CN113594480A - Heteroatom-codoped non-noble metal-based carbon material and preparation method and application thereof - Google Patents
Heteroatom-codoped non-noble metal-based carbon material and preparation method and application thereof Download PDFInfo
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 34
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229920005610 lignin Polymers 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 229910052742 iron Inorganic materials 0.000 claims abstract description 18
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 13
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 12
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 229920005552 sodium lignosulfonate Polymers 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000000197 pyrolysis Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 7
- 125000005842 heteroatom Chemical group 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 2
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 abstract description 18
- 239000001301 oxygen Substances 0.000 abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 9
- 230000009467 reduction Effects 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000006872 improvement Effects 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 238000011161 development Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000010411 electrocatalyst Substances 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 229940021013 electrolyte solution Drugs 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention belongs to the technical field of catalysts, and particularly relates to a heteroatom-codoped non-noble metal-based carbon material, and a preparation method and application thereof. The material is prepared by the following method: ultrasonically dispersing ferric chloride in ethanol uniformly, adding sodium lignosulfonate, stirring, drying and washing to obtain iron chelated lignin; grinding sodium hypophosphite and iron chelated lignin uniformly, and carrying out pyrolysis reaction to obtain the iron chelated lignin. The preparation method of the invention integrates the active sites of Fe-N-C, FeP, realizes the electrocatalytic oxygen reduction, hydrogen evolution and oxygen evolution reaction simultaneously by utilizing the synergistic effect of the two, and realizes the remarkable improvement of the catalytic activity and stability. The invention combines iron chelated lignin and sodium hypophosphite by using a salt auxiliary strategy to prepare the three-functional non-noble metal-based carbon material capable of catalyzing oxygen reduction, hydrogen evolution and oxygen evolution reactions simultaneously, and solves the problems of high cost and low reserve of noble metal catalysts in the prior art.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a heteroatom-codoped non-noble metal-based carbon material, and a preparation method and application thereof.
Background
The continuous activation and sustainable development of the current energy problem are urgent, so that the development of novel energy conversion devices such as metal-air batteries and proton exchange membrane fuel cells becomes a research hotspot. The electrocatalysis material is used as a key material of the fuel cell, and the development of the low-cost and high-performance three-function electrocatalyst which can be simultaneously applied to catalytic oxygen reduction, hydrogen evolution and oxygen evolution reactions has important significance for energy conversion devices and the like. However, due to the problem of slow reaction kinetics, only low-inventory, high-price noble metal catalysts are currently used as commercial catalysts, thereby limiting the application of commercial fuel cells. Therefore, the development of low-cost and high-performance non-noble metal electrocatalytic materials is a goal of researchers.
In the development process of non-noble metal electrocatalysts, carbon materials have attracted extensive attention due to their high cost performance, good conductivity, high specific surface area, and good stability. The three-function catalyst can not only avoid side reactions caused by the interaction of various catalysts, but also simplify the design and structure of the electrode. The performance in electrocatalytic oxygen reduction, hydrogen evolution and oxygen evolution reactions has a significant impact on carbon materials. Therefore, the development of a three-functional carbon-based electrocatalyst with high performance for the three key reactions is of great significance. Therefore, the heteroatom-codoped non-noble metal-based carbon material with high activity and high stability, which is simultaneously applied to electrocatalytic oxygen reduction, hydrogen evolution and oxygen evolution reactions, is developed, so that the wide application of the non-noble metal electrocatalyst in the commercial fuel cell is realized, and the method has wide economic benefits and social benefits and has important significance.
Disclosure of Invention
In order to obtain a heteroatom-codoped non-noble metal-based carbon material with high activity and high stability, which is simultaneously applied to electrocatalytic oxygen reduction, hydrogen evolution and oxygen evolution reactions, the invention provides a heteroatom-codoped non-noble metal-based carbon material, and the material realizes three-function electrocatalytic performance.
The invention also aims to provide a preparation method of the heteroatom-codoped non-noble metal-based carbon material, which is simple to operate and solves the problems of high cost and low storage capacity of the noble metal catalyst in the prior art.
The invention also aims to provide application of the heteroatom-codoped non-noble metal-based carbon material in electrocatalytic oxygen reduction, hydrogen evolution and oxygen evolution reactions, and the material has excellent electrocatalytic performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a preparation method of a heteroatom-codoped non-noble metal-based carbon material, which comprises the following steps:
(1) ultrasonically dispersing ferric chloride in ethanol uniformly, adding sodium lignosulfonate, stirring, drying and washing to obtain iron chelated lignin;
(2) uniformly grinding sodium hypophosphite and iron chelated lignin, and carrying out pyrolysis reaction to obtain the heteroatom co-doped non-noble metal-based carbon material.
Further, in the step (1), the concentration of the ferric chloride in the ethanol is 0.025-0.1 g/mL; the mass ratio of the ferric chloride to the sodium lignin sulfonate is 1-3: 1-3.
Further, in the step (1), the power of the ultrasonic wave is 220-; the drying is carried out at 70-90 ℃ for 20-24 h.
Further, in the step (2), the mass ratio of the sodium hypophosphite to the sodium lignosulfonate is 1-3: 0.1.
Further, in the step (2), the sodium hypophosphite is added and then dissolved, and ultrasonic treatment is adopted, wherein the ultrasonic power is 220-280W, and the ultrasonic time is 10-20 min.
The pyrolysis reaction conditions provided by the invention are as follows: raising the temperature to 850-plus-one 950 ℃ at the temperature raising rate of 5 ℃/min for 2.5-3.5h under the nitrogen atmosphere, reducing the temperature, carrying out acid cleaning for 22-26h by using 1.5-2.5M HCl solution at the temperature of 85-95 ℃, then maintaining for 0.5-1.5h at the temperature of 750-plus-one 850 ℃ under the ammonia atmosphere, and reducing the temperature to finally obtain the heteroatom-codoped non-noble metal-based carbon material.
The invention provides a heteroatom-codoped non-noble metal-based carbon material prepared by the preparation method.
The invention also provides application of the heteroatom-codoped non-noble metal-based carbon material in the field of electrocatalysis.
The invention has the beneficial effects that:
(1) the preparation method of the invention integrates the active sites of Fe-N-C, FeP, realizes the electrocatalytic oxygen reduction, hydrogen evolution and oxygen evolution reaction simultaneously by utilizing the synergistic effect of the two, and realizes the remarkable improvement of the catalytic activity and stability.
(2) The invention combines iron chelated lignin and sodium hypophosphite by using a salt auxiliary strategy to prepare the three-functional non-noble metal-based carbon material capable of catalyzing oxygen reduction, hydrogen evolution and oxygen evolution reactions simultaneously, and solves the problems of high cost and low reserve of noble metal catalysts in the prior art.
Drawings
Fig. 1 is a scanning electron microscope image of the non-metal-based carbon material prepared in example 1.
FIG. 2 shows ORR (a), OER (b), 0.5M H of examples 1 to 32SO4Linear scan polarization plots of HER at 1M KOH and HER (c).
FIG. 3 is an ORR (a), OER (b), 0.5M H of example 1, comparative examples 1-22SO4Linear scan polarization plots of HER at 1M KOH and HER (c).
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings, in order that the present disclosure may be more fully understood and fully conveyed to those skilled in the art. While the exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the invention is not limited to the embodiments set forth herein.
Example 1
(1) Adding 1.4g of ferric chloride into 20mL of ethanol, performing ultrasonic treatment for 10min under the condition that the power is 280W, uniformly dispersing, adding 2g of sodium lignosulfonate, stirring, drying for 24h at 80 ℃, and washing to obtain iron chelated lignin;
(2) grinding 1.5g of sodium hypophosphite and 0.1g of iron chelated lignin uniformly, heating to 800 ℃ at a heating rate of 5 ℃/min for 2h in a nitrogen atmosphere, cooling, carrying out acid washing with 2M HCl solution at 90 ℃ for 24h, then keeping at 800 ℃ for 1h in an ammonia atmosphere, and cooling to finally obtain the heteroatom co-doped non-noble metal based carbon material.
Scanning electron microscopy of the heteroatom-co-doped non-noble metal-based carbon material prepared in this example is shown in fig. 1, and the results show that the material contains a large number of pores with a diameter of 1 μm, which may be due to the removal of sodium hypophosphite at high temperature, and the porous structure is beneficial to the electrocatalytic performance of the material.
Example 2
(1) Adding 1.4g of ferric chloride into 20mL of ethanol, performing ultrasonic treatment for 10min under the condition that the power is 280W, uniformly dispersing, adding 2g of sodium lignosulfonate, stirring, drying for 24h at 80 ℃, and washing to obtain iron chelated lignin;
(2) grinding 1.0g of sodium hypophosphite and 0.1g of iron chelated lignin uniformly, heating to 800 ℃ at a heating rate of 5 ℃/min for 2h in a nitrogen atmosphere, cooling, carrying out acid washing with 2M HCl solution at 90 ℃ for 24h, then keeping at 800 ℃ for 1h in an ammonia atmosphere, and cooling to finally obtain the heteroatom co-doped non-noble metal based carbon material.
Example 3
(1) Adding 1.4g of ferric chloride into 20mL of ethanol, performing ultrasonic treatment for 10min under the condition that the power is 280W, uniformly dispersing, adding 2g of sodium lignosulfonate, stirring, drying for 24h at 80 ℃, and washing to obtain iron chelated lignin;
(2) grinding 2.0g of sodium hypophosphite and 0.1g of iron chelated lignin uniformly, heating to 800 ℃ at a heating rate of 5 ℃/min for 2h in a nitrogen atmosphere, cooling, carrying out acid washing with 2M HCl solution at 90 ℃ for 24h, then keeping at 800 ℃ for 1h in an ammonia atmosphere, and cooling to finally obtain the heteroatom co-doped non-noble metal based carbon material.
Comparative example 1
(1) Adding 1.4g of ferric chloride into 20mL of ethanol, performing ultrasonic treatment for 10min under the condition that the power is 280W, uniformly dispersing, adding 2g of sodium lignosulfonate, stirring, drying for 24h at 80 ℃, and washing to obtain iron chelated lignin;
(2) raising the temperature of 0.1g of iron-chelated lignin to 800 ℃ at a heating rate of 5 ℃/min for 2h in a nitrogen atmosphere, cooling, carrying out acid washing with 2M HCl solution at 90 ℃ for 24h, then maintaining at 800 ℃ for 1h in an ammonia atmosphere, and cooling to finally obtain the heteroatom-codoped non-noble metal-based carbon material.
Comparative example 2
(1) Adding 1.4g of ferric chloride into 20mL of ethanol, performing ultrasonic treatment for 10min under the condition that the power is 280W, uniformly dispersing, adding 2g of sodium lignosulfonate, stirring, drying for 24h at 80 ℃, and washing to obtain iron chelated lignin;
(2) grinding 1.5g of sodium hypophosphite and 0.1g of iron chelated lignin uniformly, heating to 800 ℃ at a heating rate of 5 ℃/min for 2h in a nitrogen atmosphere, cooling, carrying out acid washing with 2M HCl solution at 90 ℃ for 24h, then keeping at 750 ℃ for 1h in an ammonia atmosphere, and cooling to finally obtain the heteroatom co-doped non-noble metal based carbon material.
Effects of the embodiment
ORR, OER and HER electrocatalytic performance tests were performed on examples 1,2, 3 and comparative examples 1,2 using a three-electrode test system in electrolyte solutions of 0.1M KOH, 1M KOH, 0.5M H2SO4 and 1M KOH, respectively, via Chenghua CHI760E electrochemical workstation.
(one) ORR (FIG. 2a), OER (FIG. 2b), 0.5M H by examples 1-32SO4The linear scanning polarization curves of the lower HER (fig. 2 c) and the HER (fig. 2 d) under 1M KOH show that example 1 shows higher catalytic activity, indicating that the amount of sodium hypophosphite has a significant effect on the catalytic performance of the material.
(II) ORR (FIG. 3a), OER (FIG. 3b), 0.5M H by example 1 and comparative examples 1,22SO4The linear scanning polarization curves of the lower HER (FIG. 3 c) and the HER (FIG. 3 d) under 1M KOH show that example 1 still shows the optimal catalytic activity, which indicates that the doping of phosphorus element and the pyrolysis temperature of 800 ℃ have better performance on the materialStrong influence effect.
Claims (8)
1. A preparation method of a heteroatom-codoped non-noble metal-based carbon material is characterized by comprising the following steps:
(1) ultrasonically dispersing ferric chloride in ethanol uniformly, adding sodium lignosulfonate, stirring, drying and washing to obtain iron chelated lignin;
(2) uniformly grinding sodium hypophosphite and iron chelated lignin, and carrying out pyrolysis reaction to obtain the heteroatom co-doped non-noble metal-based carbon material.
2. The method according to claim 1, wherein in the step (1), the concentration of the ferric chloride in the ethanol is 0.025 to 0.1 g/mL; the mass ratio of the ferric chloride to the sodium lignin sulfonate is 1-3: 1-3.
3. The preparation method according to claim 1 or 2, wherein in the step (1), the power of the ultrasound is 220- & 280W, and the ultrasound time is 10-20 min; the drying is carried out at 70-90 ℃ for 20-24 h.
4. The preparation method according to claim 1, wherein in the step (2), the mass ratio of the sodium hypophosphite to the sodium lignosulfonate is 1-3: 0.1.
5. The preparation method according to claim 1, wherein in the step (2), the sodium hypophosphite is added and then dissolved, and ultrasonic treatment is adopted, wherein the power of ultrasonic treatment is 220-280W, and the ultrasonic time is 10-20 min.
6. The method according to claim 1, 4 or 5, wherein in the step (2), the pyrolysis is performed under the following reaction conditions: raising the temperature to 850-plus-one 950 ℃ at the temperature raising rate of 5 ℃/min for 2.5-3.5h under the nitrogen atmosphere, reducing the temperature, carrying out acid cleaning for 22-26h by using 1.5-2.5M HCl solution at the temperature of 85-95 ℃, then maintaining for 0.5-1.5h at the temperature of 750-plus-one 850 ℃ under the ammonia atmosphere, and reducing the temperature to finally obtain the heteroatom-codoped non-noble metal-based carbon material.
7. A heteroatom-codoped non-noble metal-based carbon material prepared by the preparation method as set forth in any one of claims 1 to 6.
8. Use of the heteroatom co-doped non-noble metal-based carbon material according to claim 7 in the field of electrocatalysis.
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| CN115064717A (en) * | 2022-07-12 | 2022-09-16 | 郑州大学 | ORR-OER catalyst for zinc-air battery anode and preparation method thereof |
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