CN109772405B - Preparation method of iron-nitrogen doped carbon material - Google Patents
Preparation method of iron-nitrogen doped carbon material Download PDFInfo
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- CN109772405B CN109772405B CN201910086448.2A CN201910086448A CN109772405B CN 109772405 B CN109772405 B CN 109772405B CN 201910086448 A CN201910086448 A CN 201910086448A CN 109772405 B CN109772405 B CN 109772405B
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 41
- YYXHRUSBEPGBCD-UHFFFAOYSA-N azanylidyneiron Chemical compound [N].[Fe] YYXHRUSBEPGBCD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000593 microemulsion method Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 229920000128 polypyrrole Polymers 0.000 claims abstract description 5
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 11
- 239000004530 micro-emulsion Substances 0.000 claims description 9
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- ZPIRTVJRHUMMOI-UHFFFAOYSA-N octoxybenzene Chemical compound CCCCCCCCOC1=CC=CC=C1 ZPIRTVJRHUMMOI-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000005530 etching Methods 0.000 abstract description 2
- 230000000379 polymerizing effect Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010411 electrocatalyst Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000010183 spectrum analysis Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 239000012692 Fe precursor Substances 0.000 description 1
- 239000013504 Triton X-100 Substances 0.000 description 1
- 229920004890 Triton X-100 Polymers 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
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- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
The invention provides a preparation method of an iron-nitrogen doped carbon material, which utilizes a reverse microemulsion method to form a water-in-oil system, and Fe is added into the water-in-oil system3+Further adding oil-soluble pyrrole, passing through Fe3+And polymerizing catalytic pyrrole on an oil-water interface to form polypyrrole, adding ethanol for demulsification, centrifugally separating, washing with water, drying, and sintering at high temperature in an inert atmosphere to obtain the iron-nitrogen doped carbon material. The invention utilizes the reverse microemulsion method to prepare the iron-nitrogen doped carbon material, does not need a template and activated etching, and has low cost and high efficiency.
Description
Technical Field
The invention belongs to the technical field of iron-nitrogen doped carbon materials, and particularly relates to a brand-new preparation method of an iron-nitrogen co-doped carbon material.
Background
Oxygen reduction reactions have been studied for a long time due to their contribution to energy conversion and storage devices, such as fuel cells and metal air batteries. Although noble metal-based materials are known to be the most effective electrocatalysts for oxygen reduction reactions, their high cost, scarcity and low stability hinder their large-scale applicationThe application is as follows. Accordingly, researchers have made extensive efforts to use high activity and durable non-noble metal catalysts as an alternative electrocatalyst for next generation energy conversion devices. Recently, research on non-noble metal catalysts has been greatly advanced, including non-metal hetero-atom doped carbon materials, metal oxides, and nitrogen-coordinated transition metal doped carbon materials (M-N-C), among others. These materials have high activity, good durability, and high tolerance to fuel molecules, wherein the Fe-N-C based catalyst has catalytic activity comparable to that of the oxygen reduction reaction of Pt/C. Zhou et al, using polydopamine as a carbon source and a nitrogen source, polymerized on the surface of silica spheres, prepared Fe-N-C hollow spheres by pyrolysis and subsequent sacrificial template method, whose half-wave potential (E) in alkaline medium1/2) RHE is 0.75V vs. has better electrocatalytic activity; huang et al porous Fe3O4The hollow microsphere is taken as a template, the pyrrole monomer is dispersed on the inner surface and the outer surface of the hollow microsphere, and hydrochloric acid is further added to release Fe3+The pyrrole monomer is initiated by ions to be polymerized and pyrolyzed to generate the Fe-N-C catalyst, and the catalyst has better catalytic activity, durability and methanol tolerance in alkaline and acidic media. These efforts led researchers to believe that Fe-N-C catalyst materials could be developed into efficient oxygen reduction electrocatalysts to replace Pt/C by engineering their structures, as well as the metal active sites of the catalyst. Generally, the preparation method of the iron-nitrogen doped carbon material is a high-temperature carbonization organic metal framework, a hard template method and the like, but the methods have the defects of high cost, complex synthesis process and the like.
In order to solve the above problems, it is particularly necessary to research a new preparation method of an iron-nitrogen co-doped carbon material.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to prepare the iron-nitrogen doped carbon material by using a reverse microemulsion method, without template and activated etching, and has low cost and high efficiency.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing iron-nitrogen doped carbon material comprises forming water-in-oil system by reverse microemulsion method, adding Fe3+By addition of oil-soluble pyrrole, by Fe3+And polymerizing catalytic pyrrole on an oil-water interface to form polypyrrole, adding ethanol for demulsification, centrifugally separating, washing with water, drying, and sintering at high temperature in an inert atmosphere to obtain the iron-nitrogen doped carbon material.
Further, the preparation method specifically comprises the following steps: adding 40-80 μ L saturated FeCl into 22mL reversed-phase microemulsion system3Stirring the aqueous solution for 5-30 minutes; then adding 0.5-1mL of pyrrole, and stirring for reaction for 30-60 minutes; adding 22mL of ethanol for centrifugal separation, washing the precipitate with water for three times, and drying in an oven at 60 ℃ to obtain powder; the powder is placed in a vacuum tube furnace and calcined for 1h at the temperature of 750 ℃ and 950 ℃ in the nitrogen atmosphere to obtain the iron-nitrogen co-doped mesoporous carbon material.
Or in the preparation method, the oil-soluble pyrrole can be added firstly, and then the Fe can be added after stirring3+The aqueous solution of (1), i.e., the order of addition of both, is not critical.
Wherein, the reverse microemulsion method is a method for preparing nano materials by taking a water-in-oil thermodynamic stable system as a 'nano reactor'. An inverse microemulsion is a macroscopically homogeneous and microscopically inhomogeneous liquid mixture of thermodynamically stable dispersed immiscible two-phase liquids, usually a transparent, isotropic thermodynamically stable system consisting of surfactant, co-surfactant (alcohols), oil (hydrocarbons) and water (aqueous electrolyte). The inverse microemulsion takes water as a disperse phase and oil as a disperse medium, the particles of the disperse phase are spherical, and the radius is usually 10-100 nm.
Wherein the 22mL reverse microemulsion system is a system formed by mechanically stirring 3.6mL of polyethylene glycol octyl phenyl ether (TritonX-100)/3.2 mL of hexanol/15 mL of cyclohexane/1.2 mL of water for half an hour.
Wherein, the inert atmosphere is nitrogen or argon atmosphere.
Compared with the prior art, the invention has the advantages and positive effects that:
the invention firstly puts the reverse microemulsion system into the preparation of the polypyrrole, takes the reverse microemulsion as a 'nano reactor' for synthesizing nano-particles, has high dispersion and uniform size, realizes the shape and size control of the polypyrrole, finally carbonizes to prepare the iron-nitrogen doped carbon material, and has low cost and simple synthesis process.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is a TEM photograph of the Fe-N co-doped carbon material obtained in example 1;
FIG. 2 is a scanning electron micrograph of an iron-nitrogen co-doped carbon material obtained in example 1;
FIG. 3 is an X-ray diffraction pattern of the iron-nitrogen co-doped carbon material obtained in example 1;
FIG. 4 is a TEM photograph of the Fe-N co-doped carbon material obtained in example 2;
FIG. 5 is a scanning electron micrograph of an iron-nitrogen co-doped carbon material obtained in example 2;
FIG. 6 is an X-ray diffraction pattern of the iron-nitrogen co-doped carbon material obtained in example 2;
FIG. 7 is a scanning electron microscope spectrum analysis of the iron-nitrogen co-doped carbon material obtained in example 1;
FIG. 8 is a scanning electron microscope spectrum analysis of the iron-nitrogen co-doped carbon material obtained in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and examples. It should be understood that the embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.
In order to ensure the science, the reasonability and the effectiveness of the technical scheme of the invention, the applicant carries out a series of experiments.
Example 1
3.6mL of polyethylene glycol octyl phenyl ether (TritonX-100)/3.2 mL of hexanol/15 mL of cyclohexane/1.2 mL of water, and mechanically stirring for half an hour to form an inverse microemulsion system; add 80. mu.L of saturated FeCl3Continuously stirring the aqueous solution for half an hour; then 0.5mL of pyrrole is added, and the mixture is stirred and reacts for half an hour; adding 22mLCarrying out centrifugal separation on ethanol, washing and precipitating for three times, and drying in an oven at 60 ℃ to obtain powder; the powder is placed in a vacuum tube furnace, and calcined for 1h at 900 ℃ in a nitrogen atmosphere to obtain an iron-nitrogen co-doped carbon material, and the iron-nitrogen co-doped carbon material is characterized by a Transmission Electron Microscope (TEM), a Scanning Electron Microscope (SEM), electron energy spectrum analysis (EDS) and X-ray diffraction analysis (XRD), and the results are shown in figures 1, 2, 3 and 7. As shown in FIG. 1, the calcined carbon material consists of spherical carbons having a particle size of 30 to 50nm, and a significant sintered structure is formed between the spherical carbons; as shown in FIG. 2, the surface topography of the carbon material is spherical; as shown in fig. 7, the content of nitrogen element in the carbon material was 26.78 wt.%, and the content of iron element was 2.80 wt.%; as shown in FIG. 3, the calcined carbon material matched the characteristic peak of carbon 03-0401 with very little Fe2O3Are present. Therefore, the microemulsion method is adopted in the embodiment to successfully prepare the iron-nitrogen doped carbon material.
Example 2
3.6mL of polyethylene glycol octyl phenyl ether (Triton X-100)/3.2 mL of hexanol/15 mL of cyclohexane/1.2 mL of water, and mechanically stirring for half an hour to form a reverse microemulsion system; add 40. mu.L of saturated FeCl3Continuously stirring the aqueous solution for half an hour; then adding 1mL of pyrrole, and stirring for reaction for half an hour; adding 22mL of ethanol for centrifugal separation, washing and precipitating for three times, and drying in an oven at 60 ℃ to obtain powder; the powder is placed in a vacuum tube furnace and sintered for 1h at 900 ℃ in a nitrogen atmosphere to obtain the iron-nitrogen co-doped mesoporous carbon material, and TEM, SEM, EDS and XRD characterization is carried out on the iron-nitrogen co-doped mesoporous carbon material, and the results are shown in figures 4, 5, 6 and 8. As shown in FIG. 4, the calcined carbon material consists of spherical carbons having a particle size of 30 to 50nm, and a significant sintered structure is formed between the spherical carbons; as shown in FIG. 5, the surface topography of the carbon material appears spherical; as shown in fig. 8, the content of nitrogen element in the carbon material was 13.57 wt.%, and the content of iron element was 0.92 wt.%; as shown in FIG. 6, the calcined carbon material matched the characteristic peak of carbon 03-0401, and the corresponding Fe was obtained due to the reduced amount of the iron precursor2O3The peak intensity is significantly reduced. Therefore, the microemulsion method is adopted in the embodiment to successfully prepare the iron-nitrogen doped carbon material.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (1)
1. A preparation method of an iron-nitrogen doped carbon material is characterized by comprising the following steps: forming water-in-oil system by reverse microemulsion method, adding Fe3+By addition of oil-soluble pyrrole, by Fe3+Catalyzing pyrrole to polymerize on an oil-water interface to form polypyrrole, then adding ethanol for demulsification, centrifugally separating, washing with water, drying, and sintering at high temperature in an inert atmosphere to obtain an iron-nitrogen doped carbon material;
the preparation method comprises the following specific steps: in a 20mL reverse microemulsion system: adding 40-80 mu L of saturated FeCl into polyethylene glycol octyl phenyl ether/n-hexanol/cyclohexane/water3Stirring the aqueous solution for 5-30 minutes; then adding 0.5-1mL of pyrrole, and stirring for reaction for 30-60 minutes; adding 10-30mL of ethanol, performing centrifugal separation, washing the precipitate with water for 2-5 times, and drying in an oven at 60 ℃ to obtain powder; the powder is placed in a vacuum tube furnace and calcined for 1h at the temperature of 750 ℃ and 950 ℃ in the nitrogen atmosphere to obtain the iron-nitrogen doped carbon material.
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| CN110420655B (en) * | 2019-07-29 | 2022-07-08 | 中南民族大学 | Preparation method and application of graphite carbon-coated iron-nitrogen-carbon solid-phase Fenton catalyst |
| CN111408375A (en) * | 2020-04-18 | 2020-07-14 | 台州学院 | Preparation method of CoFe/C electrocatalyst |
| CN113831532B (en) * | 2021-08-23 | 2023-06-27 | 温州大学 | Nano spherical polypyrrole, preparation method thereof, nitrogen-doped carbon material and application thereof |
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Application publication date: 20190521 Assignee: SHANDONG LINGLONG ELECTROMECHANICAL Co.,Ltd. Assignor: QINGDAO University OF SCIENCE AND TECHNOLOGY Contract record no.: X2024980016761 Denomination of invention: Preparation method of iron nitrogen doped carbon material Granted publication date: 20220215 License type: Common License Record date: 20240926 |