CN113582241A - Electrocatalytic material echinoid Co for ENRR3O4Preparation method of (1) - Google Patents
Electrocatalytic material echinoid Co for ENRR3O4Preparation method of (1) Download PDFInfo
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- CN113582241A CN113582241A CN202110828332.9A CN202110828332A CN113582241A CN 113582241 A CN113582241 A CN 113582241A CN 202110828332 A CN202110828332 A CN 202110828332A CN 113582241 A CN113582241 A CN 113582241A
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- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 title claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 230000009467 reduction Effects 0.000 claims description 13
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 8
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 8
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 241000257465 Echinoidea Species 0.000 claims 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 abstract description 20
- 238000001035 drying Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 238000009620 Haber process Methods 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- 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
- C25B1/27—Ammonia
-
- 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
- C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
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- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
Electrocatalytic material echinoid Co for ENRR3O4Belonging to the field of electrocatalysis nitrogen fixation. Comprises the steps of mechanically mixing precursors, centrifugally washing solid obtained by hydrothermal, drying in a vacuum drying muffle furnace and calcining to obtain echinoid Co3O4. The invention is mainly used for preparing echinoid Co3O4The electrocatalytic nitrogen fixation material solves the problem of spherical Co3O4The method is used for solving the problem of poor ENRR performance.
Description
Technical Field
The invention belongs to the field of ammonia production by electrocatalytic reduction of nitrogen, and particularly discloses an electrocatalytic material echinoid Co for ENRR3O4Preparation method of (1)
Background
The pressing energy and environmental crisis is driving the development of sustainable platforms to produce naturally abundant and efficient future energy carrier systems. Ammonia (NH)3) As a widely produced chemical in the agricultural, medical and textile industriesHas wide application. However, NH on an industrial scale3The synthesis still relies heavily on the energy intensive Haber-Bosch process under severe conditions, the electrochemical nitrogen reduction (NRR) is a process for the generation of NH from atmospheric nitrogen and water3The new technique of (1). However, this process must be driven by a highly active catalyst to reduce the high energy barrier to cracking the inert nitrogen-nitrogen triple bonds. Noble metal-based (Au, Rh, Pd, etc.) materials have established benchmark behavior as NRR catalysts so far, but their practical application is greatly hindered due to low reserves and high cost. Therefore, the development of potential, abundant, active and efficient non-noble metal substitutes is urgent.
Transition Metal Oxides (TMOs) have the characteristics of adjustable activity, simple and convenient synthesis, environmental friendliness and the like, and become competitive candidate materials for fixing nitrogen by electrochemistry. Wherein Co3O4Recently, the electrocatalytic material has attracted much research interest as an electrocatalytic material having excellent performance and low price. However, spherical Co3O4The ammonia yield is limited due to the few active sites.
In the electrocatalytic nitrogen reduction, to further increase Co3O4The ammonia yield of the material as an electrocatalyst, we propose a method to promote the electrocatalytic nitrogen reduction performance. By preparing a sea urchin-shaped Co3O4And (3) microspheres. This structure increases the active site pair N2Thereby greatly improving the electrochemical fixation of N2Activity and efficiency of (c). At an optimum potential of-0.3V vs. RHE, the sea urchin-like Co3O4The ammonia yield of the microspherical catalyst can reach 49 mu g.h-1·mg-1The Faraday efficiency FE can reach 18.5%.
Disclosure of Invention
The invention aims to provide echinoid Co3O4The microspheres are used for electrocatalytic nitrogen reduction to solve the problem of spherical Co3O4The method is used for solving the problem of poor ENRR performance.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention relates to a cobaltosic oxide nano material for electrocatalytic nitrogen reduction, wherein an electrode material is echinoid Co3O4The particle size of the microspheres is 8-12 μm.
The invention relates to a preparation method of cobaltosic oxide nano material for electrocatalytic nitrogen reduction, wherein a reaction system is an ultrapure water solution, and raw materials comprise cobalt nitrate, ammonium fluoride and urea, and the preparation method comprises the following specific steps:
mixing cobalt nitrate Co (No)3·6H2O, ammonium fluoride NH4F and urea are added into ultrapure water and stirred uniformly to obtain a light purple solution; putting the solution into a high-pressure autoclave, reacting for 12 hours at 120 ℃, centrifugally washing, and vacuum drying at 60 ℃ to obtain a light purple precursor; calcining the precursor in a muffle furnace at 500 ℃ for 2h at the heating rate of 3 min/DEG C to obtain the echinoid Co with the diameter of 8-12 mu m3O4。
The molar ratio of the cobalt nitrate to the ammonium fluoride to the urea is 1:2:5, and each 5mmol of the cobalt nitrate corresponds to 40-60ml of ultrapure water.
The cobaltosic oxide nano material is used for preparing ammonia by electrocatalytic nitrogen reduction, and the test method comprises the following specific steps:
in a typical H-cell, N was performed with Nafion 117 membrane2And (4) carrying out reduction experiments. The electrochemical experiment adopts a three-electrode system, namely the prepared echinoid Co3O4the/CP electrode, the platinum sheet electrode and the Ag/AgCl electrode are used as a working electrode, a counter electrode and a reference electrode and are carried out on a CHI 760E electrochemical analyzer of Shanghai CH Instrument Co. In the experiment, 0.5M LiClO was added4Electrolyte solution is subjected to N2After 30min of purification, N is carried out2And (4) carrying out reduction experiments. In N2Saturated 0.5M LiClO4In solution is subjected to N2And (4) performing electrochemical reduction. After 2 hours of controlled potential electrolysis, the electrolyte in the cathode cell was collected for color development, and the ammonia yield and Faraday Efficiency (FE) were calculated by measuring the absorbance with an ultraviolet spectrophotometer.
NH3Calculation of Generation Rate and Faraday Efficiency (FE)
NH3The generation rate calculation formula of (1) is as follows:
The FE calculation formula is as follows:
FE is Faraday efficiency, unit is%; f is the Faraday constant and has a value of 96500C mol-1(ii) a Q is the total charge consumption of the electrolysis process and is given in C.
Drawings
FIG. 1 shows the prepared sea urchin-shaped Co3O4SEM and TEM images of the microspheres;
FIG. 2 is a schematic structural view of an H-type electrolytic cell;
FIG. 3 shows NH at different potentials3Yield (a) and faraday efficiency (b);
fig. 4 shows the cycle stability for 5 cycles. (a) NH (NH)3Yield, (b) faradaic efficiency.
Detailed Description
The above description is only an example of the present invention and the general knowledge of the specific tests and the like known in the schemes is not described herein too much. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent.
Example 1
5mmol cobalt nitrate Co (No)3·6H2O, 10mmol ammonium fluoride NH4F and 25mmol of urea are added into 50mL of ultrapure water, the magnetic stirring time is 1h, and a dark purple turbid solution is obtained. The solution was placed in an autoclave and reacted at 120 ℃ for 12 hours. Centrifugally washing, and vacuum drying at 60 ℃ to obtain a light purple precursor. Calcining the precursor in a muffle furnace at 500 ℃ for 2h at the heating rate of 3 min/DEG C to obtain the echinoid Co with the diameter of 8-12 mu m3O4。
Prepared echinoid Co3O4SEM and TEM images of the microspheres are shown in FIG. 1; the structural schematic diagram of the H-shaped electrolytic cell for preparing ammonia by electrocatalysis nitrogen reduction is shown in figure 2; NH at different potentials3The yield and faraday efficiency are shown in figure 3; the cycling stability for 5 cycles is shown in figure 4 (each cycle corresponds to changing the same electrolyte once).
Claims (4)
1. Electrocatalytic material echinoid Co for ENRR3O4The preparation method is characterized by comprising the following steps: mixing cobalt nitrate Co (No)3·6H2O, ammonium fluoride NH4F and urea are added into ultrapure water and stirred uniformly to obtain a light purple solution; putting the solution into a high-pressure autoclave, reacting for 12 hours at 120 ℃, centrifugally washing, and vacuum drying at 60 ℃ to obtain a light purple precursor; calcining the precursor in a muffle furnace at 500 ℃ for 2h at the heating rate of 3 min/DEG C to obtain the echinoid Co with the diameter of 8-12 mu m3O4。
2. The method according to claim 1, wherein the molar ratio of cobalt nitrate, ammonium fluoride and urea is 1:2:5, and 40-60ml of ultrapure water is used per 5mmol of cobalt nitrate.
3. Co prepared according to the method of claim 1 or 23O4Is sea urchin shaped and has a diameter of 8-12 μm.
4. Prepared by the process of claim 1 or 2Co3O4The application of (1) in preparing ammonia by electrocatalytic nitrogen reduction.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110828332.9A CN113582241A (en) | 2021-07-21 | 2021-07-21 | Electrocatalytic material echinoid Co for ENRR3O4Preparation method of (1) |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114702080A (en) * | 2022-03-17 | 2022-07-05 | 宜昌邦普时代新能源有限公司 | Preparation method and application of sea urchin-shaped lithium cobalt oxide |
| CN115057479A (en) * | 2022-06-26 | 2022-09-16 | 北京化工大学 | CoAl 2 O 4 Preparation method of electrocatalytic material and application of ENRR thereof |
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| CN105084427A (en) * | 2014-05-19 | 2015-11-25 | 中国科学院过程工程研究所 | In-situ grown three-dimensional multi-structural cobaltosic oxide micro-nanomaterial, controllable preparation and application thereof |
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| CN108346521A (en) * | 2018-01-08 | 2018-07-31 | 华南师范大学 | The preparation method of foamed nickel supported sea urchin shape cobalt acid copper nano material |
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2021
- 2021-07-21 CN CN202110828332.9A patent/CN113582241A/en active Pending
Patent Citations (5)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114702080A (en) * | 2022-03-17 | 2022-07-05 | 宜昌邦普时代新能源有限公司 | Preparation method and application of sea urchin-shaped lithium cobalt oxide |
| WO2023173778A1 (en) * | 2022-03-17 | 2023-09-21 | 宜昌邦普时代新能源有限公司 | Preparation method for sea urchin-like lithium cobaltate and application of sea urchin-like lithium cobaltate |
| CN115057479A (en) * | 2022-06-26 | 2022-09-16 | 北京化工大学 | CoAl 2 O 4 Preparation method of electrocatalytic material and application of ENRR thereof |
| CN115057479B (en) * | 2022-06-26 | 2024-03-26 | 北京化工大学 | CoAl (cobalt aluminum alloy) 2 O 4 Preparation method of electrocatalytic material and application of ENRR thereof |
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