CN110808380B - Preparation method of Prussian blue oxygen doped reductive cathode film - Google Patents

Preparation method of Prussian blue oxygen doped reductive cathode film Download PDF

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CN110808380B
CN110808380B CN201910975387.5A CN201910975387A CN110808380B CN 110808380 B CN110808380 B CN 110808380B CN 201910975387 A CN201910975387 A CN 201910975387A CN 110808380 B CN110808380 B CN 110808380B
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prussian blue
cathode
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CN110808380A (en
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刘佳
许润钒
郁美莹
陈雪鹏
何伟华
李楠
冯玉杰
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Tianjin University
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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
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • H01M4/8828—Coating with slurry or ink
    • 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
    • H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
    • H01M4/8673—Electrically conductive fillers
    • 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
    • H01M4/88—Processes of manufacture
    • H01M4/8803—Supports for the deposition of the catalytic active composition
    • 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
    • H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
    • H01M2004/8689—Positive electrodes
    • 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

The invention relates to a preparation method of a cathode film doped with Prussian blue for improving oxygen reduction performance. Mixing one of polyvinylidene fluoride, polyvinyl chloride and polyether sulfone with an organic polymer film-forming pore-forming agent, dissolving and standing in an N, N-dimethylacetamide solution to obtain a homogeneous solution without bubbles; mixing polypyrrole, polyaniline and Prussian blue according to a mass ratio of 8:1: 1-8: 1:2, uniformly mixing the mixed material and the bubble-removed homogeneous solution according to a mass ratio (0.3-0.4 g) of 1mL, and performing ultrasonic treatment for 30-40min to prepare a conductive film solution; and soaking the stainless steel mesh coated with the conductive film liquid into deionized water to form the film, thus obtaining the Prussian blue doped cathode film. The conductivity of the Prussian blue doped cathode film is 18.4ms cm at most‑19.9ms cm from a blank cathode‑1The conductivity of the alloy is improved by 86 percent.

Description

Preparation method of Prussian blue oxygen doped reductive cathode film
Technical Field
The invention relates to a preparation method of a cathode film doped with Prussian blue for improving oxygen reduction performance.
Background
The wastewater is a potential energy substance, the potential energy contained in the wastewater is about 10 times of the energy consumption for treating the wastewater, the potential energy of the wastewater produced every day in the world is about equal to one hundred million tons of standard fuel oil, and the potential energy development of the wastewater can solve the total power consumption of the society, so that the realization of high-grade water quality recovery and energy utilization is a difficult problem in the current water treatment field while the problem of wastewater treatment is solved.
The Microbial Fuel Cell (MFC) technology can convert chemical energy in the biodegradable substances in the wastewater into electric energy by utilizing the anaerobic catalysis of microorganisms, so that the synchronous recovery of the treatment of the sewage and the electric energy is realized. The system mainly comprises an anode and a cathode. Wherein, the microorganism in the anode area degrades the substrate and simultaneously generates proton and electron, the proton diffuses to the surface of the cathode in the solution, and the electron finally reaches the cathode through an external circuit so as to form a complete battery loop. The microbial fuel cell technology has a wide development space due to the reasons of small temperature influence, few operation condition limiting factors and the like, and is one of the research hotspots in the field of environmental engineering in recent years.
The performance of the cathode is a key factor for limiting the output power of the MFC, and the cathode has good catalytic activity, high oxygen transfer efficiency and high oxygen reduction rate. The common cathode catalyst is activated carbon, but the reduction rate of a cathode electron acceptor oxygen on the surface of a carbon material is low, so that high activation loss and high overpotential are caused, the current microbial fuel cell has the power generation efficiency of only 40% -50%, and the cathode potential is reduced by 300-400 mV due to slow cathode reaction kinetics. Theoretically, the higher the cathode potential, the lower the anode potential, and the higher the MFC output voltage value. Therefore, in an MFC coupling system, a cathode film with high-efficiency catalytic performance and stable operation is developed, and the improvement of system energy output and wastewater treatment effect is facilitated.
Prussian blue has a face-centered cubic lattice structure similar to zeolite, is a porous catalytic material with high pores and high specific surface area, and is beneficial to exposing catalytic active centers. Meanwhile, the material has the characteristics of good electrochemical performance, conductivity and the like. Therefore, the Prussian blue is added into the traditional cathode film, so that the charge transfer resistance of the cathode can be effectively reduced, the oxygen reduction catalytic reaction rate of the cathode is improved, the output power of an MFC system is improved, and the efficient recovery of clean energy is realized.
Disclosure of Invention
The invention provides a preparation method of a Prussian blue oxygen doped reducing cathode film. The Prussian blue has the advantages of excellent electrochemical reversibility, high stability, easiness in preparation and the like, and is doped in the cathode film, so that the conductivity of the cathode film is improved, the charge transfer resistance of the cathode is effectively reduced, the oxygen reduction catalytic reaction rate of the cathode is improved, the output power of an MFC system is further improved, and the problem of high oxygen reduction activation loss of the MFC system is solved. In order to solve the problems in the prior art, the invention provides a preparation method of a Prussian blue doped cathode film, which comprises the following steps:
the technical scheme of the invention is as follows:
a preparation method of a Prussian blue oxygen doped reducing cathode film; the method comprises the following steps:
(1) mixing one of polyvinylidene fluoride, polyvinyl chloride and polyether sulfone and an organic polymer film-forming pore-forming agent according to a certain mass ratio at the temperature of 30-35 ℃, dissolving in an N, N-dimethylacetamide solution, wrapping with tin foil, stirring for 5-7h in the dark, and standing for 6-7h to obtain a homogeneous solution without bubbles; mixing polypyrrole, polyaniline and Prussian blue according to a mass ratio of 8:1: 1-8: 1:2, uniformly mixing the mixed material and the bubble-removed homogeneous solution according to a mass ratio (0.3-0.4 g) of 1mL, and performing ultrasonic treatment for 30-40min to prepare a conductive film solution;
(2) according to the step (1), the loading amount of the activated carbon powder in the conductive film liquid is 25-27 mg cm–2Uniformly coating the conductive film liquid prepared in the step (2) on an effective area of 7cm by using a spatula2The stainless steel net has a single surface;
(3) and (3) soaking the stainless steel mesh coated with the conductive film liquid in the step (2) into deionized water for 20-30min, and forming the film to obtain the Prussian blue doped cathode film.
The organic polymer film-forming pore-forming agent in the step 1) is one of polyethylene glycol, potassium bicarbonate and polyvinylpyrrolidone.
In the step 1), the mixing mass ratio of one of polyvinylidene fluoride, polyvinyl chloride and polyether sulfone to the organic polymer film-forming pore-forming agent is 2: (1-1.5).
The mass ratio of one of polyvinylidene fluoride, polyvinyl chloride and polyether sulfone to N, N-dimethylacetamide in the step 1) is 1 (10-13).
The invention has the following advantages:
1. the invention takes the stainless steel mesh as the membrane electrode support body, and the membrane electrode materials are directly coated on the two sides of the stainless steel mesh, thereby realizing the integral molding of the membrane electrode and simplifying the preparation process of the membrane electrode.
2. Oxygen reduction in the present invention is characterized by LSV, EIS, Tafel curves and conductivity tests. The larger the current density corresponding to-0.1V obtained by LSV test is, the smaller the charge transfer resistance value in EIS test is, the larger the exchange current density and the higher the conductivity value in Tafel curve are, the better the oxygen reduction performance of the cathode film is shown. Under the voltage of-0.1V, the maximum current density of the Prussian blue doped cathode film reaches 11.9A m-26.0A m from blank electrode-2Compared with the product, the product is increased by 99%. The polarization internal resistance is reduced, the charge transfer internal resistance of the Prussian blue doped cathode film is at least 3.4 omega, and is reduced by 74 percent compared with the charge transfer internal resistance of the blank 13.4 omega, and the highest exchange current density of the cathode film is 1.7 multiplied by 10 through Tafel test-4A m-21.2X 10 with a blank cathode-4A m-2The exchange current density of (a) was improved by 42%. The conductivity of the Prussian blue doped cathode film is 18.4ms cm at most-19.9ms cm from a blank cathode-1The conductivity is improved by 86 percent; the results show that the Prussian blue doping is beneficial to improving the catalytic efficiency of oxygen reduction.
Drawings
Fig. 1 is an LSV curve of an electrode, where a is a blank filter electrode, b is the prussian blue doped cathode film of example one, c is the prussian blue doped cathode film of example two, and d is the prussian blue doped cathode film of example three.
Fig. 2 is an EIS curve of an electrode, where a is a blank filter electrode, b is an example prussian blue doped cathode film, c is an example prussian blue doped cathode film, and d is an example third prussian blue doped cathode film.
Fig. 3 is a Tafel curve of an electrode, where a is a blank filter electrode, b is an example doped prussian blue cathode film, c is an example doped prussian blue cathode film, and d is an example three doped prussian blue cathode film.
Fig. 4 shows the conductivity of the electrode, a is a blank filter electrode, b is the prussian blue doped cathode film of the example, c is the prussian blue doped cathode film of the example two, and d is the prussian blue doped cathode film of the example three.
Detailed Description
The present invention is further described by the following embodiments with reference to the drawings, but it should be noted that the embodiments are not to be construed as limiting the scope of the present invention.
Example one
This example illustrates a method for preparing and characterizing a prussian blue oxygen doped reductive cathode film according to the present invention. The method comprises the following steps:
(1) mixing polyether sulfone and potassium bicarbonate according to a mass ratio of 2:1 at the temperature of 30 ℃, dissolving in an N, N-dimethylacetamide solution, wrapping with tinfoil, stirring in the dark for 5 hours, and standing for 6 hours to obtain a bubble-removed homogeneous solution, wherein the mass ratio of the polyether sulfone to the N, N-dimethylacetamide is 1: 10. Mixing polypyrrole, polyaniline and Prussian blue according to a mass ratio of 8:1:1, uniformly mixing the mixed material and the bubble-removed homogeneous solution according to a mass ratio of 0.3g:1mL, and performing ultrasonic treatment for 30min to prepare a conductive film solution;
(2) the polypyrrole loading in the conductive film liquid in the step (1) is 25mg cm-2Uniformly coating the conductive film liquid prepared in the step (1) on an effective area of 7cm by using a spatula2The stainless steel net has a single surface;
(3) and (3) soaking the stainless steel net with the conductive film liquid in the step (2) in deionized water for 20min to form 3 film, and obtaining the Prussian blue doped cathode film.
The characterization method of the first embodiment is as follows:
characterization method 1: the LSV curve of the film was measured and the current density of the Prussian blue doped cathode film of example one reached 9.9Am at-0.1V as shown in b of FIG. 1-2And a blank filter membrane electrode 6.0Am-2(FIG. 1-a) the current density is increased by 65% compared to;
characterization method 2: the EIS curve of the film was measured and as shown in fig. 2 b, the charge transfer resistance of the prussian blue doped cathode film of example one was 4.8 Ω, which was reduced by 64% compared to the charge transfer resistance of the blank cathode 13.4 Ω (fig. 2 a);
characterization method 3: measuring Tafel curve of the membrane, and obtaining exchange through curveCurrent Density, as shown in b in FIG. 3, the exchange Current Density of Prussian blue doped cathode film in the first example is 1.4X 10-4A m-21.2X 10 with a blank cathode- 4Am-2The exchange current density of (FIG. 3-a) was increased by 16%.
Characterization method 4: the conductivity of the film was measured, and as shown in b of FIG. 4, the conductivity of the Prussian blue doped cathode film in example one was 13.0ms cm-19.9ms cm from a blank cathode-1(FIG. 4-a) the conductivity was increased by 31% compared to the conductivity.
Example two
This example illustrates a method for preparing and characterizing a prussian blue oxygen doped reductive cathode film according to the present invention. The method comprises the following steps:
(1) mixing polyvinyl chloride and polyvinylpyrrolidone according to a mass ratio of 2:1.2 at the temperature of 32 ℃, dissolving in an organic solvent N, N-dimethylacetamide solution, wrapping with tinfoil, stirring for 6h in the dark, and standing for 6.5h to obtain a bubble-removed homogeneous solution; the mass ratio of the polyvinyl chloride to the N, N-dimethylacetamide is 1: 12. Mixing polypyrrole, polyaniline and Prussian blue according to a mass ratio of 8:1:1.5, uniformly mixing the mixed material and the bubble-removed homogeneous solution according to a mass ratio of 0.35g:1mL, and performing ultrasonic treatment for 35min to prepare a conductive film solution;
(2) the polypyrrole loading amount in the conductive film liquid according to the step (1) is 26mg cm-2Uniformly coating the conductive film liquid prepared in the step (1) on an effective area of 7cm by using a spatula2The stainless steel net has a single surface;
(3) and (3) soaking the stainless steel mesh with the conductive film liquid in the step (2) in deionized water for 25min to obtain the Prussian blue doped cathode film.
Example two characterization methods were as follows:
characterization method 1: the LSV curve of the film was measured and the current density of the Prussian blue doped cathode film of example two reached 10.7Am at-0.1V as shown in c of FIG. 1-2And a blank filter membrane electrode 6.0Am-2(FIG. 1-a) the current density is increased by 78%;
characterization method 2: the EIS curve of the film was measured and as shown in fig. 2 c, the charge transfer resistance of the prussian blue doped cathode film of example two was 3.6 Ω, which was a 73% reduction compared to the charge transfer resistance of the blank cathode 13.4 Ω (fig. 2-a);
characterization method 3: the Tafel curve of the membrane was measured and the exchange current density was obtained from the curve, as shown in fig. 3 c, in the example of the Prussian blue doped cathode membrane of 1.6X 10-4A m-21.2X 10 with a blank cathode-4A m-2The exchange current density of (FIG. 3-a) was increased by 33%.
Characterization method 4: the conductivity of the film was measured, and as shown in c of FIG. 4, the conductivity of the Prussian blue doped cathode film of example two was 15.2ms cm-19.9ms cm from a blank cathode-1(FIG. 4-a) the conductivity was improved by 53%;
EXAMPLE III
This example illustrates a method for preparing and characterizing a prussian blue oxygen-doped reductive cathode film, which comprises the following steps:
(1) mixing polyvinylidene fluoride and polyethylene glycol according to a mass ratio of 2:1.5 at the temperature of 35 ℃, dissolving in an N, N-dimethylacetamide solution, wrapping with tinfoil, stirring for 7 hours in a dark place, and standing for 7 hours to obtain a bubble-removed homogeneous solution; the mass ratio of the polyvinylidene fluoride to the N, N-dimethylacetamide is 1: 13; mixing conductive materials of polypyrrole, polyaniline and Prussian blue according to a mass ratio of 8:1:2, uniformly mixing the mixed materials and the homogeneous solution without bubbles in the mixed materials according to a mass ratio of 0.4g:1mL, and performing ultrasonic treatment for 40min to prepare a conductive membrane solution;
(2) the polypyrrole loading in the conductive film liquid according to the step (1) is 27mg cm-2Uniformly coating the conductive film liquid prepared in the step (1) on an effective area of 7cm by using a spatula2The stainless steel net has a single surface;
(3) and (3) soaking the stainless steel mesh with the conductive film liquid in the step (2) in deionized water for 30min to obtain the Prussian blue doped cathode film.
The characterization method of example three is as follows:
characterization method 1: measuring the LSV curve of the film, e.g.As shown in d of fig. 1, the current density of the prussian blue doped cathode film in the third example reaches 11.9Am at-0.1V-2And a blank filter membrane electrode 6.0Am-2(FIG. 1-a) the current density is increased by 99% compared to;
characterization method 2: the EIS curve of the film was measured and as shown by d in fig. 2, the charge transfer resistance of the prussian blue doped cathode film in example three was 3.4 Ω, which is a 74% reduction compared to the charge transfer resistance of the blank cathode 13.4 Ω (fig. 2-a);
characterization method 3: the Tafel curve of the membrane was measured and the exchange current density was obtained from the curve, as shown by d in FIG. 3, and the exchange current density of the Prussian blue doped cathode membrane in example three was 1.7X 10-4Am-21.2X 10 with a blank cathode- 4Am-2The exchange current density of (FIG. 3-a) was increased by 42%.
Characterization method 4: the conductivity of the film was measured and as shown by d in fig. 4, the conductivity of the prussian blue doped cathode film in example three was 18.4ms cm-19.9ms cm from a blank cathode-1(FIG. 4-a) the conductivity was increased by 86% compared to the conductivity;
while the methods and techniques of the present invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and/or modifications of the methods and techniques described herein may be made without departing from the spirit and scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.

Claims (1)

1. A preparation method of a Prussian blue oxygen doped reducing cathode film; the method comprises the following steps:
(1) at the temperature of 30-35 ℃, polyether sulfone and an organic polymer film-forming pore-forming agent are mixed according to a certain mass ratio, dissolved in an N, N-dimethylacetamide solution, wrapped by tinfoil, stirred in the dark for 5-7h, and kept stand for 6-7h to obtain a bubble-removed homogeneous solution; mixing polypyrrole, polyaniline and Prussian blue according to a mass ratio of 8:1: 1-8: 1:2, uniformly mixing the mixed material and the bubble-removed homogeneous solution according to a mass ratio (0.3-0.4 g) of 1mL, and performing ultrasonic treatment for 30-40min to prepare a conductive film solution;
(2) carrying 25-27 mg cm of polypyrrole in the conductive film liquid according to the step (1)–2Uniformly coating the conductive film liquid prepared in the step (1) on an effective area of 7cm by using a spatula2The stainless steel net has a single surface;
(3) soaking the stainless steel mesh coated with the conductive film liquid in the step (2) into deionized water for 20-30min to form a film, thus obtaining a Prussian blue doped cathode film;
the organic polymer film-forming pore-forming agent in the step (1) is one of polyethylene glycol and potassium bicarbonate; the mixing mass ratio of the polyether sulfone to the organic polymer film-forming pore-forming agent is 2: (1-1.5); the mass ratio of the polyether sulfone to the N, N-dimethylacetamide is 1 (10-13).
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