CN114232024A - Preparation method of monodisperse nickel-iron nano material for oxygen evolution by electrolyzing water - Google Patents
Preparation method of monodisperse nickel-iron nano material for oxygen evolution by electrolyzing water Download PDFInfo
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- 239000001301 oxygen Substances 0.000 title claims abstract description 56
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 56
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 24
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 229910000863 Ferronickel Inorganic materials 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 18
- 239000006229 carbon black Substances 0.000 claims abstract description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 13
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 12
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 3
- 239000011363 dried mixture Substances 0.000 claims abstract description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract 2
- 238000010438 heat treatment Methods 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 32
- 238000000034 method Methods 0.000 abstract description 9
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 abstract description 7
- 239000000463 material Substances 0.000 description 36
- 239000000243 solution Substances 0.000 description 14
- 230000003197 catalytic effect Effects 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000012528 membrane Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000003011 anion exchange membrane Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- -1 oxygen ion Chemical class 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910000457 iridium oxide Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/089—Alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- 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
-
- 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
Abstract
The invention discloses a preparation method of a monodisperse ferronickel nano material for oxygen evolution by electrolysis of water, which comprises the following steps: (1) dissolving nickel chloride hexahydrate, ferrous chloride tetrahydrate and polyvinylpyrrolidone in ethylene glycol, and performing ultrasonic dispersion uniformly to obtain a mixed solution; (2) transferring the obtained mixed solution into a pressure-resistant reaction tube, reacting for 10-13h at 180 ℃, then taking out the pressure-resistant reaction tube, and naturally cooling to room temperature; (3) taking out the reaction liquid obtained in the step (2), adding acetone and ethanol, and centrifuging and washing for multiple times; (4) mixing the product obtained after centrifugal washing in the step (3) with carbon black to obtain a mixture; (5) and (4) drying the mixture obtained in the step (4) in vacuum, then placing the dried mixture in a tubular furnace, introducing oxygen and roasting to prepare the monodisperse nickel-iron nano material for electrolytic water oxygen evolution. The particle size of the nano-particle nickel-iron alloy prepared by the method is less than 10nm, and the nano-particle nickel-iron alloy is uniformly distributed on carbon black, so that the dispersibility is ensured, and the nano-particle nickel-iron alloy has a larger specific surface area.
Description
Technical Field
The invention relates to the field of hydrogen and oxygen evolution materials for water electrolysis of industrial anion exchange membranes, in particular to a preparation method of a monodisperse nickel-iron nano material for water electrolysis and oxygen evolution of anion exchange membranes.
Background
The types and the advantages and the disadvantages of the existing water electrolysis technology are as follows:
1. alkaline electrolyzed water
As the most common water electrolysis technology, the alkaline water electrolysis technology has low cost and mature technology, has large-scale application examples at home and abroad, but has low current density, and the problems of potential safety hazard caused by the cross of hydrogen and oxygen gases and overhigh electrolyte concentration still exist, so that the electrolysis efficiency cannot be improved, and the electrolysis efficiency of the alkaline water electrolysis technology is obviously reduced in a low-temperature environment.
2. Proton exchange membrane electrolyzed water
As a new technology for producing hydrogen by electrolyzing water in recent years, the water electrolyzed by the proton exchange membrane has excellent performances, such as high working current density, low reaction temperature, high energy efficiency, small volume, quick response, high concentration and the like. The method has the defect of high cost, and the cathode of the water electrolyzed by the proton exchange membrane usually adopts a platinum carbon material to catalyze and separate hydrogen, and the anode adopts an iridium oxide material to catalyze and separate oxygen. At present, no large-scale industrialization example exists, the large-scale industrialization example is still mainly in a laboratory stage, and the problem of high cost limits the industrial application of the proton exchange membrane water electrolysis technology.
3. Solid oxide electrolyzed water
The hydrogen production based on the solid oxide electrolyzed water has the advantages of low cost, environmental friendliness, high efficiency and the like, and according to the difference of electrolyte materials, the hydrogen production based on the solid oxide electrolyzed water has two types: oxygen ion conduction and proton conduction. Among them, oxygen ion conduction has an advantage of stable operation at high temperature (800 ℃), but some key problems, such as poor long-term stability of the battery, interlayer diffusion, manufacturing and material problems, are not solved, resulting in that the solid oxide electrolyzed water cannot be applied on a large scale.
Disclosure of Invention
Based on the technical problems, the invention provides a preparation method of a monodisperse ferronickel nano material for oxygen evolution by water electrolysis.
The technical solution adopted by the invention is as follows:
a preparation method of a monodisperse ferronickel nano material for oxygen evolution by electrolysis of water comprises the following steps:
(1) selecting nickel chloride hexahydrate, ferrous chloride tetrahydrate, polyvinylpyrrolidone and ethylene glycol as raw materials, dissolving the nickel chloride hexahydrate, the ferrous chloride tetrahydrate and the polyvinylpyrrolidone in the ethylene glycol, performing ultrasonic treatment for 30-60min, and uniformly dispersing to obtain a mixed solution;
(2) transferring the mixed solution obtained in the step (1) into a pressure-resistant reaction tube, reacting for 10-13h at the temperature of 180-198 ℃, then taking out the pressure-resistant reaction tube, and naturally cooling to room temperature;
(3) taking out the reaction liquid obtained in the step (2), adding acetone and ethanol, and centrifuging and washing for multiple times;
(4) mixing the product obtained after centrifugal washing in the step (3) with carbon black to obtain a mixture;
(5) and (4) drying the mixture obtained in the step (4) in vacuum, then placing the dried mixture in a tube furnace, introducing oxygen and roasting to prepare the monodisperse ferronickel nano material for oxygen evolution in electrolyzed water, or the monodisperse nano particle structure ferronickel material.
Preferably, the molar ratio of the nickel chloride hexahydrate to the ferrous chloride tetrahydrate is 1-1.6: 0.4-1.
Preferably, the mass ratio of the nickel chloride hexahydrate to the polyvinylpyrrolidone to the ethylene glycol is 1-1.6:0.4-1: 1-2.
Preferably, the dosage ratio of the nickel chloride hexahydrate to the carbon black is 1-1.6mmol:42-85 mg.
Preferably, the carbon black is selected from any one of VXC-72, EC600JD, and EC300 JD.
Preferably, the roasting reaction conditions are as follows: controlling the heating rate at 2 ℃/min, heating to 300-400 ℃ and roasting for 1 h.
The particle size of the monodisperse ferronickel nano material for electrolyzing water to separate oxygen is below 10 nm.
The beneficial technical effects of the invention are as follows:
the invention provides a preparation method of a novel monodisperse ferronickel nano material for oxygen evolution of anion exchange membrane electrolyzed water, which adopts a glycol reduction system to synthesize a ferronickel alloy with a nano particle structure, adopts ferronickel to mix according to a certain weight ratio for reaction, adopts glycol to reduce at 180 ℃, and simultaneously adds polyvinylpyrrolidone as a growth inducer to promote the growth of the ferronickel alloy with the nano particle structure. And then loading the nickel-iron nano material on carbon black, and carrying out high-temperature heat treatment on the material to obtain the monodisperse nickel-iron nano material. The nickel-iron alloy prepared by the method has the advantages of uniform dispersion and high mechanical strength, the particle size of the nano-particle nickel-iron alloy prepared by the method is less than 10nm, and the nano-particle nickel-iron alloy is uniformly distributed on carbon black, so that the dispersibility is ensured, and meanwhile, the nano-particle nickel-iron alloy has a larger specific surface area. The rotating disk electrode shows lower over potential, which shows that the ferronickel nano material prepared by the method has excellent performance.
The monodisperse ferronickel nano material prepared by the method has the advantages of low overpotential of oxygen evolution half reaction, mild reaction condition, low cost and high efficiency.
According to the invention, precious metal is not used as an oxygen evolution material, the catalytic activity of the material is greatly improved by adopting monoatomic dispersion, meanwhile, the stability is good, the nano-particle material is prepared by adopting a two-step method, the particle size is controlled below 10nm by introducing oxygen and the like, and the stability is improved by high-temperature roasting; the monodisperse nickel-iron nano material prepared by the method can realize low-cost application of oxygen evolution materials.
Drawings
FIG. 1 is a process flow diagram of the present invention;
fig. 2 is a performance test chart of a three-electrode system for preparing a nickel-iron material with a monodisperse nano-particle structure in the embodiment of the invention.
Detailed Description
The invention is further described with reference to the following detailed description of embodiments in conjunction with the accompanying drawings.
Example 1
The preparation method of the nickel-iron material with the monodisperse nano-particle structure comprises the following steps:
1) 1.6mmol of NiCl2·6H2O、0.4mmol FeCl2·4H2O and 200mg PVP are dissolved in 14ml of ethylene glycol solution and dispersed evenly by ultrasonic to obtain a mixed solution.
2) Transferring the mixed solution obtained in the step 1) into a pressure-resistant reaction tube, reacting at 180 ℃ for 10h, taking out the pressure-resistant reaction tube after the reaction is finished, and naturally cooling to room temperature to obtain a reaction solution.
3) Adding 25ml of acetone and 10ml of ethanol into the reaction solution obtained in the step 2), and carrying out centrifugal washing for 6 times to obtain a transparent upper-layer solution and a colloidal precipitate at the lower part.
4) Adding the lower colloidal precipitate washed in the step 3) and 84.6166mg of EC600JD carbon black into 20ml of ethanol respectively, and ultrasonically dispersing for 1h to uniformly disperse the precipitate and the carbon black respectively. After the dispersion was completed, mixing and stirring were carried out for 12 hours to obtain a mixture.
5) And (3) drying the mixture obtained in the step 4) in vacuum for 12h, introducing oxygen into a tube furnace for roasting, wherein the roasting condition is that the temperature is increased from room temperature in a gradient manner, the heating rate is 2 ℃/min, and the temperature is increased to 300 ℃ for roasting for 1h to prepare the monodisperse nano-particle structure ferronickel material.
The catalytic oxygen evolution performance of the electrolyzed water in the embodiment is measured by a CHI760E workstation, a three-electrode test system is formed by adopting an oxygen evolution electrode as a working electrode, a carbon rod and a saturated calomel electrode, and the sweep rate is 5mV/s in 1mol/L potassium hydroxide solution.
The monodisperse nanoparticle structure ferronickel material prepared by the embodiment is at 10mA/cm2Under current density, the overpotential can reach 259 mV. The nickel-iron material with the monodisperse nano-particle structure has excellent catalytic activity and stability when being used as an oxygen evolution electrode, and is a potential application material of a high-catalytic-performance electrolytic water oxygen evolution catalyst.
Fig. 2 is a performance test chart of a three-electrode system of the nickel-iron material with the monodisperse nano-particle structure prepared in the embodiment of the invention, and the polarization curve and the overpotential of each embodiment can be seen from the chart.
Example 2
The preparation method of the nickel-iron material with the monodisperse nano-particle structure comprises the following steps:
1) 1.2mmol of NiCl2·6H2O、0.8mmol FeCl2·4H2O and 200mg PVP are dissolved in 14ml of ethylene glycol and uniformly dispersed by ultrasonic to obtain a mixed solution.
2) Transferring the mixed solution obtained in the step 1) into a pressure-resistant reaction tube, reacting at 180 ℃ for 10h, taking out the pressure-resistant reaction tube after the reaction is finished, and naturally cooling to room temperature to obtain a reaction solution.
3) Adding 25ml of acetone and 10ml of ethanol into the reaction solution taken out in the step 2), and performing centrifugal washing.
4) Ultrasonically dispersing the washed product obtained in the step 3) and 84.6166mg of EC300JD carbon black respectively, and mixing and stirring to obtain a mixture.
5) And (3) drying the mixture obtained in the step 4) in vacuum for 12h, introducing oxygen into a tube furnace for roasting under the roasting condition that the heating rate is 2 ℃/min, and roasting at 300 ℃ for 1h to prepare the monodisperse nano-particle structure ferronickel material.
The catalytic oxygen evolution performance of the electrolyzed water in the embodiment is measured by a CHI760E workstation, a three-electrode test system is formed by adopting an oxygen evolution electrode as a working electrode, a carbon rod and a saturated calomel electrode, and the sweep rate is 5mV/s in 1mol/L potassium hydroxide solution.
The monodisperse nanoparticle structure ferronickel material prepared by the embodiment is at 10mA/cm2The overpotential can reach 240mV under the current density. The nickel-iron material with the monodisperse nano-particle structure has excellent catalytic activity and stability when being used as an oxygen evolution electrode, and is a potential application material of a high-catalytic-performance electrolytic water oxygen evolution catalyst.
Example 3
The preparation method of the nickel-iron material with the monodisperse nano-particle structure comprises the following steps:
1) 1.6mmol of NiCl2·6H2O、0.4mmol FeCl2·4H2O and 200mg PVP are dissolved in 14ml of ethylene glycol and uniformly dispersed by ultrasonic to obtain a mixed solution.
2) Transferring the mixed solution obtained in the step 1) into a pressure-resistant reaction tube, reacting at 180 ℃ for 10h, taking out the pressure-resistant reaction tube after the reaction is finished, and naturally cooling to room temperature to obtain a reaction solution.
3) Adding 25ml of acetone and 10ml of ethanol into the reaction solution taken out in the step 2), and performing centrifugal washing.
4) Ultrasonically dispersing the washed product in the step 3) and 42.1593mg of EC300JD carbon black respectively, and mixing and stirring to obtain a mixture.
5) And (3) drying the mixture obtained in the step 4) in vacuum for 12h, introducing oxygen into a tube furnace for roasting under the roasting condition that the heating rate is 2 ℃/min, and roasting at 400 ℃ for 1h to prepare the monodisperse nano-particle structure ferronickel material.
The catalytic oxygen evolution performance of the electrolyzed water in the embodiment is measured by a CHI760E workstation, a three-electrode test system is formed by adopting an oxygen evolution electrode as a working electrode, a carbon rod and a saturated calomel electrode, and the sweep rate is 5mV/s in 1mol/L potassium hydroxide solution.
The monodisperse nanoparticle structure ferronickel material prepared by the embodiment is at 10mA/cm2At current density, the overpotential can reach 279 mV. The nickel-iron material with the monodisperse nano-particle structure has excellent catalytic activity and stability when being used as an oxygen evolution electrode, and is a potential application material of a high-catalytic-performance electrolytic water oxygen evolution catalyst.
Example 4
The preparation method of the nickel-iron material with the monodisperse nano-particle structure comprises the following steps:
1) 1.0mmol of NiCl2·6H2O、1.0mmol FeCl2·4H2O and 200mg PVP are dissolved in 14ml of ethylene glycol and uniformly dispersed by ultrasonic to obtain a mixed solution.
2) Transferring the solution obtained in the step 1) into a pressure-resistant reaction tube, reacting at 180 ℃ for 10h, taking out the pressure-resistant reaction tube after the reaction is finished, and naturally cooling to room temperature to obtain a reaction solution.
3) Adding 25ml of acetone and 10ml of ethanol into the reaction solution taken out in the step 2), and performing centrifugal washing.
4) Ultrasonically dispersing the washed product in the step 3) and 84.6166mg of EC300JD carbon black respectively, and mixing and stirring to obtain a mixture.
5) And (3) drying the mixture obtained in the step 4) in vacuum for 12h, introducing oxygen into a tube furnace for roasting under the roasting condition that the heating rate is 2 ℃/min, and roasting at 300 ℃ for 1h to prepare the monodisperse nano-particle structure ferronickel material.
The catalytic oxygen evolution performance of the electrolyzed water in the embodiment is measured by a CHI760E workstation, a three-electrode test system is formed by adopting an oxygen evolution electrode as a working electrode, a carbon rod and a saturated calomel electrode, and the sweep rate is 5mV/s in 1mol/L potassium hydroxide solution.
The monodisperse nanoparticle structure ferronickel material prepared by the embodiment is at 10mA/cm2Under the current density, the overpotential can reach 239 mV. The nickel-iron material with the monodisperse nano-particle structure has excellent catalytic activity and stability when being used as an oxygen evolution electrode, and is a potential application material of a high-catalytic-performance electrolytic water oxygen evolution catalyst.
Example 5
The preparation method of the nickel-iron material with the monodisperse nano-particle structure comprises the following steps:
1) 1.6mmol of NiCl2·6H2O、0.4mmol FeCl2·4H2O and 200mg PVP are dissolved in 14ml of ethylene glycol and uniformly dispersed by ultrasonic to obtain a mixed solution.
2) Transferring the mixed solution obtained in the step 1) into a pressure-resistant reaction tube, reacting at 180 ℃ for 10h, taking out the pressure-resistant reaction tube after the reaction is finished, and naturally cooling to room temperature to obtain a reaction solution.
3) Adding 25ml of acetone and 10ml of ethanol into the reaction solution taken out in the step 2), and performing centrifugal washing.
4) Ultrasonically dispersing the product washed in the step 3) and 84.6166mg of VXC-72 carbon black respectively, and mixing and stirring to obtain a mixture.
5) And (3) drying the mixture obtained in the step 4) in vacuum for 12h, introducing oxygen into a tube furnace for roasting under the roasting condition that the heating rate is 2 ℃/min, and roasting at 300 ℃ for 1h to prepare the monodisperse nano-particle structure ferronickel material.
The catalytic oxygen evolution performance of the electrolyzed water in the embodiment is measured by a CHI760E workstation, a three-electrode test system is formed by adopting an oxygen evolution electrode as a working electrode, a carbon rod and a saturated calomel electrode, and the sweep rate is 5mV/s in 1mol/L potassium hydroxide solution.
The monodisperse nanoparticle structure ferronickel material prepared by the embodiment is at 10mA/cm2At current density, over-potential196mV can be reached. The nickel-iron material with the monodisperse nano-particle structure has excellent catalytic activity and stability when being used as an oxygen evolution electrode, and is a potential application material of a high-catalytic-performance electrolytic water oxygen evolution catalyst.
Claims (7)
1. A preparation method of a monodisperse ferronickel nano material for oxygen evolution by electrolysis of water is characterized by comprising the following steps:
(1) selecting nickel chloride hexahydrate, ferrous chloride tetrahydrate, polyvinylpyrrolidone and ethylene glycol as raw materials, dissolving the nickel chloride hexahydrate, the ferrous chloride tetrahydrate and the polyvinylpyrrolidone in the ethylene glycol, and performing ultrasonic dispersion uniformly to obtain a mixed solution;
(2) transferring the mixed solution obtained in the step (1) into a pressure-resistant reaction tube, reacting for 10-13h at 180 ℃, then taking out the pressure-resistant reaction tube, and naturally cooling to room temperature;
(3) taking out the reaction liquid obtained in the step (2), adding acetone and ethanol, and centrifuging and washing for multiple times;
(4) mixing the product obtained after centrifugal washing in the step (3) with carbon black to obtain a mixture;
(5) and (4) drying the mixture obtained in the step (4) in vacuum, then placing the dried mixture in a tubular furnace, introducing oxygen and roasting to prepare the monodisperse nickel-iron nano material for electrolytic water oxygen evolution.
2. The preparation method of the monodisperse ferronickel nano-material for oxygen evolution by electrolysis of water according to claim 1 is characterized in that: the molar ratio of the nickel chloride hexahydrate to the ferrous chloride tetrahydrate is 1-1.6: 0.4-1.
3. The preparation method of the monodisperse ferronickel nano-material for oxygen evolution by electrolysis of water according to claim 1 is characterized in that: the dosage ratio of the nickel chloride hexahydrate, the polyvinylpyrrolidone and the glycol is 1-1.6:0.4-1: 1-2.
4. The preparation method of the monodisperse ferronickel nano-material for oxygen evolution by electrolysis of water according to claim 1 is characterized in that: the dosage ratio of the nickel chloride hexahydrate to the carbon black is 1-1.6mmol:42-85 mg.
5. The preparation method of the monodisperse ferronickel nano-material for oxygen evolution by electrolysis of water according to claim 1 is characterized in that: the carbon black is any one type of carbon black selected from VXC-72, EC600JD and EC300 JD.
6. The preparation method of the monodisperse ferronickel nano material for electrolytic water oxygen evolution according to claim 1 is characterized in that the roasting reaction conditions are as follows: controlling the heating rate at 2 ℃/min, heating to 300-400 ℃ and roasting for 1 h.
7. The preparation method of the monodisperse ferronickel nano-material for oxygen evolution by electrolysis of water according to claim 1 is characterized in that: the particle size of the monodisperse nickel-iron nano material for electrolyzing water to separate oxygen is below 10 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210031658.3A CN114232024B (en) | 2022-01-12 | 2022-01-12 | Preparation method of monodisperse ferronickel nanomaterial for oxygen evolution of electrolyzed water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210031658.3A CN114232024B (en) | 2022-01-12 | 2022-01-12 | Preparation method of monodisperse ferronickel nanomaterial for oxygen evolution of electrolyzed water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
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| CN115261926A (en) * | 2022-09-27 | 2022-11-01 | 邢台职业技术学院 | AEM electrolyzed water metal catalyst, and preparation method and application thereof |
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| CN109201060A (en) * | 2018-10-18 | 2019-01-15 | 北京理工大学 | A kind of preparation method of the compound oxygen-separating catalyst of nickel foam-iron-doped nickel oxide |
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| CN109201060A (en) * | 2018-10-18 | 2019-01-15 | 北京理工大学 | A kind of preparation method of the compound oxygen-separating catalyst of nickel foam-iron-doped nickel oxide |
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| CN115261926A (en) * | 2022-09-27 | 2022-11-01 | 邢台职业技术学院 | AEM electrolyzed water metal catalyst, and preparation method and application thereof |
| CN115261926B (en) * | 2022-09-27 | 2023-01-13 | 邢台职业技术学院 | AEM electrolyzed water metal catalyst, and preparation method and application thereof |
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