CN114464822A - Oxygen reduction catalyst and preparation method and application thereof - Google Patents
Oxygen reduction catalyst and preparation method and application thereof Download PDFInfo
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- CN114464822A CN114464822A CN202210063132.3A CN202210063132A CN114464822A CN 114464822 A CN114464822 A CN 114464822A CN 202210063132 A CN202210063132 A CN 202210063132A CN 114464822 A CN114464822 A CN 114464822A
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Abstract
The invention belongs to the field of energy catalysts, and discloses an oxygen reduction catalyst, and a preparation method and application thereof. The oxygen reduction catalyst has a porous structure, the oxygen reduction catalyst comprising C, N, O, P, Fe, the total mass fraction of N, O, P and Fe in the oxygen reduction catalyst being less than 14%. The oxygen reduction catalyst has excellent oxygen reduction performance, and the half-wave potential of oxygen reduction under the condition of alkaline electrolyte can exceed 0.87V, and the half-wave potential of oxygen reduction under the condition of acidic electrolyte can exceed 0.76V. The oxygen reduction catalyst does not contain noble metal, so that the preparation cost is low, and the catalytic activity of the oxygen reduction catalyst is equivalent to that of the noble metal catalyst. The preparation process of the oxygen reduction catalyst does not need to use a template, simplifies the preparation process and is very suitable for industrial mass production.
Description
Technical Field
The invention belongs to the field of energy catalysts, and particularly relates to an oxygen reduction catalyst, and a preparation method and application thereof.
Background
At present, the human society faces two problems of energy shortage and environmental deterioration, and increasing the proportion of renewable energy in a novel energy system is very important. The volatility of renewable energy sources makes it necessary to use electrochemical energy storage and electrochemical energy conversion devices in a matching manner, and the oxygen reduction reaction is a core process in various electrochemical energy storage and electrochemical energy conversion devices. Therefore, a catalyst that catalyzes rapid reduction of oxygen has attracted attention. At present, clean green batteries such as fuel cells and metal-air batteries, which comprise an oxygen reduction reaction, generally use noble metal-based catalysts (such as Pt-containing catalysts), which limits the large-scale development and application of noble metal-based catalysts due to the low content of noble metals on earth and the high preparation cost. Therefore, it has become a hot direction in the field to reduce the preparation cost of the catalyst by using the catalyst without containing the noble metal on the premise of securing the catalytic performance.
There has been no or very little prior art that uses no noble metal to prepare the catalyst and the catalytic performance obtained is comparable to that of noble metal-based catalysts (e.g., Pt-containing catalysts) in oxygen reduction reactions. In addition, the catalyst in the prior art usually needs to use a template, the preparation process is relatively complex, the production cost is increased, and the industrialization of the catalyst is not facilitated.
Therefore, there is a need to provide a new catalyst having good catalytic activity without using a noble metal.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides an oxygen reduction catalyst, and a preparation method and application thereof. The oxygen reduction catalyst does not contain noble metal, so that the preparation cost is low, and the catalytic activity of the oxygen reduction catalyst is equivalent to or even exceeds the catalytic performance of the noble metal catalyst. In addition, a template is not needed in the preparation process of the oxygen reduction catalyst, so that the preparation process of the oxygen reduction catalyst is greatly simplified, and the industrial production of the oxygen reduction catalyst is facilitated.
The invention conception of the invention is as follows: according to the invention, based on a coordination polymer formed by coordinating polyvinyl imidazole with zinc nitrate or zinc nitrate hexahydrate, an iron source and a phosphorus source are introduced to obtain a doped precursor, then the doped precursor is carbonized, in the carbonization process, zinc with a low boiling point volatilizes outwards to generate a large number of micropores, the position of the zinc inwards substituted by iron is coordinated with nitrogen, and a large number of nano holes with different apertures are generated due to the Cokendall effect, so that the prepared oxygen reduction catalyst has a high specific surface area, and the exposure degree of active sites in the oxygen reduction catalyst is improved. In addition, the invention obtains the iron-phosphorus doped hierarchical pore carbon-based oxygen reduction catalyst under the condition of not using a template agent, acid washing and other complex process flows. The preparation process of the oxygen reduction catalyst is quick, simple and convenient, has excellent oxygen reduction catalytic performance under both acidic and alkaline conditions, and is suitable for large-scale popularization and application.
A first aspect of the invention provides an oxygen reduction catalyst.
Specifically, an oxygen reduction catalyst having a porous structure, the oxygen reduction catalyst comprising C, N, O, P, Fe, the total mass fraction of N, O, P and Fe in the oxygen reduction catalyst being less than 14%.
Preferably, the pore diameter in the porous structure of the oxygen reduction catalyst is 5-100 nm; further preferably, the pore size in the porous structure of the oxygen reduction catalyst is 5 to 50 nm. The oxygen reduction catalyst mainly contains mesopores with the aperture of 5-50nm, but a small part of mesopores are mutually communicated, so that pores with more apertures can be formed.
Preferably, the mass fraction of C in the oxygen reduction catalyst is not less than 86%; further preferably, the mass fraction of C in the oxygen reduction catalyst is not less than 92%.
Preferably, the mass fraction of P in the oxygen reduction catalyst is 0.1 to 1.5%; further preferably, the mass fraction of P in the oxygen reduction catalyst is 0.2 to 1.0%.
Preferably, the mass fraction of the Fe in the oxygen reduction catalyst is 0.5 to 2.5%; further preferably, the mass fraction of Fe in the oxygen reduction catalyst is 0.8 to 1.9%.
Preferably, the mass fraction of the O in the oxygen reduction catalyst is 5 to 8%; preferably 6-7%.
Preferably, the mass fraction of the N in the oxygen reduction catalyst is 1.9 to 4%; preferably 2-3.5%.
Preferably, the oxygen reduction catalyst comprises C, N, O, P, Fe, the mass fraction of C in the oxygen reduction catalyst is not less than 86%, the mass fraction of P in the oxygen reduction catalyst is 0.1-1.5%, and the mass fraction of Fe in the oxygen reduction catalyst is 0.5-2.5%; the pore diameter in the porous structure of the oxygen reduction catalyst is 5-100 nm.
The oxygen reduction catalyst has a hierarchical pore structure (mainly mesoporous with the aperture of 5-50 nm) and rich iron-phosphorus-nitrogen active sites, and shows good oxygen reduction activity.
A second aspect of the present invention provides a method for producing the above-described oxygen reduction catalyst.
Specifically, the preparation method of the oxygen reduction catalyst comprises the following steps:
(1) dissolving zinc nitrate hexahydrate or zinc nitrate, an iron source and a phosphorus source in an organic solvent to obtain a solution A for later use;
(2) and (2) adding polyvinyl imidazole into the solution A prepared in the step (1), stirring, performing hydrothermal treatment, centrifuging, drying to obtain a doped precursor, and carbonizing the doped precursor to obtain the oxygen reduction catalyst.
Preferably, in the step (1), the iron source is at least one selected from iron phthalocyanine, iron nitrate and iron chloride.
Preferably, in the step (1), the phosphorus source is at least one selected from triphenylphosphine, sodium dihydrogen phosphate and ammonium dihydrogen phosphate.
Preferably, in the step (1), the molar ratio of zinc nitrate hexahydrate or zinc nitrate, iron source and phosphorus source is (50-80): (10-40): (1-2); further preferably, the molar ratio of zinc nitrate hexahydrate or zinc nitrate, iron source and phosphorus source is (50-80): (10-40): 1.5.
preferably, in step (1), the organic solvent comprises absolute methanol or absolute ethanol.
Preferably, in the step (2), the preparation process of the polyvinylimidazole is as follows: azodiisobutyronitrile is used as an initiator to complete the polymerization reaction of 1-vinyl imidazole in an inert atmosphere to prepare the polyvinyl imidazole.
Preferably, 1-vinylimidazole is used in an amount of 30 to 80 times, preferably 40 to 70 times, the amount of azobisisobutyronitrile used, in parts by mass.
Preferably, the temperature of the polymerization temperature is 50-75 ℃, and the time of the polymerization reaction is 15-30 min; further preferably, the temperature of the polymerization temperature is 55-70 ℃, and the time of the polymerization reaction is 15-30 min.
Preferably, in the step (2), the temperature of the hydrothermal treatment is 65-95 ℃, and the time of the hydrothermal treatment is 18-30 h; further preferably, the temperature of the hydrothermal treatment is 70-95 ℃, and the time of the hydrothermal treatment is 20-30 h.
Preferably, in the step (2), the centrifugation process uses a centrifugation solvent, the centrifugation solvent is selected from one of methanol, ethanol and isopropanol, and the centrifugation times are 4-8 times.
Preferably, in the step (2), the drying temperature is 45-90 ℃, preferably 50-80 ℃.
Preferably, in the step (2), the carbonization treatment is performed under a nitrogen atmosphere.
Preferably, in the step (2), the temperature of the carbonization treatment is 850-; further preferably, the temperature of the carbonization treatment is 907-.
Preferably, during the carbonization treatment, the temperature is increased to the temperature required for the carbonization treatment at a temperature increase rate of 4-7 ℃/min.
A third aspect of the invention provides the use of an oxygen reduction catalyst as described above.
Use of the above oxygen reduction catalyst in an electrochemical energy storage or electrochemical energy conversion device.
An apparatus comprising the above oxygen reduction catalyst.
Preferably, the device comprises a battery.
Further preferably, the battery includes a fuel cell, a metal-air battery.
Compared with the prior art, the invention has the following beneficial effects:
(1) the oxygen reduction catalyst has a porous structure, comprises C, N, O, P, Fe, the total mass fraction of N, O, P and Fe in the oxygen reduction catalyst is less than 14%, and the oxygen reduction catalyst has rich iron-phosphorus-nitrogen active sites, so that the oxygen reduction catalyst shows excellent oxygen reduction performance. The half-wave potential for oxygen reduction under alkaline electrolyte conditions may exceed 0.87V and the half-wave potential for oxygen reduction under acidic electrolyte conditions may exceed 0.76V. The oxygen reduction catalyst does not contain noble metal, not only has low preparation cost, but also has the catalytic activity equivalent to that of the noble metal catalyst.
(2) In the zinc-containing coordination polymer, zinc is volatilized in a large amount in the carbonization process to generate a large amount of micropores, so that the specific surface area of the oxygen reduction catalyst is improved, and the available iron-phosphorus-nitrogen active site density is increased. The doping of the iron-phosphorus heteroatom is matched with the volatilization of zinc, so that a large number of mesopores and pores communicated with the mesopores are generated after the carbonization treatment of the oxygen reduction catalyst, and the mass transfer capacity of the oxygen reduction catalyst is improved.
(3) The high-nitrogen-content polyvinyl imidazole is used as a nitrogen source and a carbon source, triphenylphosphine is used as a phosphorus source, iron phthalocyanine is used as an iron source, and the co-doping of iron and phosphorus can regulate and control the electronic structure of the oxygen reduction catalyst, so that a high-efficiency oxygen reduction active site is obtained, and the catalytic capability of the oxygen reduction catalyst is improved.
(4) The preparation process of the oxygen reduction catalyst does not need to use a template, simplifies the preparation process and is very suitable for industrial mass production.
Drawings
FIG. 1 is an SEM (scanning electron microscope) image of an oxygen-reducing catalyst prepared in example 1 of the present invention;
FIG. 2 is an XRD (X-ray diffraction) pattern of an oxygen-reducing catalyst prepared in example 1 of the present invention;
FIG. 3 is a linear sweep voltammogram for oxygen reduction in a 0.1mol/L KOH solution for oxygen reduction catalysts prepared in examples 1-3 of the present invention;
FIG. 4 shows oxygen reduction catalysts prepared in examples 1-3 of the present invention at 0.1mol/L HClO4Linear sweep voltammograms were reduced by oxygen in solution.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1: preparation of oxygen reduction catalyst
An oxygen reduction catalyst comprising C, N, O, P, Fe, the mass fraction of C in the oxygen reduction catalyst being about 91%, the mass fraction of P in the oxygen reduction catalyst being 0.47%, the mass fraction of Fe in the oxygen reduction catalyst being 0.96%; the pore diameter in the porous structure of the oxygen reduction catalyst is 5-100 nm.
A method of preparing an oxygen reduction catalyst comprising the steps of:
(1) dissolving 0.8g of zinc nitrate hexahydrate, 0.3g of triphenylphosphine and 0.03g of iron phthalocyanine in 40mL of anhydrous methanol to obtain a solution A for later use;
(2) adding polyvinyl imidazole into the solution A prepared in the step (1) (the preparation process of the polyvinyl imidazole comprises the steps of weighing 3.2g of 1-vinyl imidazole and 0.064g of azobisisobutyronitrile, carrying out polymerization reaction for 15min at 60 ℃ under the protection of nitrogen, stirring for 6min, then carrying out hydrothermal treatment in a 100mL hydrothermal reaction kettle at 90 ℃ for 20h, centrifugally washing the product after the hydrothermal treatment for 6 times by using methanol, drying at 70 ℃ in a vacuum drying oven to obtain a doped precursor, then placing the doped precursor in a tubular furnace under the nitrogen atmosphere, the temperature was raised to 907 ℃ at a temperature rise rate of 6 ℃/min, carbonization was carried out for 3 hours, and then cooling was carried out to room temperature (20 ℃), to obtain an oxygen reduction catalyst (denoted as Fe, P/NC-1).
The oxygen reduction catalyst Fe, P/NC-1 prepared in this example was subjected to a three-electrode system oxygen reduction performance test in a 0.1mol/L KOH solution and 0.1mol/L HClO4The half-wave potentials of oxygen reduction in the solution were 0.88V and 0.78V, respectively.
FIG. 1 is an SEM (scanning electron microscope) image of an oxygen-reducing catalyst prepared in example 1 of the present invention; as can be seen from fig. 1, the oxygen reduction catalyst Fe, P/NC-1 prepared in example 1 has a large number of nanopores with different pore diameters (the pore diameters of the oxygen reduction catalyst are mainly mesopores distributed between 5nm and 50nm, and a part of the mesopores are interconnected to form a macropore structure exceeding 50 nm), which is beneficial to improving the electrochemical active area of the oxygen reduction catalyst, increasing the number of accessible active sites in the electrochemical reaction, and accelerating the transmission rate of reactants and products.
FIG. 2 is an XRD (X-ray diffraction) pattern of an oxygen-reducing catalyst prepared in example 1 of the present invention; as can be seen from fig. 2 (the ordinate "Intensity" in fig. 2 represents Intensity, and the abscissa "2 theta (degree)") represents diffraction angle (degree)), the oxygen reduction catalyst Fe, P/NC-1 showed a (002) diffraction peak of carbon only in the vicinity of 25 °, indicating that the catalyst contains no iron-containing nanoparticles, and iron exists in a relatively dispersed form, with a relatively high utilization rate.
Example 2: preparation of oxygen reduction catalyst
An oxygen reduction catalyst comprising C, N, O, P, Fe, the mass fraction of C in the oxygen reduction catalyst being about 91%, the mass fraction of P in the oxygen reduction catalyst being 0.39%, the mass fraction of Fe in the oxygen reduction catalyst being 0.73%; the pore diameter in the porous structure of the oxygen reduction catalyst is 5-100 nm.
A method of preparing an oxygen reduction catalyst comprising the steps of:
(1) dissolving 0.7g of zinc nitrate hexahydrate, 0.25g of triphenylphosphine and 0.025g of iron phthalocyanine in 40mL of anhydrous methanol to obtain a solution A for later use;
(2) adding polyvinyl imidazole into the solution A prepared in the step (1) (the preparation process of the polyvinyl imidazole comprises the steps of weighing 3.0g of 1-vinyl imidazole and 0.07g of azobisisobutyronitrile, carrying out polymerization reaction for 20min at 70 ℃ under the protection of nitrogen, stirring for 5min, then carrying out hydrothermal treatment in a 100mL hydrothermal reaction kettle at 85 ℃ for 24h, centrifugally washing the product after the hydrothermal treatment for 5 times by using methanol, drying at 60 ℃ in a vacuum drying oven to obtain a doped precursor, then placing the doped precursor in a tubular furnace under the nitrogen atmosphere, the temperature was raised to 907 ℃ at a rate of 5 ℃/min, and carbonization was carried out for 3 hours, followed by cooling to room temperature (20 ℃) to obtain an oxygen reduction catalyst (denoted as Fe, P/NC-2).
The oxygen reduction catalyst Fe, P/NC-2 prepared in this example was subjected to a three-electrode system oxygen reduction performance test in a 0.1mol/L KOH solution and 0.1mol/L HClO4The half-wave potentials of oxygen reduction in the solution were 0.86V and 0.76V, respectively.
Example 3: preparation of oxygen reduction catalyst
An oxygen reduction catalyst comprising C, N, O, P, Fe, the mass fraction of C in the oxygen reduction catalyst being about 91%, the mass fraction of P in the oxygen reduction catalyst being 0.62%, and the mass fraction of Fe in the oxygen reduction catalyst being 1.24%; the pore diameter in the porous structure of the oxygen reduction catalyst is 5-100 nm.
A method of preparing an oxygen reduction catalyst comprising the steps of:
(1) dissolving 0.9g of zinc nitrate hexahydrate, 0.35g of triphenylphosphine and 0.035g of iron phthalocyanine in 40mL of anhydrous methanol to obtain a solution A for later use;
(2) adding polyvinyl imidazole into the solution A prepared in the step (1) (the preparation process of the polyvinyl imidazole comprises the steps of weighing 3.5g of 1-vinyl imidazole and 0.08g of azobisisobutyronitrile, carrying out polymerization reaction for 25min at 75 ℃ under the protection of nitrogen gas), stirring for 4min, then carrying out hydrothermal treatment in a 100mL hydrothermal reaction kettle at 75 ℃ for 28h, centrifugally washing the product after the hydrothermal treatment for 8 times by using methanol, drying at 65 ℃ in a vacuum drying oven to obtain a doped precursor, then placing the doped precursor in a tubular furnace under the nitrogen atmosphere, the temperature is raised to 1000 ℃ at the heating rate of 4 ℃/min, carbonization treatment is carried out for 2.5h, and then the temperature is cooled to room temperature (20 ℃) to prepare the oxygen reduction catalyst (marked as Fe, P/NC-3).
The oxygen reduction catalyst Fe, P/NC-3 prepared in this example was subjected to a three-electrode system oxygen reduction performance test in a 0.1mol/L KOH solution and 0.1mol/L HClO4The half-wave potentials of oxygen reduction in the solution were 0.85V and 0.75V, respectively.
FIG. 3 is a linear sweep voltammogram for oxygen reduction in a 0.1mol/L KOH solution for oxygen reduction catalysts prepared in examples 1-3 of the present invention;
FIG. 4 shows oxygen reduction catalysts prepared in examples 1-3 of the present invention at 0.1mol/L HClO4Linear sweep voltammograms were reduced by oxygen in solution.
As can be seen from fig. 3 and 4 (abscissa of fig. 3 to 4 represents oxygen reduction potential), the oxygen reduction activity of the oxygen reduction catalyst prepared in example 1 of the present invention was the highest in both the alkaline solution and the acidic solution, and the half-wave potential of oxygen reduction in the KOH solution of 0.1mol/L was 0.88V, indicating that the oxygen reduction catalyst prepared in example of the present invention has good catalytic performance.
In addition, the half-wave potential of the oxygen reduction of the commercial Pt/C noble metal catalyst in 0.1mol/L KOH solution is about 0.85V, which is lower than that of the oxygen reduction catalyst prepared in the embodiment 1 of the invention, and it can be seen that the oxygen reduction catalytic performance of the oxygen reduction catalyst prepared in the invention is equivalent to that of the commercial Pt/C noble metal catalyst, and under the alkaline condition, the oxygen reduction catalytic performance of the oxygen reduction catalyst prepared in the invention is even better than that of the commercial Pt/C noble metal catalyst.
In addition, the diffraction peaks and surface characteristics of the oxygen reduction catalysts obtained in examples 2 to 3 of the present invention were similar to those of example 1, and thus, the details thereof are not repeated.
Application example
A battery comprising the oxygen reduction catalyst prepared in example 1.
Comparative example 1
In comparison with example 1, zinc nitrate hexahydrate in comparative example 1 was replaced with zinc chloride, resulting in failure to produce an oxygen reduction catalyst. Therefore, the preparation method of the oxygen reduction catalyst has selectivity to the zinc salt in the preparation process.
It should be noted that, within the scope of the claimed invention, the technical solution is changed, for example, other phosphorus sources and iron sources are selected, and the oxygen reduction catalyst finally prepared has an oxygen reduction potential similar to that of the oxygen reduction catalyst prepared in example 1.
Claims (10)
1. An oxygen reduction catalyst, characterized in that the oxygen reduction catalyst has a porous structure, the oxygen reduction catalyst comprises C, N, O, P, Fe, and the total mass fraction of N, O, P and Fe in the oxygen reduction catalyst is less than 14%.
2. The oxygen-reducing catalyst according to claim 1, wherein the pore size of the porous structure of the oxygen-reducing catalyst is 5 to 100 nm.
3. The oxygen-reducing catalyst according to claim 1, wherein the mass fraction of C in the oxygen-reducing catalyst is not less than 86%.
4. The oxygen-reducing catalyst according to claim 1, wherein the mass fraction of P in the oxygen-reducing catalyst is 0.1 to 1.5%.
5. The oxygen-reducing catalyst according to claim 1, wherein the mass fraction of Fe in the oxygen-reducing catalyst is 0.5 to 2.5%.
6. The oxygen-reducing catalyst according to any one of claims 1 to 5, wherein the oxygen-reducing catalyst comprises C, N, O, P, Fe, the mass fraction of C in the oxygen-reducing catalyst is not less than 86%, the mass fraction of P in the oxygen-reducing catalyst is 0.1 to 1.5%, the mass fraction of Fe in the oxygen-reducing catalyst is 0.5 to 2.5%; the pore diameter of the porous structure of the oxygen reduction catalyst is 5-100 nm.
7. The method for producing an oxygen-reducing catalyst according to any one of claims 1 to 6, characterized by comprising the steps of:
(1) dissolving zinc nitrate hexahydrate or zinc nitrate, an iron source and a phosphorus source in an organic solvent to obtain a solution A for later use;
(2) and (2) adding polyvinyl imidazole into the solution A prepared in the step (1), stirring, performing hydrothermal treatment, centrifuging, drying to obtain a doped precursor, and carbonizing the doped precursor to obtain the oxygen reduction catalyst.
8. The preparation method as claimed in claim 7, wherein in the step (2), the temperature of the carbonization treatment is 850-1050 ℃, and the time of the carbonization treatment is 2-4 h.
9. Use of an oxygen reduction catalyst according to any one of claims 1 to 6 in an electrochemical energy storage or electrochemical energy conversion device.
10. An apparatus comprising the oxygen reduction catalyst of any one of claims 1 to 6.
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| CN115101752A (en) * | 2022-05-17 | 2022-09-23 | 杭州师范大学 | Novel Fe-N-C oxygen reduction electrocatalyst and preparation and application thereof |
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| CN113314721A (en) * | 2021-06-10 | 2021-08-27 | 广东省武理工氢能产业技术研究院 | Doping type oxygen reduction catalyst with graded ventilation structure and preparation method thereof |
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