CN114672838A - Preparation method of carbon substrate nitrogen coordination metal single atom or cluster catalyst, product and application thereof - Google Patents
Preparation method of carbon substrate nitrogen coordination metal single atom or cluster catalyst, product and application thereof Download PDFInfo
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- CN114672838A CN114672838A CN202210473093.4A CN202210473093A CN114672838A CN 114672838 A CN114672838 A CN 114672838A CN 202210473093 A CN202210473093 A CN 202210473093A CN 114672838 A CN114672838 A CN 114672838A
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
Abstract
The invention discloses a preparation method of a carbon substrate nitrogen coordination metal monoatomic or cluster catalyst. The method fully achieves the technical purposes of low price and wide raw materials, simple preparation process, easy control and operation and suitability for expanded production, and has good scientific research and market application value. The metal monoatomic or clustered catalyst coordinated with carbon substrate nitrogen prepared by the method has excellent catalytic performance and obvious effect due to the existence of the metal monoatomic or clustered catalyst.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a carbon substrate nitrogen coordination metal monoatomic or clustered catalyst, and a product and application thereof.
Background
Due to the high dispersion of active components of the catalyst material doped with metal monoatomic or metal cluster, the great improvement of the metal utilization rate and the interaction between the active center and the adjacent coordination atoms, the material shows excellent catalytic activity, stability and selectivity, and is also concerned in fields (such as sensing and the like) other than the catalytic field. At present, the methods for doping the monatomic material mainly include the following methods: atomic layer deposition, mass selective soft landing, and wet chemical methods. However, most of the existing methods for preparing the doped monatomic material are complicated.
In the field of oxygen reduction (ORR) catalysis, most of noble metals (Pt, Pd, etc.) have good performance, and now the commercialized Pt/C catalyst is the mainstream, but the cost of the whole catalyst is high and the catalyst is easily affected by methanol because the Pt/C catalyst contains noble metal Pt. In recent years, non-noble metal catalysts represented by M-N-C (M ═ Fe, Co, Ni, Mn, or the like) among catalysts have been rapidly developed due to their good performance, but the preparation of non-noble metal catalysts often requires high-temperature annealing and is prone to generating agglomeration, thereby affecting the catalytic performance, and therefore, the development and application of doped monatomic catalytic materials are becoming a trend. According to the report of the prior art, the preparation method of the doped monatomic material is mainly a wet chemical method, which greatly increases the time cost, and some preparation instruments adopted in the preparation process are expensive and have low yield.
Patent (CN113151861A) discloses a method for synthesizing a carbon-supported monatomic catalyst by thermal shock and a carbon-supported monatomic catalyst. The method mixes metal salt, organic ligand solution and carbon liquid, controls temperature for many times by using an electrode power supply, and anchors metal on carbon to generate a monatomic catalyst. However, this method involves liquid phase mixing and multi-step synthesis, and the preparation process is limited in space and time, and is not suitable for mass production. Patent (CN112387295A) discloses a preparation method of carbon-supported ruthenium monatomic, which is to obtain a carbon-supported ruthenium monatomic catalyst by mixing and drying liquid phases, then annealing and cooling the solid phase. Although this method achieves a simple starting material, the synthesis involves liquid phase mixing and drying, and is not simple enough in large scale preparation.
Therefore, how to implement a simple and convenient method, low cost and being suitable for mass production of catalytic materials doped with metal single atoms or clusters is a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, in order to effectively solve the technical problems of high cost, complex process and unsuitability for mass production in the prior art, the invention provides a preparation method of a carbon-based nitrogen coordination metal monatomic or cluster catalyst, which not only simplifies the preparation process, but also has excellent catalytic performance and obvious effect of the prepared product. The invention also provides a carbon substrate nitrogen coordination metal single atom or cluster catalyst and application thereof in the aspect of oxygen reduction technology.
The technical scheme provided by the invention is as follows:
1. a method for preparing a carbon substrate nitrogen coordinated metal monatomic or cluster catalyst, the method comprising the steps of:
(1) mixing and grinding nitrogen-containing organic micromolecules, volatile metal salt and carbon material;
(2) and (2) heating the mixture obtained in the step (1), heating to 500-1000 ℃ at 2-5 ℃ and 5m5n, preserving the heat for 1-3 h, and cooling to room temperature to obtain the catalyst.
Preferably, the molecular weight of the nitrogen-containing organic micromolecules in the step (1) is 20-10000, and the nitrogen-containing organic micromolecules are easy to melt at 50-300 ℃.
Preferably, the nitrogen-containing organic micromolecules are one or more of 1, 10-phenanthroline, urea and melamine.
Preferably, the metal element in the volatile metal salt in step (1) includes one or more of titanium, vanadium, chromium, iron, cobalt, nickel, manganese, copper, zinc, molybdenum, silver, ruthenium, palladium, platinum and rhodium.
Preferably, the volatile metal salt is one or more of metallocene or acetylacetone metal salt.
Preferably, the carbon material is activated carbon.
Preferably, the molar ratio of nitrogen element to metal element in the nitrogen-containing organic micromolecules and volatile metal salt is 1.5-3: 1. .
Preferably, the mass ratio of the nitrogen-containing organic small molecules to the carbon material is 1: 1 to 5.
Preferably, step (2) is carried out in an atmosphere furnace with ammonia, nitrogen, argon or helium as the gas.
Preferably, the nitrogen-containing organic small molecules, the volatile metal salt and the carbon material in the step (1) are ground and fully mixed.
2. The carbon substrate nitrogen coordination metal single atom or cluster catalyst prepared by the method.
3. An application of carbon substrate nitrogen coordination metal single atom or cluster catalyst as oxygen reduction catalyst.
The invention has the beneficial effects that:
compared with the prior art, the invention carries out technical innovation from preparation raw materials and process conditions, nitrogen-containing organic micromolecules, volatile metal salts and carbon materials are mixed in the preparation process, and then high-temperature treatment is directly carried out. The method fully achieves the technical purposes of low price and wide raw materials, simple preparation process, easy control and operation and suitability for expanded production, and has good scientific research and market application value. The metal monoatomic or clustered catalyst coordinated with carbon substrate nitrogen prepared by the method has excellent catalytic performance and obvious effect due to the existence of the metal monoatomic or clustered catalyst.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
fig. 1 is a HADDF-STEM diagram of a carbon-carbon based nitrogen-coordinated iron metal cluster catalyst material prepared in example 1;
fig. 2 is an FESEM view of the carbon-based nitrogen-coordinated iron metal cluster catalyst material prepared in example 1;
fig. 3 is a graph of oxygen reduction performance tests of the carbon-based nitrogen-coordinated iron metal cluster catalyst prepared in example 1 and a commercial Pt5C catalyst;
fig. 4 is a HADDF-STEM diagram of a carbon-carbon based nitrogen coordinated iron metal cluster catalyst material prepared in example 2;
fig. 5 is a graph of oxygen reduction performance test of the nitrogen-coordinated iron monatomic catalyst with the commercial Pt5C catalyst of the carbon substrate prepared in example 2;
fig. 6 is a graph of oxygen reduction performance tests of the carbon-based nitrogen-coordinated iron, cobalt metal cluster catalyst prepared in example 3 and a commercial Pt5C catalyst;
fig. 7 is a graph of oxygen reduction performance tests of the carbon-based nitrogen-coordinated iron, cobalt, nickel metal cluster catalyst prepared in example 4 with commercial Pt 5C;
FIG. 8 is a carbon-based nitrogen-coordinated iron, nickel metal cluster catalyst and commercial RuO prepared in example 52The oxygen evolution performance test chart of (1).
Detailed Description
The following embodiments of the present invention are provided by way of specific examples, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure herein. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and embodiments may be combined with each other without conflict.
Example 1
The preparation method of the iron metal cluster catalyst with carbon substrate nitrogen coordination comprises the following steps:
(1) placing 40mg of 1, 10-phenanthroline, 10mg of ferrocene and 100mg of activated carbon in a mortar for fully grinding and mixing;
(2) and (3) placing the intermediate in a tubular furnace in an argon atmosphere, raising the temperature to 800 ℃ at the temperature raising rate of 5m5n at the temperature of 5 ℃, preserving the temperature for 2h, and naturally cooling to obtain the carbon-based nitrogen-coordinated iron metal cluster catalyst.
FIG. 1 shows the catalyst material (AC-Phen-Fe) prepared in example 1cluster) And it can be seen from fig. 1 that the prepared iron metal cluster catalyst is uniformly distributed on the carbon substrate and the supported density is large at a scale of 2 nm.
FIG. 2 is a scanning electron microscope image of field emission of the catalyst material prepared in example 1, and it can be seen from FIG. 2 that the catalyst material (AC-Phen-Fe) prepared in example 1 basically uses the added activated carbon as a base material, and there is no process of nano-crystallization of the carbon material during the preparation process, which is formed by infiltration in the micropores of the carbon due to adsorption after the iron is anchored.
Taking 2mg of each of the prepared catalyst material and commercial Pt5C, respectively dispersing into 1mL of mixed solvent (the mixed solvent is formed by mixing water and ethanol in an equal volume ratio), respectively adding 20 mu L of 5% Naf5on solution, and then continuously carrying out ultrasonic treatment on the solution for 10m5n to obtain two dispersions; polishing the rotating ring disc electrode to be flat and smooth by using aluminum powder with the particle size of 0.3 mu m and 0.05 mu m respectively, washing the electrode by using deionized water, and airing for later use; two kinds of dispersions, each 5. mu.L, were dropped into the center of the rotating ring disk electrode, and dried naturally to prepare two kinds of redox test electrodes, and the redox performance of the two kinds of redox test electrodes was tested, and the results are shown in FIG. 3.
FIG. 3 is a graph of the performance of two prepared redox test electrodes in oxygen reduction catalysis, and from FIG. 3, it can be seen that the performance of the prepared electrode containing the catalyst material (AC-Phen-Fe) prepared in example 1 is much higher than that of the electrode containing commercial Pt5C, indicating that the catalyst material prepared in the present invention has good prospects in replacing noble metal oxygen reduction catalysts.
Example 2
The preparation method of the carbon substrate nitrogen coordinated iron monatomic catalyst comprises the following steps:
(1) placing 40mg of 1, 10-phenanthroline, 5mg of ferrocene and 100mg of activated carbon in a mortar for fully grinding and mixing;
(2) and (3) putting the intermediate into a tubular furnace in an argon atmosphere, raising the temperature to 800 ℃ at the temperature rise rate of 5m5n at the temperature of 5 ℃, preserving the temperature for 2h, and naturally cooling to obtain the carbon-based nitrogen-coordinated iron monatomic catalyst.
FIG. 4 is a HADDF-STEM graph of the catalyst material (AC-Phen-Fe) prepared in example 2, and it can be seen from FIG. 4 that the prepared iron metal monatomic catalyst is uniformly distributed on the carbon substrate at a scale of 2 nm.
Taking 2mg of each of the carbon-based nitrogen-coordinated iron monatomic catalyst material prepared in example 2 and commercial Pt5C, dispersing them into 1m of a mixed solvent (the mixed solvent is formed by mixing water and ethanol in an equal volume ratio), adding 20 μ L of a 5% Naf5on solution, followed by continuous sonication for 10m5n, to obtain two dispersions; polishing the rotating ring disc electrode to be flat and smooth by using aluminum powder with the particle size of 0.3 mu m and 0.05 mu m respectively, washing the electrode by using deionized water, and airing for later use; two kinds of dispersion liquid with the volume of 5 μ L are respectively dripped and rotated to the center of a rotating ring plate electrode, natural drying is carried out, two kinds of oxygen reduction testing electrodes are prepared, the oxygen reduction performance of the two kinds of oxygen reduction testing electrodes is tested, and the obtained result is shown in figure 5. It can also be seen from fig. 5 that the catalyst material prepared in example 2 has good prospects in replacing the noble metal oxygen reduction catalyst.
Example 3
The preparation method of the carbon-based nitrogen-coordinated iron and cobalt metal cluster catalyst comprises the following steps:
(1) placing 40mg of 1, 10-phenanthroline, 10mg of ferrocene, 10mg of cobaltocene and 100mg of activated carbon in a mortar for fully grinding and mixing;
(2) and (3) placing the intermediate in a tubular furnace in an argon atmosphere, raising the temperature to 800 ℃ at the temperature raising rate of 5m5n at the temperature of 5 ℃, preserving the temperature for 2h, and naturally cooling to obtain the carbon-based nitrogen-coordinated iron and cobalt metal cluster catalyst.
Taking 2mg each of the carbon-based nitrogen-coordinated iron and cobalt metal cluster catalyst material prepared in example 3 and commercialized Pt5C, dispersing into 1m of a mixed solvent (the mixed solvent is formed by mixing water and ethanol in an equal volume ratio), adding 20 μ L of a 5% Naf5on solution, followed by continuous ultrasonic treatment at 10m5n, to obtain two dispersions; polishing the rotating ring disc electrode to be flat and smooth by using aluminum powder with the particle size of 0.3 mu m and 0.05 mu m respectively, washing the electrode by using deionized water, and airing for later use; two kinds of dispersion liquid with the volume of 5 μ L are respectively dripped and rotated to the center of a rotating ring plate electrode, natural drying is carried out, two kinds of oxygen reduction testing electrodes are prepared, the oxygen reduction performance of the two kinds of oxygen reduction testing electrodes is tested, and the obtained result is shown in figure 6. It can also be seen from fig. 6 that the catalyst material prepared in example 3 has good prospects in replacing the noble metal oxygen reduction catalyst.
Example 4
The preparation method of the nitrogen-coordinated iron, cobalt and nickel metal cluster catalyst with the carbon substrate comprises the following steps:
(1) placing 40mg of 1, 10-phenanthroline, 10mg of ferrocene, 10mg of cobaltocene, 10mg of nickelocene and 100mg of activated carbon in a mortar for fully grinding and mixing;
(2) and (3) placing the intermediate in a tubular furnace in an argon atmosphere, raising the temperature to 800 ℃ at the temperature raising rate of 5m5n at the temperature of 5 ℃, preserving the temperature for 2h, and naturally cooling to obtain the nitrogen-coordinated iron, cobalt and nickel metal cluster catalyst with the carbon substrate.
Taking 2mg of each of the carbon-based nitrogen-coordinated iron, cobalt, nickel metal cluster catalyst material prepared in example 4 and commercialized Pt5C, dispersing them into 1m of a mixed solvent (the mixed solvent is formed by mixing water and ethanol in an equal volume ratio), adding 20 μ L of 5% Naf5on solution, and then subjecting to continuous ultrasound for 10m5n to obtain two dispersions; polishing the rotating ring disc electrode to be flat and smooth by using aluminum powder with the particle size of 0.3 mu m and 0.05 mu m respectively, washing the electrode by using deionized water, and airing for later use; two kinds of dispersion liquid with the volume of 5 μ L are respectively dripped and rotated to the center of a rotating ring plate electrode, natural drying is carried out, two kinds of oxygen reduction testing electrodes are prepared, the oxygen reduction performance of the two kinds of oxygen reduction testing electrodes is tested, and the obtained result is shown in figure 7. It can also be seen from fig. 7 that the catalyst material prepared in example 4 has good prospects in replacing the noble metal oxygen reduction catalyst.
Example 5
The preparation method of the carbon-based nitrogen-coordinated iron and nickel metal cluster catalyst comprises the following steps:
(1) placing 40mg of 1, 10-phenanthroline, 10mg of ferrocene, 10mg of nickelocene and 100mg of activated carbon in a mortar for fully grinding and mixing;
(2) and (3) placing the intermediate in a tubular furnace in an argon atmosphere, raising the temperature to 800 ℃ at the temperature raising rate of 5m5n at the temperature of 5 ℃, preserving the temperature for 2h, and naturally cooling to obtain the nitrogen-coordinated iron and nickel metal cluster catalyst with the carbon substrate.
Taking 2mg of the carbon-based nitrogen-coordinated iron-nickel metal cluster catalyst material prepared in example 5, and adding 20 μ L of a 5% Naf5on solution to a 1m mixed solvent (the mixed solvent is formed by mixing water and ethanol in an equal volume ratio), followed by continuous ultrasonic treatment for 10 minutes to obtain a dispersion liquid; polishing the disc electrode to be flat and smooth by using aluminum powder with the particle size of 0.3 mu m and 0.05 mu m respectively, washing the disc electrode by using deionized water, and airing the disc electrode for later use; and respectively dropwise adding 5 mu L of dispersion liquid to the center of the disc electrode, naturally drying to prepare an oxygen evolution test electrode, and testing the oxygen evolution performance of the oxygen evolution test electrode, wherein the result is shown in figure 8.
In summary, the oxidation-reduction performance and the oxygen evolution performance of the carbon-supported nitrogen-coordinated metal monoatomic or metal cluster catalyst material prepared by the preparation method in the examples and the electrodes prepared by dropwise adding the carbon-supported nitrogen-coordinated metal monoatomic or metal cluster catalyst material to the center of the circular disc electrode and the center of the circular disc electrode show that the catalyst material prepared by the method of the present invention can be prepared from the metal iron, nickel, cobalt and manganese with low cost, compared with the catalyst material containing the commercially available Pt5C and RuO with high price2The catalyst can obviously reduce the preparation cost on the premise of not influencing the performance, and the material can have good application in different catalysis directions due to different activity effects of metals, thereby showing that the preparation method and the product prepared by the method have remarkable progress.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of a carbon substrate nitrogen coordination metal single atom or cluster catalyst is characterized by comprising the following steps:
(1) mixing and grinding nitrogen-containing organic micromolecules, volatile metal salt and carbon material;
(2) and (2) heating the mixture obtained in the step (1), heating to 500-1000 ℃ at the temperature of 2-5 ℃ and 5m5n, preserving heat for 1-3 h, and cooling to room temperature to obtain the catalyst.
2. The method for preparing the carbon-based nitrogen coordinated metal monoatomic or cluster catalyst according to claim 1, wherein the molecular weight of the nitrogen-containing organic small molecule in the step (1) is 20 to 10000, and the nitrogen-containing organic small molecule is easily melted at 50 to 300 ℃.
3. The method for preparing the carbon substrate nitrogen coordination metal monoatomic or cluster catalyst according to claim 1, wherein the nitrogen-containing organic micromolecules are one or more of 1, 10-phenanthroline, urea and melamine.
4. The method for preparing the carbon-based nitrogen coordinated metal monoatomic or clustered catalyst according to claim 1, wherein the metal element in the volatile metal salt in the step (1) includes one or more of titanium, vanadium, chromium, iron, cobalt, nickel, manganese, copper, zinc, molybdenum, silver, ruthenium, palladium, platinum and rhodium.
5. The method for preparing the carbon substrate nitrogen coordinated metal single atom or cluster catalyst as claimed in claim 1, wherein the volatile metal salt is one or more of metallocene or acetylacetone metal salt, and the carbon material is activated carbon.
6. The method for preparing the carbon-based nitrogen coordinated metal monoatomic or cluster catalyst according to claim 1, wherein the molar ratio of nitrogen element to metal element in the nitrogen-containing organic small molecule and volatile metal salt is 1.5-3: 1, the mass ratio of the nitrogen-containing organic small molecules to the carbon material is 1: 1 to 5.
7. The method for preparing the carbon substrate nitrogen coordinated metal monoatomic or clustered catalyst according to claim 1, wherein the step (2) is performed in an atmosphere furnace, and the gas is ammonia, nitrogen, argon or helium.
8. The method for preparing the carbon-based nitrogen coordinated metal single atom or cluster catalyst according to claim 1, wherein the nitrogen-containing organic small molecule, the volatile metal salt and the carbon material in the step (1) are ground and then fully mixed.
9. The carbon substrate nitrogen coordinated metal monoatomic or clustered catalyst prepared by the method according to any one of claims 1 to 8.
10. An application of carbon substrate nitrogen coordination metal single atom or cluster catalyst as oxygen reduction catalyst.
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| CN115722224A (en) * | 2022-09-12 | 2023-03-03 | 遂宁碳基环保科技有限公司 | Carbon-supported transition metal catalyst for sewage treatment and preparation method and application thereof |
| CN116139937A (en) * | 2023-04-20 | 2023-05-23 | 天津渤化化工发展有限公司 | Non-mercury catalyst, solid-phase grinding preparation method and application thereof in synthesizing chloroethylene by acetylene method |
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