CN112421061A - Method for preparing Fe-N-C oxygen reduction catalyst by taking pig blood as raw material - Google Patents
Method for preparing Fe-N-C oxygen reduction catalyst by taking pig blood as raw material Download PDFInfo
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- CN112421061A CN112421061A CN202011179356.8A CN202011179356A CN112421061A CN 112421061 A CN112421061 A CN 112421061A CN 202011179356 A CN202011179356 A CN 202011179356A CN 112421061 A CN112421061 A CN 112421061A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/9041—Metals or alloys
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
A method for preparing a Fe-N-C oxygen reduction catalyst by taking pig blood as a raw material belongs to the technical field of catalysts and preparation thereof. The method comprises the following steps: 1) drying commercially available pig blood; 2) placing the dried pig blood in a microwave reactor in Ar or N2Carrying out microwave reaction under protection, wherein the reaction power is 2000-3000W, and the reaction time is 15-20 min, so as to obtain black powder; 3) stirring the black powder in 0.5-3 mol/L dilute hydrochloric acid for 30-60 min, filtering, cleaning and drying. The Fe-N-C oxygen reduction catalyst obtained by the invention is of a structure rich in mesopores, has good electrocatalytic activity on oxygen reduction reaction, and has an initial potential of 0.91V and a half-wave potential of 0.74V; the method not only effectively utilizes the waste biomass resources, but also has the advantages of non-toxic and harmless preparation process, low cost, simple operation, easy industrial production and good industrial prospect.
Description
Technical Field
The invention belongs to the technical field of catalysts and preparation thereof, and particularly relates to a method for preparing a Fe-N-C oxygen reduction catalyst by taking pig blood as a raw material.
Background
Electrocatalytic oxygen reduction is a core reaction of many energy conversion and storage devices, such as fuel cells, metal air batteries. Carbon supported platinum and platinum alloy catalysts are the best currently recognized and most widely used oxygen reduction catalysts. Due to the limitations of high cost and low resources of noble metal catalysts such as platinum, non-noble metal catalysts have attracted more and more attention in recent years. Fe-N-C has the characteristics of high activity, high stability, low cost and the like, and is considered to be one of the most promising electrocatalytic materials for replacing platinum-based materials as cathode oxygen reduction of fuel cells and metal air cells. The Fe-N-C oxygen reduction catalyst is prepared by mixing, annealing and carbonizing proper carbon source, nitrogen source and iron source which are used as precursors. The Chinese invention patent discloses a Fe-N-C catalyst and a preparation method and application thereof (application number 201711337998.4), and discloses a synthesis method of a rich mesoporous Fe-N-C catalyst, which is limited by weakened adsorption between iron ions and a nitrogen source precursor, and is very limited by a carbon source, a nitrogen source and an iron source precursor which can be used for synthesizing the Fe-N-C oxygen reduction catalyst.
Pig blood contains a large amount of carbon, nitrogen, iron and other elements. The pig blood has rich iron content, the iron content of every 100 g of pig blood is up to 45 mg, the iron element in the pig blood mainly exists in the form of heme iron, and iron and nitrogen easily form a ring chelate structure Fe-N4, so that the pig blood is a good iron source, a nitrogen source and a carbon source. Based on the above discussion and analysis, if pig blood can be used as a raw material to synthesize the Fe-N-C oxygen reduction catalyst simply and rapidly at low cost, the method is a key for promoting the research and development of the Fe-N-C oxygen reduction catalyst to replace a platinum-based catalyst, and has important value for the development of fuel cells and metal air cells.
Disclosure of Invention
The invention aims to provide a low-cost and rapid preparation method of a Fe-N-C oxygen reduction catalyst.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing Fe-N-C oxygen reduction catalyst by taking pig blood as raw material is characterized by comprising the following steps:
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a method for preparing a Fe-N-C oxygen reduction catalyst by taking pig blood as a raw material, the obtained Fe-N-C oxygen reduction catalyst is of a structure rich in mesopores, has good electrocatalytic activity on oxygen reduction reaction, and has an initial potential of 0.91V and a half-wave potential of 0.74V.
2. The invention provides a method for preparing a Fe-N-C oxygen reduction catalyst by taking pig blood as a raw material, which not only effectively utilizes waste biomass resources, but also has the advantages of nontoxic and harmless preparation process, low cost, simple operation, easy industrial production and good industrial prospect.
Drawings
FIG. 1 is an SEM photograph of an Fe-N-C oxygen reduction catalyst prepared in example 1;
FIG. 2 is an SEM picture of the Fe-N-C oxygen reduction catalyst prepared in example 4;
FIG. 3 is a Raman diagram of the Fe-N-C oxygen reduction catalyst prepared in example 2;
FIG. 4 is a Raman diagram of the Fe-N-C oxygen reduction catalyst prepared in example 6;
FIG. 5 is an XPS survey of the Fe-N-C oxygen reduction catalyst prepared in example 2;
FIG. 6 is a linear polarization curve of the Fe-N-C oxygen reduction catalyst prepared in example 1;
FIG. 7 is a linear polarization curve of the Fe-N-C oxygen reduction catalyst prepared in example 4.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The pig blood used in the following examples of the present invention was commercially available pig blood without special treatment; the concentrated hydrochloric acid is commercially available analytically pure; the deionized water is self-made.
Example 1
Weighing 20g of commercially available pig blood, and drying in an oven at 80 ℃ for 1.5h to remove water in the pig blood; placing the dried pig blood in a microwave reactor, and carrying out microwave reaction for 15min under the protection of Ar gas flow and 2000W power to obtain black powder; placing the obtained black powder in 0.5mol/L dilute hydrochloric acid, and stirring for 30min to remove other impurities; filtering, washing the black powder with deionized water, and drying to obtain the Fe-N-C oxygen reduction catalyst. The weight of the Fe-N-C oxygen reduction catalyst was weighed out to be 7.5 g.
Example 2
Weighing 20g of commercially available pig blood, and drying in an oven at 90 ℃ for 1h to remove water in the pig blood; placing the dried pig blood in a microwave reactor in N2Carrying out microwave reaction for 18min under the protection of airflow and the power of 2300W to obtain black powder; placing the obtained black powder in 0.5mol/L dilute hydrochloric acid, and stirring for 30min to remove other impurities; filtering, washing the black powder with deionized water, and drying to obtain the Fe-N-C oxygen reduction catalyst. The weight of the Fe-N-C oxygen reduction catalyst was weighed out to be 7.8 g.
Example 3
Weighing 20g of commercially available pig blood, and drying in an oven at 80 ℃ for 2h to remove water in the pig blood; placing the dried pig blood in a microwave reactor in N2Carrying out microwave reaction for 15min under the protection of airflow and under the power of 2700W to obtain black powder; placing the obtained black powder in 1mol/L diluted hydrochloric acid, and stirring for 30min to remove other impurities; filtering, washing the black powder with deionized water, and drying to obtain the Fe-N-C oxygen reduction catalyst. The weight of the Fe-N-C oxygen reduction catalyst was weighed out to be 7.3 g.
Example 4
Weighing 20g of commercially available pig blood, and drying in an oven at 100 ℃ for 1h to remove water in the pig blood; placing the dried pig blood in a microwave reactor, and carrying out microwave reaction for 20min under the protection of Ar gas flow and 3000W power to obtain black powder; placing the obtained black powder in 1mol/L diluted hydrochloric acid, and stirring for 30min to remove other impurities; filtering, washing the black powder with deionized water, and drying to obtain the Fe-N-C oxygen reduction catalyst. The weight of the Fe-N-C oxygen reduction catalyst was weighed out to be 7.1 g.
Example 5
Weighing 20g of commercially available pig blood, and drying in an oven at 90 ℃ for 1.5h to remove water in the pig blood; placing the dried pig blood in a microwave reactor, and carrying out microwave reaction for 15min under the protection of Ar gas flow and 3000W power to obtain black powder; placing the obtained black powder in 2mol/L diluted hydrochloric acid, and stirring for 30min to remove other impurities; filtering, washing the black powder with deionized water, and drying to obtain the Fe-N-C oxygen reduction catalyst. The weight of the Fe-N-C oxygen reduction catalyst was weighed out to be 7.2 g.
Example 6
Weighing 20g of commercially available pig blood, and drying in an oven at 80 ℃ for 2h to remove water in the pig blood; placing the dried pig blood in a microwave reactor, and carrying out microwave reaction for 19min under the protection of Ar gas flow and the power of 2800W to obtain black powder; placing the obtained black powder in 0.5mol/L dilute hydrochloric acid, and stirring for 30min to remove other impurities; filtering, washing the black powder with deionized water, and drying to obtain the Fe-N-C oxygen reduction catalyst. The weight of the Fe-N-C oxygen reduction catalyst was weighed out to be 7.2 g.
FIG. 1 is an SEM photograph of an Fe-N-C oxygen reduction catalyst prepared in example 1; as can be seen from FIG. 1, the surface of the Fe-N-C oxygen reduction catalyst exhibits a porous structure, and mesopores having a diameter of about 50nm are densely distributed on the surface of the Fe-N-C oxygen reduction catalyst. The porous structure is beneficial to the diffusion of oxygen, increases the contact area of the oxygen and the Fe-N-C oxygen reduction catalyst, and increases the active area of the Fe-N-C oxygen reduction catalyst.
FIG. 2 is an SEM picture of the Fe-N-C oxygen reduction catalyst prepared in example 4; as can be seen from FIG. 2, the surface of the Fe-N-C oxygen reduction catalyst exhibits a porous structure, and mesopores having a diameter of about 100nm are densely distributed on the surface of the Fe-N-C oxygen reduction catalyst.
FIG. 3 is a Raman diagram of the Fe-N-C oxygen reduction catalyst prepared in example 2; as can be seen from FIG. 3, the respective concentrations of the Fe-N-C oxygen reduction catalysts were 1354cm-1And 1578cm-1There are strong peaks representing the D-band and G-band of graphitic carbon, respectively.
FIG. 4 is a Raman diagram of the Fe-N-C oxygen reduction catalyst prepared in example 6; as can be seen from FIG. 4, the respective concentrations of the Fe-N-C oxygen reduction catalysts were 1354cm-1And 1578cm-1There are strong peaks representing the D-band and G-band of graphitic carbon, respectively.
FIG. 5 is an XPS survey of the Fe-N-C oxygen reduction catalyst prepared in example 2; as can be seen from FIG. 5, the Fe-N-C oxygen reduction catalyst consists primarily of C, N, Fe, with O likely being an impurity peak during the test.
FIG. 6 is a linear polarization curve of the Fe-N-C oxygen reduction catalyst prepared in example 1; as can be seen from FIG. 6, the peak potential of platinum carbon is 0.925V, and the half-wave potential is 0.754V; the peak potential of the Fe-N-C oxygen reduction catalyst is 0.874V, and the half-wave potential is 0.705V. The prepared Fe-N-C oxygen reduction catalyst is equivalent to platinum carbon in performance.
FIG. 7 is a linear polarization curve of the Fe-N-C oxygen reduction catalyst prepared in example 4; as is clear from FIG. 7, the peak potential of the Fe-N-C oxygen reduction catalyst was 0.911V, the half-wave potential was 0.743V, and the oxygen reduction performance was comparable to that of platinum-carbon.
Claims (1)
1. A method for preparing Fe-N-C oxygen reduction catalyst by taking pig blood as raw material is characterized by comprising the following steps:
step 1, drying commercially available pig blood;
step 2, placing the dried pig blood in the step 1 into a microwave reactor, and adding Ar or N2Carrying out microwave reaction under the protection of airflow, wherein the reaction power of a microwave reactor is 2000-3000W, the microwave reaction time is 15-20 min, and black powder is obtained after the reaction is finished;
step 3, placing the black powder obtained in the step 2 in 0.5-3 mol/L diluted hydrochloric acid, and stirring for 30-60 min; filtering, cleaning and drying to obtain the Fe-N-C oxygen reduction catalyst.
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