CN107799796A - A kind of anode of microbial fuel cell of nitrogen modification and preparation method thereof - Google Patents

A kind of anode of microbial fuel cell of nitrogen modification and preparation method thereof Download PDF

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Publication number
CN107799796A
CN107799796A CN201710846141.9A CN201710846141A CN107799796A CN 107799796 A CN107799796 A CN 107799796A CN 201710846141 A CN201710846141 A CN 201710846141A CN 107799796 A CN107799796 A CN 107799796A
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fuel cell
anode
microbial fuel
preparation
nitrogen modification
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李伟善
李鸿英
廖波
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South China Normal University
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South China Normal 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
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
    • 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
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • H01M4/8846—Impregnation
    • 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
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8882—Heat treatment, e.g. drying, baking
    • H01M4/8885—Sintering or firing
    • H01M4/8889—Cosintering or cofiring of a catalytic active layer with another type of layer
    • 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
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8892—Impregnation or coating of the catalyst layer, e.g. by an ionomer
    • 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
    • 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
    • H01M2004/8684—Negative 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inert Electrodes (AREA)

Abstract

The invention belongs to microbiological fuel cell field, discloses a kind of anode of microbial fuel cell of nitrogen modification and preparation method thereof.The preparation method is：Compound containing manganese, zinc or tungsten and egg are added to the water, is dispersed with stirring uniformly, obtains mixed solution；Carbon carrier is added in above-mentioned mixed solution, taken out after supersound process, cleaning, dry, then in nitrogen atmosphere and 800~1000 DEG C of 10~30min of temperature lower calcination, then gained carbon carrier is added in the monomer solution of conducting polymer, conducting polymer is prepared by electro-deposition on the carbon carrier, obtains the anode of microbial fuel cell of the nitrogen modification.Gained anode of microbial fuel cell material of the invention has big specific surface area, and the anode material after nitrogen modification has preferable compatibility with microorganism, is advantageous to the formation of biomembrane and improves the power density of microbiological fuel cell.

Description

A kind of anode of microbial fuel cell of nitrogen modification and preparation method thereof
Technical field
The invention belongs to microbiological fuel cell field, and in particular to a kind of anode of microbial fuel cell of nitrogen modification and Its preparation method.
Background technology
Microbiological fuel cell (MFC) is a New Environment Protection Technology for applying to living resources in electrochemistry.With Global resources shortage and problem of environmental pollution become increasingly conspicuous, and greatly embody the advantages of MFC, i.e., are sent out using discarded object Electricity.Wastewater treatment, biotic environment reparation, the electric energy of the special dimension such as deep-sea and space uses all has close ties with MFC.So And power output extremely low MFC is always to restrict a key factor of its development.
The electron transfer process of MFC anodes is an important step of energy conversion, is had extremely to the transformation efficiency of energy Important influence, it is the crucial point of penetration for improving microbiological fuel cell performance.And the formation of anode biomembrane can promote electronics Quick transmission from microorganism to electrode, can make MFC more efficiently work.
The content of the invention
In place of shortcoming and defect existing for above prior art, primary and foremost purpose of the invention is that providing a kind of nitrogen repaiies The preparation method of the anode of microbial fuel cell of decorations.
Another object of the present invention is to provide a kind of Microbial fuel for the nitrogen modification being prepared by the above method Galvanic anode.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of the anode of microbial fuel cell of nitrogen modification, including following preparation process：
(1) compound containing manganese, zinc or tungsten and egg are added to the water, are dispersed with stirring uniformly, obtain mixed solution；
(2) carbon carrier is added in mixed solution obtained by step (1), taken out after supersound process, cleaned, dry, then In nitrogen atmosphere and 800~1000 DEG C of 10~30min of temperature lower calcination, the carbon carrier of the supported catalyst of nitrogen modification is obtained；
(3) carbon carrier obtained by step (2) is added in the monomer solution of conducting polymer, by being electrodeposited in carbon carrier On prepare conducting polymer, obtain the anode of microbial fuel cell of nitrogen modification.
Preferably, the mass percent containing manganese, zinc or tungsten compound and egg described in step (1) be 0.5%~ 2%；The mass ratio of egg and water is 1:(1~2).
Preferably, carbon carrier described in step (2) is one kind in biomass carbon, carbon felt and carbon cloth.
Preferably, cleaning refers to be cleaned with deionized water described in step (2), and the drying refers in 60~80 DEG C of temperature Lower drying.
Preferably, the monomer solution of conducting polymer refers to chromium solution, aniline solution and 3,4- second described in step (3) At least one of alkene dioxy thiophene solution；The mass concentration of the monomer solution of conducting polymer is 0.5%~5%.
Preferably, the condition of electro-deposition is described in step (3)：It is to electricity by reference electrode, platinum electrode of calomel electrode Pole and carbon carrier are that working electrode forms a battery, and speed is swept from 0V to 0.6V with 10mV/s.
A kind of anode of microbial fuel cell of nitrogen modification, is prepared by the above method.
The present invention principle be：By the nitrogen compound in egg with compound of the absorption containing manganese, zinc or tungsten in ultrasound During adsorb on the carbon carrier, after calcining, the nitrogenous electrode of gained is advantageous to the formation of biomembrane, and based on containing manganese, zinc Or the catalytic of the compound of tungsten, be advantageous to the growth of microorganism.Meanwhile the deposition of conducting polymer is advantageous to the biography of electronics Pass.So as to it improve the power density of microbiological fuel cell.
The preparation method of the present invention and the anode of microbial fuel cell of resulting nitrogen modification have the following advantages that and had Beneficial effect：
Gained anode of microbial fuel cell material of the invention has big specific surface area, and the anode material after nitrogen modification Material has preferable compatibility with microorganism, is advantageous to the formation of biomembrane and improves the power density of microbiological fuel cell.
Brief description of the drawings
Fig. 1 is the circulation of the microbiological fuel cell prepared using the gained anode of embodiment 1 and unmodified carbon felt as anode Volt-ampere curve figure；
Fig. 2 is the gained anode of embodiment 1 and unmodified carbon felt to opsonigenous substance (H2) catalysis oxidation result figure；
Fig. 3 is the polarization of the microbiological fuel cell prepared using the gained anode of embodiment 1 and unmodified carbon felt as anode Curve and power density curve map.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited In this.
Embodiment 1
The preparation method of the anode of microbial fuel cell of the nitrogen modification of the present embodiment, specific preparation process are as follows：
(1) 0.25g tungsten-carbide powders and 30g Fresh Eggs are added to clearly in 30g deionized waters, are dispersed with stirring uniformly, Obtain mixed solution；
(2) 3cm*3cm carbon felt is added in mixed solution obtained by step (1), taken after being ultrasonically treated 20min Go out, cleaned with deionized water, use tube furnace to be obtained in nitrogen atmosphere and 900 DEG C of temperature lower calcination 15min after 80 DEG C of forced air dryings The carbon felt of the supported catalyst of nitrogen modification；
(3) carbon felt obtained by step (2) is added in the chromium solution that mass concentration is 2%, by being electrodeposited in carbon felt Preparing conducting polymer, (condition of electro-deposition is：It is work to electrode and carbon felt to be as reference electrode, platinum electrode using calomel electrode Electrode forms a battery, and speed is swept from 0V to 0.6V with 10mV/s), obtain the microbiological fuel cell sun of the nitrogen modification Pole.
Embodiment 2
The preparation method of the anode of microbial fuel cell of the nitrogen modification of the present embodiment, specific preparation process are as follows：
(1) 0.25g manganese oxide powders and 30g Fresh Eggs are added to clearly in 60g deionized water water, are dispersed with stirring It is even, obtain mixed solution；
(2) 3cm*3cm carbon cloth is added in mixed solution obtained by step (1), taken after being ultrasonically treated 30min Go out, cleaned with deionized water, use tube furnace to be obtained in nitrogen atmosphere and 1000 DEG C of temperature lower calcination 15min after 60 DEG C of forced air dryings To the carbon cloth of the supported catalyst of nitrogen modification；
(3) carbon cloth obtained by step (2) is added in the chromium solution that mass concentration is 5%, by being electrodeposited in carbon cloth Preparing conducting polymer, (condition of electro-deposition is：It is work to electrode and carbon cloth to be as reference electrode, platinum electrode using calomel electrode Electrode forms a battery, and speed is swept from 0V to 0.6V with 10mV/s), obtain the microbiological fuel cell sun of the nitrogen modification Pole.
Embodiment 3
The preparation method of the anode of microbial fuel cell of the nitrogen modification of the present embodiment, specific preparation process are as follows：
(1) 0.5g Zinc oxide powders and 30g Fresh Eggs are added to clearly in 40g deionized water water, are dispersed with stirring uniformly, Obtain mixed solution；
(2) 3cm*3cm carbon cloth is added in mixed solution obtained by step (1), taken after being ultrasonically treated 30min Go out, cleaned with deionized water, use tube furnace to be obtained in nitrogen atmosphere and 900 DEG C of temperature lower calcination 30min after 60 DEG C of forced air dryings The carbon cloth of the supported catalyst of nitrogen modification；
(3) carbon cloth obtained by step (2) is added in the aniline solution that mass concentration is 0.5%, by being electrodeposited in carbon Cloth prepares conducting polymer, and (condition of electro-deposition is：It is for work to electrode and carbon cloth by reference electrode, platinum electrode of calomel electrode Make electrode and form a battery, speed is swept from 0V to 0.6V with 10mV/s), obtain the microbiological fuel cell sun of the nitrogen modification Pole.
Embodiment 4
The preparation method of the anode of microbial fuel cell of the nitrogen modification of the present embodiment, specific preparation process are as follows：
(1) 0.2g tungsten-carbide powders and 30g Fresh Eggs are added to clearly in 50g deionized water water, are dispersed with stirring uniformly, Obtain mixed solution；
(2) 3cm*3cm carbon felt is added in mixed solution obtained by step (1), taken after being ultrasonically treated 30min Go out, cleaned with deionized water, use tube furnace to be obtained in nitrogen atmosphere and 950 DEG C of temperature lower calcination 20min after 60 DEG C of forced air dryings The carbon felt of the supported catalyst of nitrogen modification；
(3) carbon felt obtained by step (2) is added in the aniline solution that mass concentration is 1%, by being electrodeposited in carbon cloth Preparing conducting polymer, (condition of electro-deposition is：It is work to electrode and carbon felt to be as reference electrode, platinum electrode using calomel electrode Electrode forms a battery, and speed is swept from 0V to 0.6V with 10mV/s), obtain the microbiological fuel cell sun of the nitrogen modification Pole.
Embodiment 5
The preparation method of the anode of microbial fuel cell of the nitrogen modification of the present embodiment, specific preparation process are as follows：
(1) 0.3g tungsten-carbide powders and 30g Fresh Eggs are added to clearly in 60g deionized water water, are dispersed with stirring uniformly, Obtain mixed solution；
(2) 3cm*3cm carbon cloth is added in mixed solution obtained by step (1), taken after being ultrasonically treated 30min Go out, cleaned with deionized water, use tube furnace to be obtained in nitrogen atmosphere and 1000 DEG C of temperature lower calcination 30min after 60 DEG C of forced air dryings To the carbon cloth of the supported catalyst of nitrogen modification；
(3) carbon cloth obtained by step (2) is added in the 3,4-rthylene dioxythiophene solution that mass concentration is 1%, passed through Carbon cloth is electrodeposited in prepare conducting polymer (condition of electro-deposition is：It is to electrode by reference electrode, platinum electrode of calomel electrode It is that working electrode forms a battery with carbon cloth, speed is swept from 0V to 0.6V with 10mV/s), obtain the microorganism of the nitrogen modification Anode of fuel cell.
Embodiment 6
The preparation method of the anode of microbial fuel cell of the nitrogen modification of the present embodiment, specific preparation process are as follows：
(1) 0.25g manganese oxide powders and 30g Fresh Eggs are added to clearly in 40g deionized water water, are dispersed with stirring It is even, obtain mixed solution；
(2) 3cm*3cm carbon cloth is added in mixed solution obtained by step (1), taken after being ultrasonically treated 30min Go out, cleaned with deionized water, use tube furnace to be obtained in nitrogen atmosphere and 950 DEG C of temperature lower calcination 15min after 60 DEG C of forced air dryings The carbon cloth of the supported catalyst of nitrogen modification；
(3) carbon cloth obtained by step (2) is added in the 3,4-rthylene dioxythiophene solution that mass concentration is 3%, passed through Carbon cloth is electrodeposited in prepare conducting polymer (condition of electro-deposition is：It is to electrode by reference electrode, platinum electrode of calomel electrode It is that working electrode forms a battery with carbon cloth, speed is swept from 0V to 0.6V with 10mV/s), obtain the microorganism of the nitrogen modification Anode of fuel cell.
Electrochemical property test is carried out to the anode of microbial fuel cell of nitrogen modification obtained by the present invention, test condition is such as Under：
The electro-chemical test of all uses be all Solartron 1480 (Solartron Analytical, England) carried out on electrochemical workstation.The electro-chemical tests such as cyclic voltammetric, chrono-amperometric use three-electrode system to implement Prepared electrode is working electrode in example 1, and air film piezoelectricity extremely auxiliary electrode, saturated calomel electrode is reference electrode.And with The carbon felt after 4h is placed in 80 DEG C of convection ovens as a comparison.
(1) cyclic voltammetric (CV) is tested
The cyclic voltammetry curve of anode is tested after refinement bacterium, scanning range is -0.6-0.4V (vs.Hg/Hg2Cl2), sweep It is 10mV s to retouch speed-1.The cyclic voltammetry curve figure of gained microbiological fuel cell is as shown in Figure 1, it can be seen that embodiment 1 The anode of microbial fuel cell response current of gained nitrogen modification is larger, illustrates that it has big ratio surface.Also, in -0.1V There are a pair of reversible redox peaks with -0.3V, illustrate the catalytic action of electrode pair bacterium.
(2) chrono-amperometric is tested
Using chronoamperometry Electrode material to opsonigenous substance (H2) catalysis oxidation.In non-refinement bacterium Chrono-amperometric is surveyed in 0.1M KCl solution, application current potential is 0.2V.As a result it is as shown in Figure 2, it is found that present invention gained nitrogen is repaiied The anode of microbial fuel cell of decorations is to H2There is stronger catalytic action.
(3) power polarization test
The polarization curve of battery is drawn by linear voltammetric scan method, and sweep speed is 10mV s-1, scanning range For from open circuit 0V to reference 0V.Equally often carry out once linear volt-ampere and sweep test, battery all needs first to place 3 days, to obtain stabilization Power output.When finally calculating the power density of battery, the area of electrode is using projected area.Gained Microbial fuel The polarization curve and power density curve of battery are as shown in Figure 3.As can be seen that the Microbial fuel electricity of present invention gained nitrogen modification The maximum power density of pond anode is much larger than unmodified carbon felt electrode, about 12 times.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (7)

1. a kind of preparation method of the anode of microbial fuel cell of nitrogen modification, it is characterised in that including following preparation process：
(1) compound containing manganese, zinc or tungsten and egg are added to the water, are dispersed with stirring uniformly, obtain mixed solution；
(2) carbon carrier is added in mixed solution obtained by step (1), taken out after supersound process, cleaned, dry, then in nitrogen Gas atmosphere and 800~1000 DEG C of 10~30min of temperature lower calcination, obtain the carbon carrier of the supported catalyst of nitrogen modification；
(3) carbon carrier obtained by step (2) is added in the monomer solution of conducting polymer, made on the carbon carrier by electro-deposition Standby conducting polymer, obtain the anode of microbial fuel cell of the nitrogen modification.
A kind of 2. preparation method of the anode of microbial fuel cell of nitrogen modification according to claim 1, it is characterised in that： Mass percent containing manganese, zinc or tungsten compound and egg described in step (1) is 0.5%~2%；The matter of egg and water Amount is than being 1:(1~2).
A kind of 3. preparation method of the anode of microbial fuel cell of nitrogen modification according to claim 1, it is characterised in that： Carbon carrier described in step (2) is one kind in biomass carbon, carbon felt and carbon cloth.
A kind of 4. preparation method of the anode of microbial fuel cell of nitrogen modification according to claim 1, it is characterised in that： Cleaning refers to be cleaned with deionized water described in step (2), and the drying refers to dry at a temperature of 60~80 DEG C.
A kind of 5. preparation method of the anode of microbial fuel cell of nitrogen modification according to claim 1, it is characterised in that： The monomer solution of conducting polymer described in step (3) refers to chromium solution, aniline solution and 3,4- ethene dioxythiophene solution At least one of；The mass concentration of the monomer solution of conducting polymer is 0.5%~5%.
A kind of 6. preparation method of the anode of microbial fuel cell of nitrogen modification according to claim 1, it is characterised in that： The condition of electro-deposition is described in step (3)：It is work to electrode and carbon carrier to be as reference electrode, platinum electrode using calomel electrode Electrode forms a battery, and speed is swept from 0V to 0.6V with 10mV/s.
A kind of 7. anode of microbial fuel cell of nitrogen modification, it is characterised in that：By described in any one of claim 1~6 Method is prepared.
CN201710846141.9A 2017-09-19 2017-09-19 A kind of anode of microbial fuel cell of nitrogen modification and preparation method thereof Pending CN107799796A (en)

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Publication number Priority date Publication date Assignee Title
CN108832146A (en) * 2018-05-30 2018-11-16 青岛科技大学 A kind of preparation method of porous carbon bioelectrode
WO2022000364A1 (en) * 2020-07-01 2022-01-06 东莞理工学院 Biomembrane electrode material based on special-shaped carbon fiber, and preparation method therefor and use thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108832146A (en) * 2018-05-30 2018-11-16 青岛科技大学 A kind of preparation method of porous carbon bioelectrode
CN108832146B (en) * 2018-05-30 2021-01-29 青岛科技大学 Preparation method of porous carbon bioelectrode
WO2022000364A1 (en) * 2020-07-01 2022-01-06 东莞理工学院 Biomembrane electrode material based on special-shaped carbon fiber, and preparation method therefor and use thereof

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Application publication date: 20180313