CN107694586B - It a kind of graphene winding molybdenum carbide/carbosphere elctro-catalyst and preparation method thereof and applies in water electrolysis hydrogen production in acid condition - Google Patents
It a kind of graphene winding molybdenum carbide/carbosphere elctro-catalyst and preparation method thereof and applies in water electrolysis hydrogen production in acid condition Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910039444 MoC Inorganic materials 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- 238000004804 winding Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000001257 hydrogen Substances 0.000 title claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 17
- 239000002253 acid Substances 0.000 title claims abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 238000001694 spray drying Methods 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 15
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920001661 Chitosan Polymers 0.000 claims abstract description 11
- 239000012046 mixed solvent Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000012300 argon atmosphere Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 30
- 238000006555 catalytic reaction Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 239000012298 atmosphere Substances 0.000 abstract description 2
- 239000011261 inert gas Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 230000008569 process Effects 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 150000004676 glycans Chemical class 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 229910003178 Mo2C Inorganic materials 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 235000018660 ammonium molybdate Nutrition 0.000 description 2
- 239000011609 ammonium molybdate Substances 0.000 description 2
- 229940010552 ammonium molybdate Drugs 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004502 linear sweep voltammetry Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 235000007686 potassium Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- 239000011684 sodium molybdate Substances 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
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
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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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- 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
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- 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
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Abstract
The invention belongs to catalysis material fields, it is related to a kind of graphene winding molybdenum carbide/carbosphere elctro-catalyst and preparation method thereof and applies in water electrolysis hydrogen production in acid condition, the following steps are included: step 1: molybdate and graphene oxide is soluble in water, chitosan is dissolved in the in the mixed solvent of acetic acid and water, then two kinds of solution are mixed, is stirred under certain speed；Step 2: by step 1 mixed solution by spray drying, then collecting solid powder, the high temperature anneal under atmosphere of inert gases, obtains graphene winding molybdenum carbide/carbosphere elctro-catalyst.Winding molybdenum carbide/the carbosphere of graphene prepared by the present invention is of uniform size, and molybdenum carbide nanoparticle is uniformly dispersed, and its preparation process is simple, and easy to operate, controllability is strong, and excellent chemical property is shown in electrolysis water liberation of hydrogen.
Description
Technical field
The invention belongs to catalysis material field, it is related to a kind of graphene winding molybdenum carbide/carbosphere elctro-catalyst and its system
It is applied in Preparation Method and in acid condition water electrolysis hydrogen production.
Background technique
With the fast development of modern society, global environmental pollution is serious, and energy consumption is rapid, scarcity of resources, compels to be essential
Want a kind of clean reproducible energy.Therefore, the development of effective cleaning and sustainable Hydrogen Energy source technology has attracted more next
More concerns, in the past few years, hydrogen be known as a promising energy, for reduce we to fossil fuel according to
Rely, reduces the discharge of greenhouse gases and other toxic gases, benefit environment.In the past few years, more and more attention collection
In in order to realize the water decomposition of high-energy reducing liberation of hydrogen with catalyst producing hydrogen by sustainable electrochemical process
The driving energy of reaction (HER) is very important.
Pt/C is that H2-producing capacity is best currently on the market, a kind of most stable of catalyst.But since its resource is less, at
This is higher, cannot apply on a large scale.More and more researchs, which concentrate on pursuing, has similar activity and stability with Pt
Inexpensive substitute.In the past decade, before transient metal sulfide, nitride, phosphide, carbide have been used as
The elctro-catalyst on way is reported, especially transition metal carbide, for example, molybdenum carbide (J. Mater. Chem. A, 2017,
5,4879) there is significant catalytic activity, due to its unique electricity and catalytic performance similar to noble metal (passes through induction
Carbon is to metal lattice).But after high-temperature process carbide will appear polymerism so that becoming large-sized, specific surface area
Reduce；CN106925312 discloses a kind of grapheme modified composite material and preparation method of carbonization molybdenum doping linear polymer,
Molybdenum carbide nanoparticle is dispersed in polymer and graphene, but preparation method is more complicated, is unfavorable for actually answering
With.
Summary of the invention
The present invention is in view of the above-mentioned problems, provide a kind of graphene winding molybdenum carbide/carbosphere elctro-catalyst and its preparation side
It is applied in method and in acid condition water electrolysis hydrogen production.
The technical solution used in the present invention is as follows: a kind of graphene winding molybdenum carbide/carbosphere elctro-catalyst preparation
Method, comprising the following steps:
Step 1: molybdate and graphene oxide is soluble in water, chitosan is dissolved in the in the mixed solvent of acetic acid and water,
Then two kinds of solution are mixed, is stirred under certain speed；
Step 2: by step 1 mixed solution by spray drying, solid powder is then collected, under atmosphere of inert gases
The high temperature anneal obtains graphene winding molybdenum carbide/carbosphere elctro-catalyst.
In step 1, the mass ratio of the chitosan and molybdate is 0.5:1 ~ 2:1.
In step 1, the mass ratio of the molybdate and graphene oxide is 1:10-5:10.
In step 1, molybdate can be one of ammonium molybdate, sodium molybdate, potassium molybdate or a variety of.
In step 1, the mass volume ratio of chitosan and acetic acid is 1:1-1:4 g/ml.
In step 1, it is 500-1600 r/min that speed, which is mixed, in two kinds of solution.
It is 100 ~ 130 DEG C that temperature is arranged when spray drying, and sample introduction speed is 4 ~ 6mL/min.
In annealing, annealing temperature is 600 DEG C ~ 900 DEG C, 1 ~ 5 DEG C/min of heating rate, keeps the temperature 2 ~ 5h.
A kind of graphene winding molybdenum carbide/carbosphere elctro-catalyst obtained by above-mentioned preparation method
Above-mentioned graphene winding molybdenum carbide/carbosphere elctro-catalyst is applied in water electrolysis hydrogen production in acid condition.
Beneficial effects of the present invention are as follows:
1. the chitosan solution of different quality ratio and ammonium molybdate solution spray-on process are mixed high-speed stirred by the present invention, obtain
To uniformly mixed solution, be conducive to make the evenly dispersed full and uniform mixing for realizing raw material of molybdenum carbide nanoparticle in product.It is special
Be not using the amino in chitosan in conjunction with molybdenum acid ion so that Mo2C nanoparticle is evenly distributed in carbosphere,
The agglomeration occurred by high temperature is avoided, thus the more active sites of exposure.
2. graphene oxide can effectively improve the electric conductivity of elctro-catalyst in the present invention, accelerate electricity in electrochemical process
Lotus delivery rate, microballoon made from spray drying process have the property of bigger serface and porous rate, be conducive to electrolyte with
The diffusion of hydrogen reduces the resistance to mass tranfer during electro-catalysis.
3. nitrogen rich in the chitosan of raw material employed in the present invention, nitrogen-atoms is realized after high annealing
Doped and compounded material is conducive to the precipitation of electrolysis water process hydrogen to reduce the adsorption energy of hydrogen on the surface of the material.
4. preparation process of the present invention is simple, easy to operate, controllability is strong, can be used for being mass produced and for industrial electro
Solve elutriation hydrogen.
Detailed description of the invention
Fig. 1 is that the method is urged according to graphene synthesized in embodiment 2 winding molybdenum carbide/carbosphere electricity through the invention
The XRD diagram of agent；
Fig. 2 is that graphene winds molybdenum carbide/carbosphere elctro-catalyst scanning electron microscope and high-resolution picture；
Fig. 3 and Fig. 4 is that graphene winds molybdenum carbide/carbosphere elctro-catalyst catalytic hydrogen evolution performance map.Wherein, Mo2C/NC
For 1 sample of comparative example, S-Mo2C/NC0.3GO750 is 2 sample of embodiment.
Specific embodiment
The present invention is specifically described or is further illustrated by the following examples, its object is to better understand this
The technical connotation of invention, but it is not intended to limit the present invention.
Embodiment 1:
Sample preparation: 1g molybdate and 14mL7.2mg/mL graphene oxide are dissolved in 28mL deionized water, by 1g shell
Glycan is dissolved in the in the mixed solvent of 2 mL acetic acid and 186mL deionized water, then mixes two kinds of solution, in 500-1600 r/
It is stirred under the speed of min.By mixed solution by spray drying, setting temperature is 100 ~ 130 DEG C when spray drying, sample introduction speed
For 4 ~ 6mL/min, solid powder is then collected, the high temperature anneal under argon atmosphere is warming up to 750 DEG C through 6h, keeps the temperature 3h
Natural cooling afterwards obtains graphene winding molybdenum carbide/carbosphere elctro-catalyst.
Electro-catalysis application: the sample of 2mg and the conductive carbon of 1mg are dissolved in 500 μ L alcohol-water mixtures, and ultrasound keeps its mixing equal
It is even, black suspension is formed, pipetting 10 μ L suspensions in 5 μ L mass fractions on glass-carbon electrode, are added dropwise after natural drying is 0.5%
Nafion.In three-electrode system, (glass-carbon electrode is saturated Ag/AgCl electrode as reference electrode, platinum filament electricity as working electrode
Pole is used as to electrode) in, with 0.5M H2SO4Solution is the linear sweep voltammetry curve that electrolyte solution measures catalyst.The sample
Product current density is 10mA/cm2When, overpotential 76mV.
Embodiment 2:
Sample preparation: 1g molybdate and 42mL7.2mg/mL graphene oxide are dissolved in 28mL deionized water, by 1g shell
Glycan is dissolved in the in the mixed solvent of 2 mL acetic acid and 158mL deionized water, then mixes two kinds of solution, in 500-1600 r/
It is stirred under the speed of min.By mixed solution by spray drying, setting temperature is 100 ~ 130 DEG C when spray drying, sample introduction speed
For 4 ~ 6mL/min, solid powder is then collected, the high temperature anneal under argon atmosphere is warming up to 750 DEG C through 6h, keeps the temperature 3h
Natural cooling afterwards obtains graphene winding molybdenum carbide/carbosphere elctro-catalyst.
Electro-catalysis application: electrode and test are prepared with example 1.The sample current density is 10mA/cm2When, overpotential is
70mV.This sample electrocatalysis characteristic is optimal.
Embodiment 3:
Sample preparation: 1g molybdate and 70mL7.2mg/mL graphene oxide are dissolved in 28mL deionized water, by 1g shell
Glycan is dissolved in the in the mixed solvent of 2 mL acetic acid and 130mL deionized water, then mixes two kinds of solution, in 500-1600 r/
It is stirred under the speed of min.By mixed solution by spray drying, setting temperature is 100 ~ 130 DEG C when spray drying, sample introduction speed
For 4 ~ 6mL/min, solid powder is then collected, the high temperature anneal under argon atmosphere is warming up to 750 DEG C through 6h, keeps the temperature 3h
Natural cooling afterwards obtains graphene winding molybdenum carbide/carbosphere elctro-catalyst.
Electro-catalysis application: electrode and test are prepared with example 1.The sample current density is 10mA/cm2When, overpotential is
96mV。
Embodiment 4:
Sample preparation: 1g molybdate and 42mL7.2mg/mL graphene oxide are dissolved in 28mL deionized water, by 1g shell
Glycan is dissolved in the in the mixed solvent of 2 mL acetic acid and 158mL deionized water, then mixes two kinds of solution, in 500-1600 r/
It is stirred under the speed of min.By mixed solution by spray drying, setting temperature is 100 ~ 130 DEG C when spray drying, sample introduction speed
For 4 ~ 6mL/min, solid powder is then collected, the high temperature anneal under argon atmosphere is warming up to 850 DEG C through 6h 50min,
Natural cooling after heat preservation 3h obtains graphene winding molybdenum carbide/carbosphere elctro-catalyst.
Electro-catalysis application: electrode and test are prepared with example 1.The sample current density is 10mA/cm2When, overpotential is
88mV。
Comparative example 1:
Sample preparation: 1g molybdate is dissolved in 28mL deionized water, and 1g chitosan is dissolved in 2 mL acetic acid and 200 mL
Then two kinds of solution are mixed, are stirred under the speed of 500-1600 r/min by the in the mixed solvent of deionized water.It will mix molten
Liquid is by spray drying, and setting temperature is 100 ~ 130 DEG C when spray drying, and sample introduction speed is 4 ~ 6mL/min, then collects solid
Powder, the high temperature anneal under argon atmosphere are warming up to 750 DEG C through 6h, keep the temperature natural cooling after 3h, obtain graphene winding
Molybdenum carbide/carbosphere elctro-catalyst.
Electro-catalysis application: electrode and test are prepared with example 1.The sample current density is 10mA/cm2When, overpotential is
97mV。
Comparative example 2:
Sample preparation: 1g molybdate is dissolved in 28mL deionized water, and 0.5g chitosan is dissolved in 2 mL acetic acid and 200mL
Then two kinds of solution are mixed, are stirred under the speed of 500-1600 r/min by the in the mixed solvent of deionized water.It will mix molten
Liquid is by spray drying, and setting temperature is 100 ~ 130 DEG C when spray drying, and sample introduction speed is 4 ~ 6mL/min, then collects solid
Powder, the high temperature anneal under argon atmosphere are warming up to 750 DEG C through 6h, keep the temperature natural cooling after 3h, obtain graphene winding
Molybdenum carbide/carbosphere elctro-catalyst.
Electro-catalysis application: electrode and test are prepared with example 1.When the sample current density is 10mA/cm2, overpotential is
114mV。
Comparative example 3:
Sample preparation: 1g molybdate is dissolved in 28mL deionized water, and 2g chitosan is dissolved in 2 mL acetic acid and 200mL is gone
Then two kinds of solution are mixed, are stirred under the speed of 500-1600 r/min by the in the mixed solvent of ionized water.By mixed solution
By spray drying, setting temperature is 100 ~ 130 DEG C when spray drying, and sample introduction speed is 4 ~ 6mL/min, then collects solid powder
End, the high temperature anneal under argon atmosphere are warming up to 750 DEG C through 6h, keep the temperature natural cooling after 3h, obtain graphene winding carbon
Change molybdenum/carbosphere elctro-catalyst.
Electro-catalysis application: electrode and test are prepared with example 1.The sample current density is 10mA/cm2When, overpotential is
148mV。
Claims (3)
1. a kind of graphene winds molybdenum carbide/carbosphere elctro-catalyst preparation method, which comprises the following steps:
1g molybdate and 42mL7.2mg/mL graphene oxide are dissolved in 28mL deionized water, 1g chitosan is dissolved in 2 mL second
Then two kinds of solution are mixed, are stirred under the speed of 500-1600 r/min by the in the mixed solvent of acid and 158mL deionized water
It mixes, by mixed solution by spray drying, setting temperature is 100 ~ 130 DEG C when spray drying, and sample introduction speed is 4 ~ 6mL/min,
Then solid powder is collected, the high temperature anneal under argon atmosphere is warming up to 750 DEG C through 6h, keeps the temperature natural cooling after 3h, obtain
Molybdenum carbide/carbosphere elctro-catalyst is wound to graphene.
2. a kind of graphene winding molybdenum carbide/carbosphere elctro-catalyst obtained by preparation method described in claim 1.
3. graphene winding molybdenum carbide/carbosphere elctro-catalyst as claimed in claim 2 is in acid condition in water electrolysis hydrogen production
Using.
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