CN106898792B - Cellulose base single-chamber microbial fuel cell air cathode and preparation method thereof - Google Patents

Cellulose base single-chamber microbial fuel cell air cathode and preparation method thereof Download PDF

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CN106898792B
CN106898792B CN201710087335.5A CN201710087335A CN106898792B CN 106898792 B CN106898792 B CN 106898792B CN 201710087335 A CN201710087335 A CN 201710087335A CN 106898792 B CN106898792 B CN 106898792B
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cellulose
air cathode
nano
fuel cell
base material
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CN106898792A (en
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吴敏
慈吉良
黄勇
曹春
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Technical Institute of Physics and Chemistry of CAS
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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
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H01M8/0234—Carbonaceous material
    • 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
    • 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
    • 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
    • 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)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Materials Engineering (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Inert Electrodes (AREA)
  • Fuel Cell (AREA)

Abstract

The present invention provides a kind of cellulose base single-chamber microbial fuel cell air cathode, and the diffusion layer of the air cathode is compounded in substrate by nano-cellulose to be formed, and the nano-cellulose is made by raw material of native cellulose；The material of the substrate is carbon cloth or carbon paper.The present invention also provides the preparation methods of the single-chamber microbial fuel cell air cathode.The air cathode diffusion layer of the single-chamber microbial fuel cell of novel cellulose base proposed by the present invention is using native cellulose as raw material, and native cellulose has many advantages, such as that from a wealth of sources, yield is high, renewable, environment friendly and pollution-free, at low cost.Compound Pt/C and nafion layers on the diffusion layer, preparation method is simple, does not need high temperature sintering, the air cathode of the single-chamber microbial fuel cell of obtained novel cellulose base, by theoretical and actual verification, is shown to be a kind of high performance air cathode.

Description

Cellulose base single-chamber microbial fuel cell air cathode and preparation method thereof
Technical field
The invention belongs to fuel cell fields, and in particular to a kind of preparation side of the electrode material of microbiological fuel cell Method.
Background technique
With the development of industry, environmental pollution and water pollution problems become two hang-ups for restricting contemporary society's development, promote People are made to constantly look for renewable, sustainable development new cleaning fuel.Microbiological fuel cell (MFC) is a kind of novel Sewage disposal technology while acting on realization efficient process waste water, converts the chemical energy in waste water to by microorganism Clean biometric matter electric energy.It is divided by external form, microbiological fuel cell can be divided into double chamber type and single chamber type.Dual chamber MFC is by two electricity Pole room composition, one is anaerobic room (anode chamber), another is aerobic room (cathode chamber).In anaerobic room, substance (fuel) is micro- Biological oxidation generates carbon dioxide, and electronics is transferred to anode by no carriers or mediator or directly passes through microbial respiratory Enzyme is transferred to anode；Anode chamber is connected in inside battery with proton exchange membrane with cathode chamber, and outside constitutes external circuit by conducting wire. In aerobic room, electronics arrives separately at cathodic combination by proton exchange membrane by external circuit, proton and forms water.Single chamber MFC is saved Cathode chamber, by microbiological oxidation at single chamber anode, electronics is transmitted to external circuit by anode and then reaches cathode, proton substance It is transferred on cathode, in air, oxygen generates water as direct electron acceptor, with proton reaction for cathode exposure.
The air cathode of single-chamber microbial fuel cell is a key factor for influencing its electricity generation performance, at present both at home and abroad Generally using polytetrafluoroethylene (PTFE) (PTFE) as adhesive and diffusion layer when preparing air cathode, but this PTFE diffusion layer at This height, preparation process is complicated, and non-degradable causes environment pollution, these disadvantages significantly limit single-chamber microbial fuel The development and application of battery.
Summary of the invention
(1) technical problems to be solved
The purpose of the present invention is it is micro- to be prepared for novel single chamber using cellulose as raw material for the problems of prior art Biological fuel cell air cathode diffusion layer, substitution PTFE are prepared for air cathode with high performance.
It is another object of the present invention to propose the single-chamber microbial fuel cell containing air cathode.
(2) technical solution
Realize the technical solution of above-mentioned purpose of the present invention are as follows:
A kind of cellulose base single-chamber microbial fuel cell air cathode, the diffusion layer of the air cathode are by nanofiber Element is compounded in substrate and forms, and the nano-cellulose is made by raw material of native cellulose；The material of the substrate is carbon Cloth or carbon paper.
A kind of preparation method of single-chamber microbial fuel cell air cathode, comprising steps of
1) using native cellulose as raw material, nano-cellulose suspension is prepared,
2) base material is cut into piece, Suction filtration device is put up, the base material cut out is placed on filter membrane,
3) nano-cellulose suspension dimethylformamide is diluted 5~15 times, pours into filter bowl and is filtered,
4) after having filtered dimethylformamide (DMF), base material is taken off from filter membrane；
5) cellulose nano-fibrous (CNF) film of base material lower surface is cleared, the CNF film of carbon cloth upper surface is protected It stays completely, obtains cellulose nano-fibrous (CC-CNF) diffusion layer of carbon cloth-.
6) proportion for pressing diffusion layer every square centimeter 0.1~0.4mg Pt, weighs Pt/C catalyst；
7) into Pt/C catalyst be added deionized water, Nafion solution and isopropanol mixed solvent, and ultrasound 15~ Catalyst dispersion is prepared within 40 minutes；
8) by dispersion liquid that step 7) obtains with brush be uniformly coated on diffusion layer without cellulose nano-fibrous (CNF) The one side of film obtains single-chamber microbial fuel cell air cathode after dry.
In above-mentioned preparation method, the preparation of nano-cellulose suspension uses the prior art.The base material is carbon cloth Or carbon paper.
Further, the step 2) filter membrane is nylon micro porous filter membrane, and filter sizes are 0.2~1 μm.
Wherein, in step 3), relative to carbon cloth area, the suspension vol diluted is 3~5mL/cm2；The suction filtration Vacuum degree be -0.1~1.0Mpa.
Wherein, in step 5), obtained film is placed in vacuum drying oven drying, dry 10 at a temperature of 60~80 DEG C~ 15 hours.
Wherein, in the step 7), according to the dosage of Pt/C catalyst according to following proportion addition solvent: 0.80~0.85 μL mg-1Deionized water, 6.5~6.8 μ L mg-1Nafion solution and 3~4 μ L mg-1Isopropanol；The Nafion is molten The content of liquid is 5~10wt%.
Single-chamber microbial fuel cell containing single-chamber microbial fuel cell air cathode of the present invention.
(3) beneficial effect
The air cathode diffusion layer of the single-chamber microbial fuel cell of novel cellulose base proposed by the present invention, is with natural Cellulose is raw material, and native cellulose has many advantages, such as that from a wealth of sources, yield is high, renewable, environment friendly and pollution-free, at low cost, Preparation process will not introduce fluorochemical monomer as prepared by PTFE, be a kind of green material.
Compound Pt/C and nafion layers on the diffusion layer, preparation method is simple, does not need high temperature sintering, and what is obtained is new The air cathode of the single-chamber microbial fuel cell of fiber type element base is shown to be a kind of high-performance by theoretical and actual verification Air cathode.
Detailed description of the invention
Fig. 1 is the structure diagram for the Suction filtration device that the present invention prepares CC-CNF diffusion layer.
Fig. 2 is the linear sweep voltammetry curve of air cathode single-chamber microbial fuel cell of the present invention.
Fig. 3 is the linear sweep voltammetry curve for the air cathode single-chamber microbial fuel cell that diffusion layer is PTFE.
Fig. 4 is the cycle charge-discharge curve of single-chamber microbial fuel cell of the present invention.
Fig. 5 is the cycle charge-discharge curve that diffusion layer is PTFE air cathode single-chamber microbial fuel cell.
Fig. 6 is the power density curve of single-chamber microbial fuel cell of the present invention.
Fig. 7 is the power density curve that diffusion layer is PTFE air cathode single-chamber microbial fuel cell.
In Fig. 1,1 is filter bowl, and 2 be carbon cloth, and 3 be filter membrane, and 4 be filter, and 5 be triangular flask, and 6 be clip.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below Example is not intended to limit the scope of the invention for illustrating the present invention.
In embodiment, nano-cellulose suspension is prepared according to patent (publication No. CN103132169) the method.
Embodiment 1
1) molten using corn cob fiber element as raw material according to 1 the method for patent (publication No. CN 103132169) embodiment Agent is dimethylformamide (DMF), prepares nano-cellulose suspension.
2) carbon cloth is cut into the disk that diameter is 3.8cm, Suction filtration device is put up, the carbon cloth 2 cut out is placed in filter membrane 3 On.The composite layer of carbon cloth 2 and filter membrane is placed in Suction filtration device such as Fig. 1,1 bottom of filter bowl, connects filter 4 by funnel and with pressing from both sides Son 6 fixes, and triangular flask 5, the interface for the vacuum pump that the setting of triangular flask bottleneck filters are placed below filter.Filter membrane 3 is nylon Miillpore filter (50mm*0.45 μm).
3) nano-cellulose suspension dimethylformamide being diluted 10 times, suspension total volume is that 40mL pours into filter bowl, It is filtered with pump, vacuum degree -0.4MPa, a few hours time is filtered, until liquid exhausts completely.
4) after having filtered DMF, carbon cloth is taken off from filter membrane.
5) the CNF film of carbon cloth lower surface is cleared, the CNF film of carbon cloth upper surface retains completely, obtains CC-CNF expansion Dissipate layer.
6) CC-CNF is placed in vacuum drying oven drying, after 12 hours dry at a temperature of 60 DEG C, obtains dry CC- CNF diffusion layer.
7) proportion for pressing CC-CNF every square centimeter 0.2mg Pt, weighs Pt/C (20wt%) catalyst.
8) solvent: 0.83 μ L mg is added according to following proportion according to the dosage of unit mass Pt/C catalyst-1Deionization Water, 6.67 μ L mg-1Nafion (5wt%) solution and 3.33 μ L mg-1Isopropanol, and ultrasound is prepared and urges for 30 minutes Agent dispersion liquid.
9) dispersion liquid that step 8) obtains is uniformly coated on to carbon cloth that step 6) obtains is another not to have CNF film with brush Surface, dry 24 hours, obtain single-chamber microbial fuel cell air cathode.
To obtained single-chamber microbial fuel cell air cathode carry out linear sweep voltammetry test, practical electricity generation performance and Peak power output identification, is as a result shown in Fig. 2, Fig. 4 and Fig. 6 respectively.
In linear sweep voltammetry curve determination, reference electrode is saturation Ag/AgCl electrode, electrolyte is phosphate-buffered Liquid.By Fig. 2 and Fig. 3 it is found that under identical scanning potential, the current density of the response of air cathode made from the present embodiment is higher than PTFE air cathode.
Single-chamber microbial battery is made with the present embodiment air cathode, electrolyte is phosphate buffer, and anode is micro- life Object anode, discharge voltage is 570-580mV (Fig. 4), higher than the discharge voltage of PTFE air cathode microbial fuel cell (530-540mV) (Fig. 5), peak power output are 1518 ± 39mW/m2(Fig. 6) is higher than PTFE air cathode microbial fuel Peak power output (1167 ± 29mW/m2, Fig. 7).
Embodiment 2
Embodiment 1 is repeated, the difference is that only: the cellulosic material is paper cellulose.By nano-cellulose Suspension dimethylformamide filters after diluting 10 times.Obtain CC-CNF diffusion layer.
Embodiment 3
Embodiment 1 is repeated, the difference is that only: the cellulosic material is microcrystalline cellulose.By nano-cellulose Suspension filters after diluting 12 times with dimethylformamide.Obtain dry CC-CNF diffusion layer.
Embodiment 4
Embodiment 1 is repeated, the difference is that only: the cellulosic material is cotton cellulose；Obtain dry CC- CNF diffusion layer.
The step of preparing air cathode are as follows:
S1 presses the proportion of CC-CNF every square centimeter 0.2mg Pt, weighs Pt/C (20wt%) catalyst.
Solvent: 0.85 μ L mg is added according to following proportion according to the dosage of unit mass Pt/C catalyst in S2-1Deionization Water, 6.65 μ L mg-1Nafion (5wt%) solution and 3.6 μ L mg-1Isopropanol, and ultrasound catalysis is prepared within 30 minutes Agent dispersing liquid.
Dispersion liquid that step 8) obtains is uniformly coated on that carbon cloth that step 6) obtains is another not to have CNF film by S3 with brush Surface, dry 24 hours, obtain single-chamber microbial fuel cell air cathode.
Embodiment 5
Embodiment 1 is repeated, the difference is that only: the cellulosic material is woody cellulose.Obtain dry CC- CNF diffusion layer.
Comparative example
It with commercially available PTFE solution, is coated on carbon cloth, 300-350 DEG C of high temperature sintering is that PTFE air cathode diffusion layer is (equal For prior art means), air cathode is made according to the method as embodiment 1, linear sweep voltammetry Dependence Results are shown in Fig. 3, compared to the air cathode (Fig. 2) of the application, under identical scanning potential, the corresponding current density of PTFE air cathode Lower than the current density of air cathode of the present invention.
Microorganism single battery is made according to the method as embodiment 1, its discharge voltage is 530- according to Fig. 5 540mV, referring to Fig. 7, peak power output is 1167 ± 29mW/m2。
Above embodiment be only preferred embodiments of the present invention will be described, not to the scope of the present invention into Row limits, and without departing from the spirit of the design of the present invention, this field ordinary engineering and technical personnel is to technical side of the invention The all variations and modifications that case is made, should fall within the scope of protection determined by the claims of the present invention.

Claims (7)

1. a kind of cellulose base single-chamber microbial fuel cell air cathode, which is characterized in that the diffusion layer of the air cathode is It is compounded in substrate and is formed by nano-cellulose, the nano-cellulose is made by raw material of native cellulose；The substrate Material be carbon cloth or carbon paper；
The single-chamber microbial fuel cell air cathode is made up of following steps:
1) native cellulose and n,N-Dimethylformamide are mixed, above-mentioned mixing is added in chloroacetic chloride by cellulose solid content 1% In object, molar ratio between the chloroacetic chloride and cellulose is 1:0.1, and all reaction mixtures are carried out mill, mill it is same When along with the hydroxyl on cellulose fiber surface esterification occurs, until obtain containing diameter in 2~1000nm, a length of 10 ~100 μm of nano-cellulose suspension,
2) base material is cut into piece, Suction filtration device is put up, the base material cut out is placed on filter membrane,
3) nano-cellulose suspension dimethylformamide is diluted 5~15 times, pours into filter bowl and is filtered,
4) after having filtered dimethylformamide, base material is taken off from filter membrane；
5) by the cellulose nano-fibrous cleared of base material lower surface, the cellulose nano-fibrous film of base material upper surface Retain completely, obtains the cellulose nano-fibrous diffusion layer of base material-；
6) proportion for pressing diffusion layer every square centimeter 0.1~0.4mg Pt, weighs Pt/C catalyst；
7) mixed solvent of deionized water, Nafion solution and isopropanol, and 15~40 points of ultrasound are added into Pt/C catalyst Catalyst dispersion is prepared in clock；
8) by dispersion liquid that step 7) obtains with brush be uniformly coated on diffusion layer without the one of cellulose nano-fibrous film Face obtains single-chamber microbial fuel cell air cathode after dry.
2. air cathode according to claim 1, which is characterized in that in step 5), obtained film is placed in vacuum and is dried It is dried in case, it is 10~15 hours dry at a temperature of 60~80 DEG C.
3. a kind of preparation method of single-chamber microbial fuel cell air cathode, which is characterized in that comprising steps of
1) native cellulose and n,N-Dimethylformamide are mixed, above-mentioned mixing is added in chloroacetic chloride by cellulose solid content 1% In object, molar ratio between the chloroacetic chloride and cellulose is 1:0.1, and all reaction mixtures are carried out mill, mill it is same When along with the hydroxyl on cellulose fiber surface esterification occurs, until obtain containing diameter in 2~1000nm, a length of 10 ~100 μm of nano-cellulose suspension,
2) base material is cut into piece, Suction filtration device is put up, the base material cut out is placed on filter membrane,
3) nano-cellulose suspension dimethylformamide is diluted 5~15 times, pours into filter bowl and is filtered,
4) after having filtered dimethylformamide, base material is taken off from filter membrane；
5) by the cellulose nano-fibrous cleared of base material lower surface, the cellulose nano-fibrous film of base material upper surface Retain completely, obtains the cellulose nano-fibrous diffusion layer of base material-；
6) proportion for pressing diffusion layer every square centimeter 0.1~0.4mg Pt, weighs Pt/C catalyst；
7) mixed solvent of deionized water, Nafion solution and isopropanol, and 15~40 points of ultrasound are added into Pt/C catalyst Catalyst dispersion is prepared in clock；
8) by dispersion liquid that step 7) obtains with brush be uniformly coated on diffusion layer without the one of cellulose nano-fibrous film Face obtains single-chamber microbial fuel cell air cathode after dry；
In above-mentioned steps, the base material is carbon cloth or carbon paper.
4. preparation method according to claim 3, which is characterized in that the step 2) filter membrane is nylon micro porous filter membrane, filter Membrane aperture is 0.2~1 μm.
5. preparation method according to claim 3, which is characterized in that in step 3), relative to carbon cloth area, dilute Suspension vol is 3~5mL/cm2；The vacuum degree of the suction filtration is -0.1~1.0Mpa.
6. preparation method according to claim 3, which is characterized in that in the step 7), according to the use of Pt/C catalyst Solvent: 0.80~0.85 μ L mg is added according to following proportion in amount-1Deionized water, 6.5~6.8 μ L mg-1Nafion solution With 3~4 μ L mg-1Isopropanol；The content of the Nafion solution is 5~10wt%.
7. containing the single-chamber microbial fuel cell of single-chamber microbial fuel cell air cathode described in claim 1.
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Citations (3)

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Publication number Priority date Publication date Assignee Title
CN101710626A (en) * 2009-11-12 2010-05-19 南京大学 Single-chamber microbial fuel cell and application thereof in wastewater treatment
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CN104112868A (en) * 2014-06-11 2014-10-22 武汉大学 Constructing method and device for single-chamber medium-free algae microbial fuel cell

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CN101710626A (en) * 2009-11-12 2010-05-19 南京大学 Single-chamber microbial fuel cell and application thereof in wastewater treatment
CN103730667A (en) * 2014-01-15 2014-04-16 中国科学院化学研究所 Method for manufacturing air cathode of single-chamber microbial fuel cell
CN104112868A (en) * 2014-06-11 2014-10-22 武汉大学 Constructing method and device for single-chamber medium-free algae microbial fuel cell

Non-Patent Citations (1)

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