5M obtained after cooling H2SO4Solution soaks 15h
（Remove the impurity such as cobalt oxide）, lower sediment washes alternating totally six times by washing alcohol, after 60 DEG C of h of oven drying 10, in mortar
20min is ground, obtains vanadium nitride elctro-catalyst.
Fig. 2 is the SEM figures of the nano vanadium nitride prepared by the present embodiment, and as can be seen from the figure sample topography is small
There is loose hole in grain, particle size distribution, sample dispersion is good, and hole is by course of reaction between 20nm or so, particle
Gas caused by middle reactant causes.
Embodiment 5
Step 1：1.5g urea is weighed, 0.15g ammonium metavanadates, 0.3g cabaltous nitrate hexahydrates, is sufficiently mixed grinding 20min；
Step 2：Raw material obtained by step 1 is put into porcelain boat, reacted in using argon gas as the tube furnace of atmosphere, heating rate is
5 DEG C/min, holding temperature is 800 DEG C, soaking time 2h, the powder 0.5M obtained after cooling H2SO4Solution soaks 10h
（Remove the impurity such as cobalt oxide）, lower sediment washes alternating totally six times by washing alcohol, after 60 DEG C of h of oven drying 6, in mortar
40min is ground, obtains vanadium nitride elctro-catalyst.
Fig. 3 is the LSV figures of the nano vanadium nitride prepared by the present embodiment, represents under the test conditions of pH 0, works as current density
For 10mA/cm2, when sweep speed is 3 mV/s, the sample overpotential is 240mV, illustrates there is excellent catalytic activity.
Embodiment 6
Step 1：1.5g urea is weighed, 0.15g ammonium metavanadates, 0.3g cabaltous nitrate hexahydrates, is sufficiently mixed grinding 50min；
Step 2：Raw material obtained by step 1 is put into porcelain boat, reacted in using nitrogen as the tube furnace of atmosphere, heating rate is
10 DEG C/min, holding temperature is 700 DEG C, soaking time 2h, the powder 0.5M obtained after cooling H2SO4Solution soaks 20h
（Remove the impurity such as cobalt oxide）, lower sediment washes alternating totally six times by washing ethanol, after 60 DEG C of h of oven drying 10, mortar
Middle grinding 50min, obtains vanadium nitride elctro-catalyst.
Claims (10)
1. a kind of preparation method of vanadium nitride elctro-catalyst, it is characterised in that comprise the following steps：
Step 1：Urea, ammonium metavanadate, cabaltous nitrate hexahydrate are sufficiently mixed according to formula rate, are fully ground, is reacted
Raw material；
Step 2：Reactant feed prepared by the step 1 pyroreaction under atmosphere protection, 700-900 DEG C of reaction temperature, instead
2-5h between seasonable, the powder obtained after cooling go the removal of impurity with pickle, wash lower sediment, drying precipitated, are fully ground, obtain
To vanadium nitride elctro-catalyst.
A kind of 2. preparation method of vanadium nitride elctro-catalyst according to claim 1, it is characterised in that the urea, partially
Ammonium vanadate, the mass ratio of cabaltous nitrate hexahydrate are 10：(1-2)：2.
A kind of 3. preparation method of vanadium nitride elctro-catalyst according to claim 1, it is characterised in that it is described Step 1:
Grinding in step 2,20 ~ 50min is fully ground to gained powder using mortar.
4. the preparation method of a kind of vanadium nitride elctro-catalyst according to claim 1, it is characterised in that the step 2
Atmosphere is any one in argon gas, nitrogen or vacuum.
5. the preparation method of a kind of vanadium nitride elctro-catalyst according to claim 1, it is characterised in that in the step 2
Pyroreaction, using ceramics be used as sample carrier.
6. the preparation method of a kind of vanadium nitride elctro-catalyst according to claim 1, it is characterised in that in the step 2
Pyroreaction, heated using tube furnace, 5-10 DEG C of heating rate/min, 700-900 DEG C of reaction temperature, reaction time 2-
5h。
7. the preparation method of a kind of vanadium nitride elctro-catalyst according to claim 1, it is characterised in that in the step 2
Go the removal of impurity with pickle, with 0.5M H2SO4Solution immersion 10-20h goes the removal of impurity.
8. the preparation method of a kind of vanadium nitride elctro-catalyst according to claim 1, it is characterised in that the step 2 is washed
Lower floor's solution is washed, is washed using washing with alcohol and replaces washing.
9. the preparation method of a kind of vanadium nitride elctro-catalyst according to claim 1, it is characterised in that in the step 2
Drying to lower sediment, in 60 DEG C of oven drying 6-10 h.
10. a kind of vanadium nitride elctro-catalyst prepared by claim 1 methods described, it is characterised in that by claim 1
Prepared by methods described, pattern is uniform.
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