CN115007189A - Polyatomic doped iron-based catalyst and preparation method thereof - Google Patents
Polyatomic doped iron-based catalyst and preparation method thereof Download PDFInfo
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- CN115007189A CN115007189A CN202210805101.0A CN202210805101A CN115007189A CN 115007189 A CN115007189 A CN 115007189A CN 202210805101 A CN202210805101 A CN 202210805101A CN 115007189 A CN115007189 A CN 115007189A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 54
- 239000003054 catalyst Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004327 boric acid Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000012265 solid product Substances 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 10
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- CWLKGDAVCFYWJK-UHFFFAOYSA-N 3-aminophenol Chemical compound NC1=CC=CC(O)=C1 CWLKGDAVCFYWJK-UHFFFAOYSA-N 0.000 claims description 5
- 229940018563 3-aminophenol Drugs 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 5
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 7
- 230000002378 acidificating effect Effects 0.000 abstract description 6
- 238000011068 loading method Methods 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000004005 microsphere Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000003763 carbonization Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 238000013507 mapping Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to the technical field of nano materials, and discloses a polyatomic doping iron-based catalyst and a preparation method thereof in order to solve the problems of low load and poor ORR (oxygen radical reduction) performance of the iron-based catalyst prepared by the existing preparation method, wherein the preparation method of the polyatomic doping iron-based catalyst comprises the following steps: dissolving boric acid in an ethanol water solution, and uniformly mixing to obtain a solvent. The preparation method takes boric acid as an acidic system, is beneficial to realizing in-situ coordination of iron element under an acidic condition, and is easy to form an iron nanocluster or iron monatomic structure in the carbonization process; in the prepared polyatomic doped iron-based catalyst, B, C, N, Fe and other elements are uniformly distributed in a nanometer microsphere structure, namely the polyatomic doped iron-based catalyst prepared by the method has higher loading capacity and excellent ORR performance.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a multi-atom doped iron-based catalyst and a preparation method thereof.
Background
The metal monatomic catalyst material shows relatively ideal catalytic performance based on the advantages of high atom utilization efficiency, good dispersibility, uniform and controllable metal active sites, excellent selectivity, high stability and the like.
However, the conventional preparation method of the metal monatomic catalyst has the problems that the prepared iron-based catalyst has low loading capacity and poor ORR performance when the iron-based catalyst is prepared.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a multi-atom doped iron-based catalyst and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a polyatomic doped iron-based catalyst comprises the following steps:
step 1: dissolving boric acid in an ethanol water solution, and uniformly mixing to obtain a solvent;
step 2: sequentially adding polyether F127, 3-aminophenol and hexamethylenetetramine into the solvent obtained in the step 1, stirring and heating to 80 ℃, reacting for 8 hours at 80 ℃, and stopping heating to obtain a reaction solution;
and step 3: standing the reaction solution obtained in the step 2, centrifuging the upper suspension, removing the supernatant generated by centrifugation, and collecting the solid product A obtained by centrifugation;
and 4, step 4: washing the solid product A with ethanol and deionized water respectively, and transferring to FeCl 3 ·6H 2 Soaking in the solution O at room temperature, performing suction filtration, collecting a solid product B obtained by suction filtration, and drying;
and 5: and calcining the dried solid product B at high temperature to obtain the polyatomic doped iron-based catalyst.
Preferably, in step 1, the volume ratio of ethanol to water in the ethanol aqueous solution is 1: 6.
preferably, the concentration of boric acid in the solvent obtained in step 1 is one of 0.2, 0.5 and 1.0 mol/L.
Preferably, in step 4, FeCl 3 ·6H 2 The concentration of the O solution is 0.25 mol/L;
solid product A in FeCl 3 ·6H 2 The time for soaking in the O solution is 2 h.
Preferably, in step 4, the drying method of the solid product B comprises the following steps: the solid product B was dried in an oven at 80 ℃ for 6 h.
Preferably, in step 5, the calcining method of the solid product B is as follows: putting the solid product B into a box-type furnace, heating to 410 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, and keeping for 2 h; then heating to 800 ℃ at the heating rate of 5 ℃/min and keeping for 2 h.
The polyatomic doped iron-based catalyst is prepared by the preparation method of the polyatomic doped iron-based catalyst.
The preparation method disclosed by the invention takes boric acid as an acidic system, is beneficial to realizing in-situ coordination of iron element under an acidic condition, and is easy to form an iron nanocluster or iron monoatomic structure in a carbonization process.
In the polyatomic doped iron-based catalyst prepared by the invention, elements such as B, C, N, Fe and the like are uniformly distributed in a nanometer microsphere structure, namely, the polyatomic doped iron-based catalyst prepared by the invention has higher loading capacity and excellent ORR performance.
Drawings
FIG. 1 is a scanning electron microscope image of a polyatomic doped iron-based catalyst prepared according to an embodiment of the present invention;
FIG. 2 is a TEM image and a Mapping image of the polyatomic doped iron-based catalyst prepared by the embodiment of the invention;
FIG. 3 is an X-ray diffraction pattern of a polyatomic doped iron-based catalyst prepared by an example of the present invention;
fig. 4 is a graph of Oxygen Reduction Reaction (ORR) performance of the polyatomic doped iron-based catalyst prepared according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
According to the volume ratio of 1: 6 mixing ethanol and water to obtain an ethanol water solution; accurately weighing 9.150g of boric acid, dissolving the boric acid in an ethanol water solution, metering the volume to 300mL, and uniformly mixing to obtain 300mL of 0.5mol/L solvent;
2g F127, 1.1g of 3-aminophenol and 1.0g of hexamethylenetetramine are sequentially added into the solvent system, and the mixture is stirred by magnetic force from the room temperature to be heated to 80 ℃; keeping the reaction at 80 ℃ for 8h, and then stopping heating to obtain reaction liquid;
standing the reaction solution for 10min, centrifuging the upper suspension, removing the supernatant generated by centrifugation, and collecting the solid product A obtained by centrifugation;
the solid product A was washed with ethanol and deionized water, and transferred to 100mL of 0.25mol/L FeCl 3 ·6H 2 Soaking in O solution at room temperature for 2 h; carrying out suction filtration, collecting a solid product B obtained by suction filtration, and drying in an oven at 80 ℃ for 6 h;
and (3) placing the solid product B into a box-type furnace, heating to 410 ℃ at a heating rate of 1 ℃/min for 2h in a nitrogen atmosphere, and heating to 800 ℃ at a heating rate of 5 ℃/min for 2h to obtain the nitrogen and boron co-doped iron-based catalyst.
Example 2
According to the volume ratio of 1: 6 mixing ethanol and water to obtain an ethanol water solution; accurately weighing 3.660g of boric acid, dissolving the boric acid in an ethanol water solution, metering the volume to 300mL, and uniformly mixing to obtain 300mL of 0.2mol/L solvent;
2g F127, 1.1g of 3-aminophenol and 1.0g of hexamethylenetetramine are sequentially added into the solvent system, and the mixture is stirred by magnetic force from the room temperature to be heated to 80 ℃; keeping the reaction at 80 ℃ for 8h, and then stopping heating to obtain a reaction solution;
standing the reaction solution for 10min, centrifuging the upper suspension, removing the supernatant generated by centrifugation, and collecting the solid product A obtained by centrifugation;
the solid product A was washed with ethanol and deionized water, and transferred to 100mL of 0.25mol/L FeCl 3 ·6H 2 Soaking in O solution at room temperature for 2 h; carrying out suction filtration, collecting a solid product B obtained by suction filtration, and drying in an oven at 80 ℃ for 6 h;
and (3) placing the solid product B into a box-type furnace, heating to 410 ℃ at a heating rate of 1 ℃/min for 2h in a nitrogen atmosphere, and heating to 800 ℃ at a heating rate of 5 ℃/min for 2h to obtain the nitrogen and boron co-doped iron-based catalyst.
Example 3
According to the volume ratio of 1: 6 mixing ethanol and water to obtain an ethanol water solution; accurately weighing 18.3g of boric acid, dissolving in an ethanol water solution, metering to 300mL, and uniformly mixing to obtain 300mL of 1mol/L solvent;
2g F127, 1.1g of 3-aminophenol and 1.0g of hexamethylenetetramine are sequentially added into the solvent system, and magnetic stirring is carried out from the room temperature condition to raise the temperature to 80 ℃; keeping the reaction at 80 ℃ for 8h, and then stopping heating to obtain reaction liquid;
standing the reaction solution for 10min, centrifuging the upper suspension, removing the supernatant generated by centrifugation, and collecting the solid product A obtained by centrifugation;
the solid product A was washed with ethanol and deionized water, and transferred to 100mL of 0.25mol/L FeCl 3 ·6H 2 Soaking in O solution at room temperature for 2 h; carrying out suction filtration, collecting a solid product B obtained by suction filtration, and drying in an oven at 80 ℃ for 6 h;
and (3) placing the solid product B in a box-type furnace, heating to 410 ℃ at a heating rate of 1 ℃/min for 2h in a nitrogen atmosphere, and heating to 800 ℃ at a heating rate of 5 ℃/min for 2h to obtain the nitrogen and boron co-doped iron-based catalyst.
The polyatomic doped iron-based catalyst prepared in example 1 was subjected to performance tests including scanning electron microscopy characterization, transmission electron microscopy and Mapping characterization, polycrystalline X-ray diffraction characterization, and electrochemical performance testing:
1. characterization of scanning Electron microscope
The structural morphology of the iron-based catalyst was observed by scanning electron microscopy, and the results are shown in fig. 1. As can be seen from FIG. 1, the prepared iron-based catalyst has a uniform spherical structure with a diameter of about 300 nm; the spherical surface has obvious defects, and more active sites can be provided; the iron element is not obviously aggregated, and no iron particles exist on the spherical surface, which preliminarily shows that the iron element is uniformly distributed in the nanospheres.
2. Transmission electron microscopy and Mapping characterization
The structural morphology of the iron-based catalyst is further observed by adopting a projection electron microscope, the result is shown in figure 2, 2a (200nm) and 2b (5nm) are Transmission Electron Microscope (TEM) result images of target materials with different magnifications, and the distribution state of the iron element is not obviously observed in the images to prove that the iron element exists in a tiny nano-size form, and the nano-cluster and the monatomic iron are probably existed at the same time; 2 c-2 f are element test result graphs, and the results prove that B, C, N, Fe elements are uniformly distributed in the nano microsphere structure, and in addition, 2f shows that the prepared iron-based catalyst has higher loading capacity.
3. Polycrystalline X-ray diffraction characterization
The element component information of the iron-based catalyst is represented by polycrystalline X-ray diffraction, the result is shown in figure 3, and the test result of figure 3 shows that the prepared target material only has an amorphous carbon peak, does not have a related crystal form iron metal signal peak, and proves that the iron element in the target material exists in a form of single atom or nanocluster.
4. Electrochemical Performance test-Oxygen Reduction Reaction (ORR)
In order to study the catalytic activity of the prepared iron-based catalyst, 20% Pt/C was selected as a control for evaluation of the catalytic performance of cathode oxygen reduction (ORR). Using a three-electrode system in O 2 Cyclic voltammetric scans were performed in a saturated 0.1M aqueous KOH solution at an electrode rotation rate of 1600r/min and a scan rate of 5 mV/s. Under the condition of room temperature, 0.1M KOH aqueous solution is used as electrolyte, a saturated calomel electrode is used as a reference electrode, a Pt sheet is used as an auxiliary electrode, and a platinum carbon electrode is used as a working electrode.
As can be seen from FIG. 4, the half-wave potential of the iron-based catalyst prepared by the method(E 1/2 ) At 0.88V, exhibited ORR catalytic activity superior to that of the commercial 20% Pt/C catalyst, indicating that the iron-based catalyst prepared had excellent ORR performance.
The preparation method takes boric acid as an acidic system, is beneficial to realizing in-situ coordination of iron element under an acidic condition, is easy to form an iron nanocluster or iron monatomic structure in the carbonization process, and has the advantages of greenness, economy, high efficiency and large-scale synthesis.
In the polyatomic doped iron-based catalyst prepared by the invention, elements such as B, C, N, Fe are uniformly distributed in a nano microsphere structure, namely the polyatomic doped iron-based catalyst prepared by the invention has higher loading capacity and excellent ORR performance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. A preparation method of a polyatomic doped iron-based catalyst is characterized by comprising the following steps:
step 1: dissolving boric acid in an ethanol water solution, and uniformly mixing to obtain a solvent;
step 2: sequentially adding polyether F127, 3-aminophenol and hexamethylenetetramine into the solvent obtained in the step 1, stirring and heating to 80 ℃, reacting for 8 hours at the temperature of 80 ℃, and stopping heating to obtain a reaction solution;
and step 3: standing the reaction solution obtained in the step 2, centrifuging the upper suspension, removing the supernatant generated by centrifugation, and collecting the solid product A obtained by centrifugation;
and 4, step 4: washing the solid product A with ethanol and deionized water respectively, and transferring the solid product A to FeCl 3 ·6H 2 Soaking in the solution O at room temperature, performing suction filtration, collecting a solid product B obtained by suction filtration, and drying;
and 5: and calcining the dried solid product B at high temperature to obtain the polyatomic doped iron-based catalyst.
2. The method for preparing a polyatomic doped iron-based catalyst according to claim 1, wherein in the step 1, the volume ratio of ethanol to water in the ethanol aqueous solution is 1: 6.
3. the method of claim 1, wherein the concentration of boric acid in the solvent obtained in step 1 is one of 0.2, 0.5 and 1.0 mol/L.
4. The method of claim 1, wherein in step 4, FeCl is added 3 ·6H 2 The concentration of the O solution is 0.25 mol/L;
solid product A in FeCl 3 ·6H 2 The time for soaking in the O solution is 2 h.
5. The method for preparing a polyatomic doped iron-based catalyst according to claim 1, wherein in the step 4, the solid product B is dried by the following method: the solid product B was dried in an oven at 80 ℃ for 6 h.
6. The method for preparing the polyatomic doped iron-based catalyst according to claim 1, wherein in the step 5, the solid product B is calcined by the following method: putting the solid product B into a box-type furnace, heating to 410 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, and keeping for 2 h; then heating to 800 ℃ at the heating rate of 5 ℃/min and keeping for 2 h.
7. A polyatomic doped iron-based catalyst prepared by the method of preparing a polyatomic doped iron-based catalyst according to any one of claims 1 to 6.
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