CN109621960A - A kind of preparation method and application of graphene-supported nano Co OOH catalyst - Google Patents
A kind of preparation method and application of graphene-supported nano Co OOH catalyst Download PDFInfo
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- CN109621960A CN109621960A CN201811448219.2A CN201811448219A CN109621960A CN 109621960 A CN109621960 A CN 109621960A CN 201811448219 A CN201811448219 A CN 201811448219A CN 109621960 A CN109621960 A CN 109621960A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 30
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 26
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 24
- BLJNPOIVYYWHMA-UHFFFAOYSA-N alumane;cobalt Chemical compound [AlH3].[Co] BLJNPOIVYYWHMA-UHFFFAOYSA-N 0.000 claims abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- 239000012046 mixed solvent Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 159000000013 aluminium salts Chemical class 0.000 claims abstract description 6
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims abstract description 6
- 150000001868 cobalt Chemical class 0.000 claims abstract description 6
- 239000013077 target material Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 9
- SWCIQHXIXUMHKA-UHFFFAOYSA-N aluminum;trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SWCIQHXIXUMHKA-UHFFFAOYSA-N 0.000 claims description 4
- AMVQGJHFDJVOOB-UHFFFAOYSA-H aluminium sulfate octadecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O AMVQGJHFDJVOOB-UHFFFAOYSA-H 0.000 claims description 3
- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 claims description 3
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 238000007086 side reaction Methods 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 23
- 229910018916 CoOOH Inorganic materials 0.000 description 10
- 229910017052 cobalt Inorganic materials 0.000 description 10
- 239000010941 cobalt Substances 0.000 description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 239000004411 aluminium Substances 0.000 description 7
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 7
- 229910000000 metal hydroxide Inorganic materials 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000004457 water analysis Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to technical field of nanometer material preparation, a kind of preparation method and application of graphene-supported nano Co OOH catalyst, wherein preparation method is the following steps are included: (1) adds graphene oxide into the in the mixed solvent of ethylene glycol and water, cobalt salt, aluminium salt, urea is then added, back flow reaction is cooled to room temperature, it using deionized water centrifuge washing to neutrality, then is placed in drying box after drying and grinding, obtains graphene-supported cobalt aluminum bimetal hydroxide.(2) step 1 graphene-supported cobalt aluminum bimetal hydroxide is obtained to be added in strong alkali solution, ultrasonic disperse is stirred at room temperature, then using deionized water centrifuge washing to neutrality, it is placed in drying box, graphene-supported nano Co OOH catalyst target material is obtained after drying and grinding.Method of the invention is easy to operate, mild condition is easily-controllable, and is used as the series of advantages such as water decomposition Oxygen anodic evolution catalyst is high with catalytic activity, and reaction power is learnt well.
Description
Technical field
The present invention relates to a kind of preparation method and applications of graphene-supported nano Co OOH catalyst, belong to nano material
Preparation technical field.
Background technique
Water electrolysis hydrogen production is a kind of effective way for solving the increasingly serious at present energy and environmental problem, and in this process
Excessively high current potential needed for Anodic analyses oxygen half-reaction is the principal element for limiting its efficiency.The noble metal in the catalyst of catalysis analysis oxygen
Catalytic activity it is higher, but noble metal is expensive and content is less in nature, limits its extensive use in the industry.
In recent years, Transition metal based materials are widely studied and are applied to be catalyzed oxygen evolution reaction.Wherein, a large number of studies show that
Transition metals cobalt sill has the catalysis oxygen evolution activity for the even better than noble metal catalyst of matching in excellence or beauty.This is mainly due to cobalt-based materials
Material will form the CoOOH active intermediate kind with excellent properties in catalytic process.Therefore, it directly prepares and applies CoOOH
Material will effectively improve catalytic reaction activity as oxygen evolution reaction catalysts.In addition, graphene is as a kind of new carbon,
As composite material constructed by catalyst carrier light degradation, capacitor, lithium ion battery and in terms of have it is excellent
Different performance.Inspired by this, introduce graphene as conducting base load C oOOH for electrolysis water integral power performance with
The promotion of efficiency has important researching value and meaning.However, since CoOOH is usually the centre of formation during electro-catalysis
Species cause it to be synthetically prepared the relative complex difficulty of process.
Summary of the invention
In order to overcome the problems, such as that prior art exists, it is an object of the present invention to provide a kind of graphene-supported nano Co OOH to urge
The preparation method and application of agent.Graphene carrier large specific surface area used by the catalyst, the active component nanometer of load
CoOOH is uniformly dispersed and stability is good, preparation process simple process, safe operation, low in cost.Resulting material is prepared to use
Make oxygen-separating catalyst, catalytic activity is high, and kinetics performance is good, can effectively improve electrolysis water efficiency.
In order to achieve the above-mentioned object of the invention, in the presence of solving the problems, such as prior art, technical solution that the present invention takes
It is: a kind of preparation method of graphene-supported nano Co OOH catalyst, comprising the following steps:
Step 1 adds graphene oxide into the mixed solvent to 50~500mL ethylene glycol and water, and compound concentration is
The graphene oxide solution of 0.05~0.1mg/mL, 30~120min of ultrasonic disperse are then added cobalt salt, adjust concentration be 2~
4mg/mL, be added aluminium salt, adjustings concentration be 1~3mg/mL, be added urea, adjustings concentration be 4~10mg/mL, stir 5~
After 30min, prepared mixing dispersion solution is transferred in round-bottomed flask, temperature is controlled in 70~100 DEG C of back flow reactions 18
~48h, is cooled to room temperature, and using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, and temperature is controlled 40~60
It is ground after DEG C dry 6~12h, obtains graphene-supported cobalt aluminum bimetal hydroxide, the volume ratio of the ethylene glycol and water
For 1:1~4, the cobalt salt is selected from one of cobalt chloride hexahydrate, cabaltous nitrate hexahydrate or Cobalt monosulfate heptahydrate, the aluminium salt
Selected from one of Aluminium chloride hexahydrate, ANN aluminium nitrate nonahydrate or Patent alum.
Step 1 is obtained the graphene-supported cobalt aluminum bimetal hydroxide in part and is added to 40-60mL concentration by step 2
For in the strong alkali solution of 3~6mol/L, adjusting concentration is 1~4mg/mL, 1~10min of ultrasonic disperse, it is stirred at room temperature 12~
48h is placed in drying box then using deionized water centrifuge washing to neutrality, and temperature is controlled in 40~60 DEG C of dry 6~12h
After grind, obtain graphene-supported nano Co OOH catalyst target material, the strong alkali solution be selected from sodium hydroxide solution or
One of potassium hydroxide solution.
Graphene-supported nano Co OOH catalyst made from the preparation method, in anode of electrolytic water analysis oxygen catalysis reaction
Application in aspect.
The medicine have the advantages that a kind of preparation method and application of graphene-supported nano Co OOH catalyst, wherein making
Preparation Method is the following steps are included: (1) adds graphene oxide into the in the mixed solvent of ethylene glycol and water, ultrasonic disperse, then
Cobalt salt, aluminium salt, urea is added, back flow reaction is cooled to room temperature, and using deionized water centrifuge washing to neutrality, then is placed in drying box
After middle drying and grinding, graphene-supported cobalt aluminum bimetal hydroxide is obtained.(2) step 1 is obtained into graphene-supported cobalt
Aluminum bimetal hydroxide is added in strong alkali solution, and ultrasonic disperse is stirred at room temperature, and then uses deionized water centrifuge washing
It to neutrality, is placed in drying box, graphene-supported nano Co OOH catalyst target material is obtained after drying and grinding.With existing skill
Art is compared, and the present invention has the following advantages that, first is that this method have it is easy to operate, mild condition is easily-controllable, raw material sources are abundant, at
This is cheap, is not required to high-temperature calcination and the characteristics of strong oxidizer aoxidizes.Second is that CoOOH nanometer sheet in catalyst prepared by the present invention
It is uniformly dispersed in two-dimensional slice graphene surface, size uniformity.Utilize the special structure of graphene and excellent electron-transporting
Can, in conjunction with the high catalytic activity of CoOOH, it is special that excellent catalytic activity and dynamics are shown in terms of catalyticing anode oxygen evolution reaction
Property.This preparation method is also simultaneously development and exploitation potential application in lithium ion battery, fuel cell, photocatalysis and super electricity
The composite material of container etc. provides technical foundation.
Detailed description of the invention
Fig. 1 is that the scanning electron microscope of the graphene-supported cobalt aluminum bimetal hydroxide presoma prepared in embodiment 1 is shone
Piece figure.
Fig. 2 is the X-ray diffraction point of the graphene-supported cobalt aluminum bimetal hydroxide presoma prepared in embodiment 1
Analysis figure.
Fig. 3 is the stereoscan photograph figure of the graphene-supported nano Co OOH prepared in embodiment 4.
Fig. 4 is the transmission electron microscope photo figure of the graphene-supported nano Co OOH prepared in embodiment 4.
Fig. 5 is the X-ray diffraction analysis figure of the graphene-supported nano Co OOH prepared in embodiment 4.
Fig. 6 is the graphene-supported nano Co OOH catalyst electro-catalysis water decomposition Oxygen anodic evolution prepared in embodiment 5
Polarization curve.
Fig. 7 is the graphene-supported nano Co OOH catalyst electro-catalysis water decomposition Oxygen anodic evolution prepared in embodiment 5
Tafel curve graph.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Embodiment 1
Add graphene oxide into the in the mixed solvent of 200mL ethylene glycol Yu 300mL water, compound concentration 0.05mg/
The graphene oxide solution of ml, ultrasonic disperse 60min, subsequent addition 1.19g cobalt chloride hexahydrate, 0.61g Aluminium chloride hexahydrate,
2.11g urea after stirring 10min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 95 DEG C
48h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 50 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Fig. 1 is its stereoscan photograph, You Tuke
To know, cobalt aluminum bimetal hydroxide is hexagon laminated structure and of uniform size, about 1~2 μm.Fig. 2 is its X-ray diffraction point
Analysis figure.The resulting graphene-supported cobalt aluminum bimetal hydroxide of 40mg is taken to be added to the hydroxide that 40mL concentration is 6mol/L
In sodium solution, ultrasonic disperse 1min is stirred at room temperature for 24 hours.Drying box is then placed in neutrality using deionized water centrifuge washing
In, temperature control is ground after 60 DEG C of dry 12h, obtains graphene-supported nano Co OOH catalyst.
Embodiment 2
Add graphene oxide into the in the mixed solvent of 100mL ethylene glycol Yu 200mL water, compound concentration 0.05mg/
The graphene oxide solution of ml, ultrasonic disperse 90min, subsequent addition 0.88g cabaltous nitrate hexahydrate, 0.57g ANN aluminium nitrate nonahydrate,
1.27g urea after stirring 10min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 80 DEG C
36h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 60 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Take the resulting graphene-supported cobalt aluminium of 80mg
Double-metal hydroxide is added in the sodium hydroxide solution that 60mL concentration is 4mol/L, and ultrasonic disperse 1min is stirred at room temperature
24h.Then using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 60 DEG C of dry 12h,
Obtain graphene-supported nano Co OOH catalyst.
Embodiment 3
The in the mixed solvent of 50mL ethylene glycol Yu 50mL water is added graphene oxide into, compound concentration is 0.1mg/ml's
Graphene oxide solution, ultrasonic disperse 120min, subsequent addition 0.24g cobalt chloride hexahydrate, 0.12g Aluminium chloride hexahydrate,
0.42g urea after stirring 10min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 95 DEG C
48h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 40 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Take the resulting graphene-supported cobalt of 100mg
Aluminum bimetal hydroxide is added in the potassium hydroxide solution that 50mL concentration is 6mol/L, and ultrasonic disperse 3min is stirred at room temperature
12h.Then using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 60 DEG C of dry 12h,
Obtain graphene-supported nano Co OOH catalyst.
Embodiment 4
Add graphene oxide into the in the mixed solvent of 200mL ethylene glycol Yu 300mL water, compound concentration 0.05mg/
The graphene oxide solution of ml, ultrasonic disperse 90min, subsequent addition 1.19g cobalt chloride hexahydrate, 0.61g Aluminium chloride hexahydrate,
2.11g urea after stirring 10min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 95 DEG C
48h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 50 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Take the resulting graphene-supported cobalt aluminium of 40mg
Double-metal hydroxide is added in the sodium hydroxide solution that 40mL concentration is 5mol/L, and ultrasonic disperse 1min is stirred at room temperature
12h.Then using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 50 DEG C of dry 12h,
Obtain graphene-supported nano Co OOH catalyst.Fig. 3 is the scanning of the graphene-supported nano Co OOH prepared in the present embodiment
Electromicroscopic photograph, it can be seen that CoOOH nanometer sheet forms petal-like structures.Fig. 4 is graphene-supported receiving of preparing in the present embodiment
The transmission electron microscope photo of rice CoOOH, as seen from the figure, the CoOOH nanometer sheet of stratiform uniformly loads on the surface of graphene, and size is big
Small about 100~200nm.Fig. 5 is the X-ray diffraction analysis figure of the graphene-supported nano Co OOH prepared in the present embodiment,
Show that CoOOH has good crystallinity.
Embodiment 5
Add graphene oxide into the in the mixed solvent of 40mL ethylene glycol Yu 60mL water, compound concentration 0.06mg/ml
Graphene oxide solution, ultrasonic disperse 90min, then be added 0.24g cobalt chloride hexahydrate, 0.12g Aluminium chloride hexahydrate,
0.42g urea after stirring 15min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 95 DEG C
48h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 60 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Take the resulting graphene-supported cobalt aluminium of 40mg
Double-metal hydroxide is added in the sodium hydroxide solution that 40mL concentration is 5mol/L, and ultrasonic disperse 1min is stirred at room temperature
44h.Then using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 60 DEG C of dry 12h,
Obtain graphene-supported nano Co OOH catalyst.Graphene-supported nano Co OOH is applied to anode of electrolytic water as elctro-catalyst
Oxygen evolution reaction: weighing 4mg catalyst fines and be dispersed in 790 μ L ethyl alcohol, in the mixed solution of 200 μ L water and 10 μ L Nafion, surpasses
Sound disperses 30min.10 μ L dispersant liquid drops are taken to be coated in glass-carbon electrode (0.196cm2) surface, it dries under room temperature.By above-mentioned electricity
Pole is as working electrode, using 1mol/L potassium hydroxide aqueous solution as electrolyte, using platinized platinum as to electrode, Ag/AgCl conduct
Reference electrode carries out electrochemical property test, and Fig. 6 is polarization curve of the present embodiment as the electrode material, the results show that
The catalyst reaches 10mA cm-2Current density needed for overpotential be only 358mV.Fig. 7 is its Tafel curve graph, as seen from the figure
The catalyst has excellent catalytic kinetics performance.
Embodiment 6
Add graphene oxide into the in the mixed solvent of 80mL ethylene glycol Yu 120mL water, compound concentration 0.06mg/ml
Graphene oxide solution, ultrasonic disperse 60min, then be added 0.57g Cobalt monosulfate heptahydrate, 0.56g Patent alum,
0.84g urea after stirring 10min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 80 DEG C
48h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 40 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Take the resulting graphene-supported cobalt aluminium of 60mg
Double-metal hydroxide is added in the sodium hydroxide solution that 60mL concentration is 4mol/L, and ultrasonic disperse 5min is stirred at room temperature
48h.Then using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 60 DEG C of dry 12h,
Obtain graphene-supported nano Co OOH catalyst.
Embodiment 7
Add graphene oxide into the in the mixed solvent of 40mL ethylene glycol Yu 60mL water, compound concentration 0.05mg/ml
Graphene oxide solution, ultrasonic disperse 60min, then be added 0.24g cobalt chloride hexahydrate, 0.12g Aluminium chloride hexahydrate,
0.42g urea after stirring 10min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 95 DEG C
48h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 40 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Take the resulting graphene-supported cobalt aluminium of 40mg
Double-metal hydroxide is added in the sodium hydroxide solution that 40mL concentration is 5mol/L, and ultrasonic disperse 1min is stirred at room temperature
12h.Then using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 40 DEG C of dry 12h,
Obtain graphene-supported nano Co OOH catalyst.Catalyst obtained by the embodiment is used for anode of electrolytic water oxygen evolution reaction, as a result
It has been shown that, the catalyst reach 10mA cm-2Current density needed for overpotential be 361mV.
Embodiment 8
Add graphene oxide into the in the mixed solvent of 200mL ethylene glycol Yu 200mL water, compound concentration 0.1mg/ml
Graphene oxide solution, ultrasonic disperse 120min, then be added 0.96g cobalt chloride hexahydrate, 0.75g ANN aluminium nitrate nonahydrate,
1.68g urea after stirring 20min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 80 DEG C
48h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 60 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Take the resulting graphene-supported cobalt aluminium of 40mg
Double-metal hydroxide is added in the sodium hydroxide solution that 40mL concentration is 4mol/L, and ultrasonic disperse 1min is stirred at room temperature
36h.Then using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 60 DEG C of dry 12h,
Obtain graphene-supported nano Co OOH catalyst.
Embodiment 9
Add graphene oxide into the in the mixed solvent of 250mL ethylene glycol Yu 250mL water, compound concentration 0.07mg/
The graphene oxide solution of ml, ultrasonic disperse 90min, subsequent addition 1.19g cobalt chloride hexahydrate, 0.61g Aluminium chloride hexahydrate,
2.11g urea after stirring 10min, prepared mixed rear dispersion liquid is transferred in round-bottomed flask, temperature control flows back at 85 DEG C
48h is reacted, is cooled to room temperature, using deionized water centrifuge washing to neutrality, is subsequently placed in drying box, temperature is controlled at 40 DEG C
It is ground after dry 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide.Take the resulting graphene-supported cobalt aluminium of 60mg
Double-metal hydroxide is added in the potassium hydroxide solution that 60mL concentration is 5mol/L, and ultrasonic disperse 3min is stirred at room temperature
36h.Then using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 40 DEG C of dry 12h,
Obtain graphene-supported nano Co OOH catalyst.Catalyst obtained by the embodiment is used for anode of electrolytic water oxygen evolution reaction, as a result
It has been shown that, the catalyst reach 10mA cm-2Current density needed for overpotential be 360mV.
Claims (2)
1. a kind of preparation method of graphene-supported nano Co OOH catalyst, it is characterised in that the following steps are included:
Step 1 adds graphene oxide into the mixed solvent to 50~500mL ethylene glycol and water, and compound concentration is 0.05~
Cobalt salt is then added in the graphene oxide solution of 0.1mg/mL, 30~120min of ultrasonic disperse, and adjusting concentration is 2~4mg/mL,
Aluminium salt is added, adjusting concentration is 1~3mg/mL, and urea is added, and adjusting concentration is 4~10mg/mL, will after stirring 5~30min
Prepared mixing dispersion solution is transferred in round-bottomed flask, and temperature control is in 70~100 DEG C of 18~48h of back flow reaction, cooling
Be subsequently placed in drying box to room temperature using deionized water centrifuge washing to neutrality, temperature control 40~60 DEG C dry 6~
It is ground after 12h, obtains graphene-supported cobalt aluminum bimetal hydroxide, the volume ratio of the ethylene glycol and water is 1:1~4,
The cobalt salt is selected from one of cobalt chloride hexahydrate, cabaltous nitrate hexahydrate or Cobalt monosulfate heptahydrate, and the aluminium salt is selected from six water
Close one of aluminium chloride, ANN aluminium nitrate nonahydrate or Patent alum；
Step 2, step 1 is obtained the graphene-supported cobalt aluminum bimetal hydroxide in part be added to 40-60mL concentration be 3~
In the strong alkali solution of 6mol/L, adjusting concentration is 1~4mg/mL, and 12~48h is stirred at room temperature in 1~10min of ultrasonic disperse, with
Afterwards using deionized water centrifuge washing to neutrality, it is placed in drying box, temperature control is ground after 40~60 DEG C of dry 6~12h,
Graphene-supported nano Co OOH catalyst target material is obtained, the strong alkali solution is selected from sodium hydroxide solution or hydroxide
One of potassium solution.
2. graphene-supported nano Co OOH catalyst made from preparation method according to claim 1 is analysed in anode of electrolytic water
Application in oxygen catalyzed side reaction face.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129827A (en) * | 2019-06-18 | 2019-08-16 | 上海氯碱化工股份有限公司 | The method for preparing modified ruthenium titanium coating anode by lithium Induction Transformation method |
| CN110257858A (en) * | 2019-06-28 | 2019-09-20 | 青岛科技大学 | A kind of Ag/CoAl-LDH/ nickel foam NF multilevel structure combination electrode material and preparation method thereof |
| CN110947374A (en) * | 2019-12-16 | 2020-04-03 | 佛山职业技术学院 | Hydroxyl metal oxide nano catalyst and preparation method thereof |
| CN111821983A (en) * | 2020-04-26 | 2020-10-27 | 闽南师范大学 | Graphene oxide-europium hydroxide-cobalt hydroxide composite material, synthesis method and application of graphene oxide-europium hydroxide-cobalt hydroxide composite material in catalytic degradation |
| CN112844386A (en) * | 2020-12-25 | 2021-05-28 | 湖南大学 | Preparation method and application of trace boron-doped cobalt oxyhydroxide |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301841A (en) * | 2012-03-15 | 2013-09-18 | 北京化工大学 | Graphene loaded high-dispersion nano Ni catalyst as well as preparation method and application thereof |
| CN104992843A (en) * | 2015-08-01 | 2015-10-21 | 大连理工大学 | Titanium disulfide nano sheet/graphene composite material counter electrode and preparation method thereof |
| CN106914244A (en) * | 2017-03-06 | 2017-07-04 | 南京工业大学 | A kind of graphene-based metallic compound nano array material preparation and application |
| CN106935419A (en) * | 2017-04-06 | 2017-07-07 | 中国科学院山西煤炭化学研究所 | A kind of method that cobalt nickel bimetal oxide and Graphene prepare electrode material for super capacitor |
| CN108043393A (en) * | 2017-12-16 | 2018-05-18 | 大连理工大学 | A kind of preparation method and application of carbon material palladium/carbon material catalyst of immobilized Pd nano particle in situ |
-
2018
- 2018-11-30 CN CN201811448219.2A patent/CN109621960A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301841A (en) * | 2012-03-15 | 2013-09-18 | 北京化工大学 | Graphene loaded high-dispersion nano Ni catalyst as well as preparation method and application thereof |
| CN104992843A (en) * | 2015-08-01 | 2015-10-21 | 大连理工大学 | Titanium disulfide nano sheet/graphene composite material counter electrode and preparation method thereof |
| CN106914244A (en) * | 2017-03-06 | 2017-07-04 | 南京工业大学 | A kind of graphene-based metallic compound nano array material preparation and application |
| CN106935419A (en) * | 2017-04-06 | 2017-07-07 | 中国科学院山西煤炭化学研究所 | A kind of method that cobalt nickel bimetal oxide and Graphene prepare electrode material for super capacitor |
| CN108043393A (en) * | 2017-12-16 | 2018-05-18 | 大连理工大学 | A kind of preparation method and application of carbon material palladium/carbon material catalyst of immobilized Pd nano particle in situ |
Non-Patent Citations (1)
| Title |
|---|
| XIAOTONG HAN ET AL.: "Ultrasensitive Iron-Triggered Nanosized Fe-CoOOH Integrated with Graphene for Highly Efficient Oxygen Evolution", 《ADV. ENERGY MATER.》 * |
Cited By (11)
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|---|---|---|---|---|
| CN110129827A (en) * | 2019-06-18 | 2019-08-16 | 上海氯碱化工股份有限公司 | The method for preparing modified ruthenium titanium coating anode by lithium Induction Transformation method |
| CN110257858A (en) * | 2019-06-28 | 2019-09-20 | 青岛科技大学 | A kind of Ag/CoAl-LDH/ nickel foam NF multilevel structure combination electrode material and preparation method thereof |
| CN110257858B (en) * | 2019-06-28 | 2021-02-26 | 青岛科技大学 | Ag/CoAl-LDH/foamed nickel NF multi-level structure composite electrode material and preparation method thereof |
| CN110947374A (en) * | 2019-12-16 | 2020-04-03 | 佛山职业技术学院 | Hydroxyl metal oxide nano catalyst and preparation method thereof |
| CN113529113A (en) * | 2020-03-31 | 2021-10-22 | 中国科学院宁波材料技术与工程研究所 | Preparation method of 2, 5-furandicarboxylic acid |
| CN113529113B (en) * | 2020-03-31 | 2022-09-16 | 中国科学院宁波材料技术与工程研究所 | Preparation method of 2, 5-furandicarboxylic acid |
| CN111821983A (en) * | 2020-04-26 | 2020-10-27 | 闽南师范大学 | Graphene oxide-europium hydroxide-cobalt hydroxide composite material, synthesis method and application of graphene oxide-europium hydroxide-cobalt hydroxide composite material in catalytic degradation |
| CN112844386A (en) * | 2020-12-25 | 2021-05-28 | 湖南大学 | Preparation method and application of trace boron-doped cobalt oxyhydroxide |
| CN113233517A (en) * | 2021-06-29 | 2021-08-10 | 上海交通大学 | Single-layer/few-layer two-dimensional transition metal oxide nano material aqueous dispersion liquid and preparation method thereof |
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