CN112117466B - Preparation method of nitrogen self-doped porous graphite carbon MFCs air cathode catalyst - Google Patents
Preparation method of nitrogen self-doped porous graphite carbon MFCs air cathode catalyst Download PDFInfo
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- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
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- H—ELECTRICITY
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- H01M4/8605—Porous electrodes
- H01M4/861—Porous electrodes with a gradient in the porosity
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a preparation method of a nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst. The method prepares the porous graphite biomass carbon by using the waste mangosteen pericarp biomass, dopes nitrogen elements contained in the biomass material without adding a nitrogen source, and combines the activation of KOH and Co 2+ The catalytic graphitization and the preparation process are simple, and the mangosteen pericarp biomass is successfully converted into the high-performance ORR catalyst for the MFC air cathode.
Description
Technical Field
The invention relates to the field of microbial fuel cells, in particular to a preparation method of a nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst.
Background
Microbial Fuel Cells (MFCs) are a green technology that can process organic matters in wastewater and generate electric energy, and have important significance in the fields of sustainable development and new energy development.
The air cathode MFCs is one of the main research directions of MFCs due to its advantages of simple structure, high efficiency, low cost, etc. The existing air cathode MFCS also has disadvantages such as: the slow kinetics of Oxygen Reduction Reactions (ORR), high overpotentials, and mass transfer resistances of oxygen result in poor ORR performance of air cathode MFCs. Therefore, the development of an air cathode oxygen reduction catalyst with high efficiency, low cost and good stability is very important for the large-scale application of the MFCs.
In the prior art, various air cathode oxygen reduction catalysts are developed, and a noble metal platinum (Pt) based catalyst has high electrocatalytic activity and is an oxygen reduction catalyst for researching and applying MFCs. However, Pt is expensive, expensive to produce and use, and difficult to apply in large scale production. Carbon-based materials are considered to be one of the best alternatives to Pt-based catalysts. The specific surface area and pore structure of carbon-based catalysts are important factors affecting ORR performance.
The prior art generally uses a chemical activator to activate the carbon-based material to obtain a porous structure with high specific surface area, but the addition of the chemical activator reduces the graphitization degree of the material, thereby reducing the conductivity of the material. Other methods for preparing porous graphitic carbon materials, such as sacrificial templating methods using silica or surfactants, require expensive precursor materials and are complicated to prepare and difficult to market on a large scale.
The biomass as a carbon-containing precursor has the characteristics of richness, reproducibility, low price and the like, and the unique natural structure and the abundant element composition of the biomass play an important role in synthesizing the carbon material.
Therefore, the development of a low-cost and high-efficiency method for preparing the carbon material with a proper porous structure, high graphitization degree and proper heteroatom doping is significant for the application of the carbon material in the field of ORR catalysts.
Disclosure of Invention
The invention aims to overcome the problems and provides a method for preparing a mangosteen peel carbon source and a mangosteen peel nitrogen source by combining KOH activation and Co 2+ A strategy for synthesizing nitrogen self-doped porous graphite carbon with low cost and high efficiency by catalyzing graphitization.
The technical scheme disclosed by the invention is as follows:
the preparation method of the nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst comprises the following steps:
s1, washing the mangosteen pericarp with deionized water repeatedly, drying at the temperature of 100-120 ℃, and crushing the dried mangosteen pericarp into powder to obtain a product A;
s2, heating the product A to 400 ℃ at a heating rate of 5-8 ℃/min under the protection of nitrogen, then pyrolyzing for 2-3h to obtain a dark black product, and grinding to obtain a product B;
s3, adding the product B into CoCl 2 Soaking in water solution under stirring for 6-10h, performing solid-liquid separation to obtain solid phase, drying, adding into KOH solution, reacting under stirring for 6-10h, separating solid phase again, and drying to obtain product C;
s4, heating the product C to 600-850 ℃ at a heating rate of 5-8 ℃/min under the protection of nitrogen, and then calcining for 2-3h to obtain a black product D;
s5, immersing the product D into an HCl solution for reaction for 8-12 hours, separating a solid phase, repeatedly washing the solid phase to be neutral by using deionized water, and drying to obtain the nitrogen self-doped porous graphite carbon.
As a modification, the drying in S1 is carried out in an oven for 10 to 12 hours.
As a modification, CoCl as described in S3 2 The concentration of the aqueous solution is 0.05mol/L, and the product B is mixed with CoCl 2 The mass ratio of (A) to (B) is 1:1-2: 1.
As an improvement, the concentration of the KOH solution in S3 is 0.1g/mL, and the mass ratio of the product B to KOH is 1:1-1: 2.
As an improvement, the product washed to be neutral by the deionized water in S5 is dried for 10 to 12 hours at the temperature of 60 to 80 ℃.
The invention has the advantages that:
the method prepares the porous graphite biomass carbon by using the waste mangosteen pericarp biomass, dopes nitrogen elements contained in the biomass material without adding a nitrogen source, and combines the activation of KOH and Co 2+ Catalytic graphitization and simple preparation processIn one way, mangosteen pericarp biomass was successfully converted to a high performance ORR catalyst for MFCs air cathodes.
Drawings
FIG. 1 is a 5 μm electron micrograph of example 1 of the present invention;
FIG. 2 is a 5 μm electron micrograph of example 2 of the present invention;
FIG. 3 is a 5 μm electron micrograph of example 3 of the present invention;
FIG. 4 is a 2 μm electron micrograph of example 4 of the present invention;
FIG. 5 is a 5 μm electron micrograph of example 4 of the present invention;
FIG. 6 is a 5 μm electron micrograph of example 5 of the present invention;
FIG. 7 shows XPS survey spectra of examples 1-5 of the present invention;
FIG. 8 is a nitrogen adsorption-desorption isotherm for examples 1-5 of the present invention;
FIG. 9 is a plot of power density versus polarization for examples 1-5 of the present invention;
FIG. 10 shows Raman curves of examples 1-5 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples. It should be understood that the examples of the present invention are illustrative only and are not intended to limit the scope of the present invention. Further, after reading the teaching of the present invention, the skilled person can make changes or modifications to the invention, and such equivalent forms also fall within the scope defined by the claims of the present application.
Example 1
The embodiment discloses a preparation method of a nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst, which comprises the following steps:
s1, repeatedly washing mangosteen pericarp with deionized water, drying at 100 ℃ for 12 hours, and crushing the dried mangosteen pericarp into powder to obtain a product A;
s2, under the protection of nitrogen, gradually heating the product A to 400 ℃ in a tubular furnace at a heating rate of 5 ℃/min, then pyrolyzing for 2h to obtain a dark black product, and grinding to obtain a product B;
s3, adding 10g of product B into 200mL of 005mol/L of CoCl 2 Soaking the mixture in an aqueous solution for 8 hours under the condition of magnetic stirring, then carrying out solid-liquid separation to obtain a solid phase, drying the solid phase in a 60-DEG C oven, adding the dried solid phase into 200mL of KOH solution with the concentration of 0.1g/mL, soaking the mixture for 8 hours under the stirring state, separating the solid phase again, and drying the solid phase to obtain a product C;
s4, under the protection of nitrogen, heating the product C to 600 ℃ in a tubular furnace at a heating rate of 5 ℃/min, and then calcining for 1h to obtain a black product D;
s5, immersing the product D in HCl solution for 8 hours, then carrying out solid-liquid separation in a suction filtration mode, repeatedly washing with deionized water until the solution is neutral, drying at 70 ℃ for 12 hours, and then obtaining the nitrogen self-doped porous graphite carbon.
Example 2
The embodiment discloses a preparation method of a nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst, which comprises the following steps:
s1, repeatedly washing mangosteen pericarp with deionized water, drying at 100 ℃ for 12 hours, and crushing the dried mangosteen pericarp into powder to obtain a product A;
s2, under the protection of nitrogen, gradually heating the product A to 400 ℃ in a tubular furnace at a heating rate of 5 ℃/min, then pyrolyzing for 2h to obtain a dark black product, and grinding to obtain a product B;
s3, adding 10g of product B into 200mL of 0.05mol/L CoCl 2 Soaking the mixture in an aqueous solution for 8 hours under the condition of magnetic stirring, then carrying out solid-liquid separation to obtain a solid phase, drying the solid phase in a 60-DEG C oven, adding the dried solid phase into 200mL of KOH solution with the concentration of 0.1g/mL, soaking the mixture for 8 hours under the stirring state, separating the solid phase again, and drying the solid phase to obtain a product C;
s4, under the protection of nitrogen, heating the product C to 700 ℃ in a tubular furnace at a heating rate of 5 ℃/min, and then calcining for 2h to obtain a black product D;
s5, immersing the product D in HCl solution for 8 hours, then performing solid-liquid separation in a suction filtration mode, repeatedly washing the product D with deionized water until the solution is neutral, and drying the product D at 70 ℃ for 12 hours to obtain the nitrogen self-doped porous graphite carbon.
Example 3
The embodiment discloses a preparation method of a nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst, which comprises the following steps:
s1, repeatedly washing mangosteen pericarp with deionized water, then drying at 100 ℃ for 12 hours, and crushing the dried mangosteen pericarp into powder to obtain a product A;
s2, under the protection of nitrogen, gradually heating the product A to 400 ℃ in a tubular furnace at a heating rate of 5 ℃/min, then pyrolyzing for 2 hours to obtain a dark black product, and grinding to obtain a product B;
s3, adding 10g of product B into 200mL of 0.05mol/L CoCl 2 Soaking the mixture in an aqueous solution for 8 hours under the condition of magnetic stirring, then carrying out solid-liquid separation to obtain a solid phase, drying the solid phase in a 60-DEG C oven, adding the dried solid phase into 200mL of KOH solution with the concentration of 0.1g/mL, soaking the mixture for 8 hours under the stirring state, separating the solid phase again, and drying the solid phase to obtain a product C;
s4, under the protection of nitrogen, heating the product C to 750 ℃ in a tubular furnace at a heating rate of 5 ℃/min, and then calcining for 2h to obtain a black product D;
s5, immersing the product D in HCl solution for 8 hours, then carrying out solid-liquid separation in a suction filtration mode, repeatedly washing with deionized water until the solution is neutral, drying at 70 ℃ for 12 hours, and then obtaining the nitrogen self-doped porous graphite carbon.
Example 4
The embodiment discloses a preparation method of a nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst, which comprises the following steps:
s1, repeatedly washing mangosteen pericarp with deionized water, drying at 100 ℃ for 12 hours, and crushing the dried mangosteen pericarp into powder to obtain a product A;
s2, under the protection of nitrogen, gradually heating the product A to 400 ℃ in a tubular furnace at a heating rate of 5 ℃/min, then pyrolyzing for 2h to obtain a dark black product, and grinding to obtain a product B;
s3, adding 10g of product B into 200mL of 0.05mol/L CoCl 2 Soaking in water solution under magnetic stirring for 8 hr, performing solid-liquid separation to obtain solid phase at 60 deg.CAfter drying in the oven, adding the dried product into 200mL of KOH solution with the concentration of 0.1g/mL, soaking for 8 hours under the stirring state, separating out a solid phase again, and drying to obtain a product C;
s4, under the protection of nitrogen, heating the product C to 800 ℃ in a tubular furnace at a heating rate of 5 ℃/min, and then calcining for 2h to obtain a black product D;
s5, immersing the product D in HCl solution for 8 hours, then carrying out solid-liquid separation in a suction filtration mode, repeatedly washing with deionized water until the solution is neutral, drying at 70 ℃ for 12 hours, and then obtaining the nitrogen self-doped porous graphite carbon.
Example 5
The embodiment discloses a preparation method of a nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst, which comprises the following steps:
s1, repeatedly washing mangosteen pericarp with deionized water, drying at 100 ℃ for 12 hours, and crushing the dried mangosteen pericarp into powder to obtain a product A;
s2, under the protection of nitrogen, gradually heating the product A to 400 ℃ in a tubular furnace at a heating rate of 5 ℃/min, then pyrolyzing for 2h to obtain a dark black product, and grinding to obtain a product B;
s3, adding 10g of product B into 200mL of 0.05mol/L CoCl 2 Soaking the mixture in an aqueous solution for 8 hours under the condition of magnetic stirring, then carrying out solid-liquid separation to obtain a solid phase, drying the solid phase in a 60-DEG C oven, adding the dried solid phase into 200mL of KOH solution with the concentration of 0.1g/mL, soaking the mixture for 8 hours under the stirring state, separating the solid phase again, and drying the solid phase to obtain a product C;
s4, under the protection of nitrogen, heating the product C to 850 ℃ in a tubular furnace at a heating rate of 5 ℃/min, and then calcining for 2h to obtain a black product D;
s5, immersing the product D in HCl solution for 8 hours, then carrying out solid-liquid separation in a suction filtration mode, repeatedly washing with deionized water until the solution is neutral, drying at 70 ℃ for 12 hours, and then obtaining the nitrogen self-doped porous graphite carbon.
As can be seen from fig. 1-6, the material exhibits a smoother surface when calcined at 600 ℃ (example 1), with some large pores formed, most of the structure being unactivated. As the calcination temperature is increased, the surface becomes increasingly rough and porous until the material exhibits a three-dimensional cellular porous structure with interconnections at 800 ℃, thereby increasing the specific surface area of the material. As the activation temperature was further increased to 850 ℃, the pore structure of the material began to collapse.
As can be seen from fig. 7, examples 1-5 all allowed nitrogen to be successfully doped into graphitic carbon.
As can be derived from fig. 8, the same type I isotherms were present in examples 1 and 2, indicating that the materials have a large amount of microporous structure and limited mesopores and macropores, whereas examples 3-5, isotherms of the materials were observed to be type I and type IV at moderate relative pressures (0.4< P/P0<0.9), and a hysteresis loop of type H4 was present, demonstrating the presence of microporous and mesoporous structures. Meanwhile, the adsorption isotherm curve of example 4 has a slightly increasing tendency at higher relative pressures (P/P0>0.90), corresponding to the presence of macropores, indicating that the material at this activation temperature achieves a meso-macroporous coexistence structure.
As can be seen from fig. 9, the power density of the material of example 4 used in a microbial fuel cell was slightly higher than that of platinum (Pt), while the power density of the other examples was lower.
As can be seen from fig. 10, in examples 1 to 5, the ratio of the D peak to the G peak decreases with increasing calcination temperature, the degree of graphitization thereof also increases, and in examples 3 to 5, a 2D peak, which is a characteristic peak of typical graphite carbon, appears.
From the above conclusions, it can be concluded that example 4 is a preferred embodiment.
The embodiments of the present invention have been described in detail above, but they are merely exemplary, and the present invention is not equivalent to the above described embodiments. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, it is intended that all equivalent alterations and modifications be included within the scope of the invention, without departing from the spirit and scope of the invention.
Claims (5)
1. The preparation method of the nitrogen self-doped porous graphitic carbon MFCs air cathode catalyst is characterized by comprising the following steps of:
s1, washing the mangosteen pericarp with deionized water repeatedly, drying at the temperature of 100-120 ℃, and crushing the dried mangosteen pericarp into powder to obtain a product A;
s2, heating the product A to 400 ℃ at a heating rate of 5-8 ℃/min under the protection of nitrogen, then pyrolyzing for 2-3h to obtain a dark black product, and grinding to obtain a product B;
s3, adding the product B into CoCl 2 Soaking in water solution under stirring for 6-10h, performing solid-liquid separation to obtain solid phase, drying, adding into KOH solution, reacting under stirring for 6-10h, separating solid phase again, and drying to obtain product C;
s4, heating the product C to 600-850 ℃ at a heating rate of 5-8 ℃/min under the protection of nitrogen, and then calcining for 2-3h to obtain a black product D;
s5, immersing the product D into an HCl solution for reaction for 8-12 hours, separating a solid phase, repeatedly washing the solid phase to be neutral by using deionized water, and drying to obtain the nitrogen self-doped porous graphite carbon.
2. The method of claim 1, wherein the drying of S1 is performed in an oven for 10-12 hours.
3. The method of preparing nitrogen self-doped porous graphitic carbon MFCs air cathode catalysts of claim 1, wherein the CoCl in S3 2 The concentration of the aqueous solution is 0.05mol/L, and the product B is mixed with CoCl 2 The mass ratio of (A) to (B) is 1:1-2: 1.
4. The method of claim 1, wherein the concentration of the KOH solution in S3 is 0.1g/mL, and the mass ratio of the product B to KOH is 1:1-1: 2.
5. The method of claim 1, wherein the product of S5 washed to neutrality with deionized water is dried at 60-80 ℃ for 10-12 hours.
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