CN105375049B - Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell and preparation method - Google Patents
Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell and preparation method Download PDFInfo
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- CN105375049B CN105375049B CN201510925280.1A CN201510925280A CN105375049B CN 105375049 B CN105375049 B CN 105375049B CN 201510925280 A CN201510925280 A CN 201510925280A CN 105375049 B CN105375049 B CN 105375049B
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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
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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
- H01M4/8605—Porous electrodes
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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
- H01M4/8817—Treatment of supports before application of the catalytic active composition
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- 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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Abstract
The invention discloses carbonaceous tubular type oxygen reduction cathode microbiological fuel cell and preparation method；Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell of the present invention, including anode and negative electrode, it is characterised in that：The negative electrode uses bamboo carbon pipe；The outer surface of the bamboo carbon pipe is pasted with the separation membrane that hole is less than 1 μm coated with the ptfe emulsion that concentration is 5~10%, the inner surface of the bamboo carbon pipe；Cathode outer side winds titanium silk, and anode is inserted in bamboo charcoal tube along bamboo charcoal tube axial direction, and anode uses carbon cloth, carbon brush, carbon paper, carbon felt, carbon-point or graphite flake；End plate is respectively arranged with negative electrode both ends, end plate is bolted；Electrolyte inlet is provided with an end plate wherein, electrolyte outlet is provided with another end plate；For the present invention using natural cheap porous material as presoma and structural material, cost is low, has a good application prospect.
Description
Technical field
The present invention relates to microbiological fuel cell, more particularly to carbonaceous tubular type oxygen reduction cathode microbiological fuel cell and system
Preparation Method.
Background technology
Microbiological fuel cell (Microbial Fuel Cells, MFCs) be it is a kind of using microorganism by organic matter
Chemical energy is directly translated into the device of electric energy, has that fuel source is extensive, reaction condition is gentle, good biocompatibility, is producing
Wastewater treatment unique advantage is carried out while electric energy, turns into the focus of global regenerative resource researcher concern.However, although
Between past decades, the performance of microbiological fuel cell has obtained great lifting, but low power density and high cost according to
It is so two big bottlenecks of restriction micro-organisms fuel cell practice.Important composition portion of the negative electrode as microbiological fuel cell
Point, the rate of reduction of its performance characteristics and electron acceptor is closely related；Therefore, negative electrode just become a kind of critically important limitation because
Element.Meanwhile research is found, the performance of battery, institute can be largely lifted under the conditions of low cost using carbonaceous cathodes material
So that a kind of inexpensive, high performance cathode material of searching, which just has, to be of great significance.
The conventional negative electrode of microbiological fuel cell is broadly divided into chemical cathode and air cathode.Chemical cathode mainly uses iron
The a series of chemicals such as potassium cyanide, potassium peroxydisulfate and postassium hypochlorite is as cathode electronics acceptor.Air cathode is by making
By the use of the oxygen in air as final electron acceptor, its wide material sources, product is pollution-free, advantages of simple structure and simple.Air cathode
Typically it is made up of cathode construction material and catalyst.Conventional catalyst mainly has following several method：1. platinums are catalyzed
Agent.2. transition-metal catalysts.Such as：Manganese, ferric iron, cobalt, silver, titanium etc..3. carbonaceous catalysts.Such as：Activated carbon, nitrogen
The carbonaceous materials such as the cellulose modified with elements such as phosphorus.And conventional cathode material has：1. carbon cloths/active carbon cloth.2. carbon felts.
3. carbon papers.4. carbon fibers, 5. carbon yarn etc..
Because chemical cathode can cause secondary pollution and costly, it is unsuitable for extensive practice.Current main pin
To air cathode carry out it is widely studied, but these above-mentioned conventional cathode materials generally have mechanical performance it is poor, make plus
The shortcomings that work complex process, and the cost of metallic cathode catalyst is higher, it is also possible to cause heavy metal pollution.Therefore, price
Cheap, better performances carbonaceous catalysts have a preferable practice prospect, but carbonaceous cathodes catalyst and negative electrode knot at present
Structure still needs to further research and improved.
The content of the invention
The technical problems to be solved by the invention are to provide carbonaceous tubular type oxygen reduction cathode microbiological fuel cell and system
Preparation Method.
In order to solve the above-mentioned technical problem, first technical scheme of the invention is：The micro- life of carbonaceous tubular type oxygen reduction cathode
Thing fuel cell preparation method, it is characterised in that：Comprise the following steps：
A. cathode material is carbonized：Among fresh bamboo trunk is positioned over into baking oven, 3 are toasted in the baking oven of 80~105 DEG C of temperature
~7 days, then dry bamboo trunk is positioned over high-temperature atmosphere furnace, after high-temperature atmosphere stove evacuation, filling nitrogen, with 1~3
DEG C/min heating rate heat 900~1000 DEG C, under nitrogen atmosphere, 100~300cm of nitrogen flow3/ min, carbonization 2~
3 hours, furnace temperature is down to less than 100 DEG C taking-ups；Bamboo trunk is positioned under air ambient again, 330~350 DEG C of temperature carry out 2~3
Hour heat treatment, is then polished the inner surface of heat treated bamboo trunk and outer surface, and it is about 2~3mm to obtain wall thickness, long
Spend certain bamboo charcoal tube；
B. prepared by negative electrode：Bamboo charcoal tube is cleaned with deionized water, then dried；It is 5~10% by the concentration prepared
Polytetrafluoroethylene (PTFE) (PTFE) emulsion uniformly brush bamboo charcoal tube outer wall, and under the conditions of 330~370 DEG C heat 20~30 points
Clock；Then separation membrane of the one layer of hole less than 1 μm is mounted in bamboo charcoal inside pipe wall again；
C. battery assembles：The cathode outer side winding titanium silk prepared in stepb, anode insert along bamboo charcoal tube axial direction
In bamboo charcoal tube；End plate is loaded onto respectively at bamboo charcoal tube both ends, and blending bolt is fixed；Electrolyte is left on an end plate wherein to enter
Mouthful, electrolyte outlet is left on another end plate, forms carbonaceous tubular type oxygen reduction cathode microbiological fuel cell.
To prepare the carbonaceous oxygen reduction catalyst and cathode construction of high efficiency, low cost, the present invention will use bamboo trunk conduct
Presoma.
The present invention concrete principle be：The presoma and structure of negative electrode are used as first using the bamboo with nitrogen phosphorus enrichment material
Basis, it is dried under cryogenic, prevents that bamboo trunk is burst under higher baking temperature, treats that its dehydration rises to after to a certain degree
Temperature is dried, it is ensured that bamboo trunk drying and dehydrating.Dry bamboo is carbonized under nitrogen atmosphere, this not only ensure that the day of bamboo
Right tubular structure and microcellular structure, while obtained being rich in nitrogen P elements carbonaceous material, and high temperature cabonization ensure that carbonization material
Material has relatively low ohmic internal resistance.This nitrogen phosphorus enrichment carbonaceous material has substantial amounts of C-N and C-P chemical bonds, for hydrogen reduction
Reaction has more aerobic absorption and catalytic action so that carbonaceous cathodes have preferable hydrogen reduction performance.Be carbonized the bamboo charcoal completed
Pipe is heat-treated at a temperature of 350 DEG C or so can be good at aoxidizing a part of carbon so that bamboo charcoal tube has more flourishing micropore knot
Structure, to reach preferable oxygen transmission characteristic.Can effectively it be prevented in the ptfe emulsion of outer external coating 5~10%
The infiltration of water and saltout, while avoid the oxygen transmission thereby resulted in and be obstructed.One layer of hole of inside pipe wall attachment is less than 1 μm
Barrier material, it can effectively prevent directly short circuit caused by contact, while bacterium can be prevented to pass through separation membrane between anode and cathode
Grown in negative electrode, so as to avoid adverse effect of the biomembrane to cathode performance.
According to the preferred scheme of carbonaceous tubular type oxygen reduction cathode microbiological fuel cell preparation method of the present invention, institute
The separation membrane stated is using poly (ether sulfone) film, poly tetrafluoroethylene, polyvinylidene fluoride film or glass fibre membrane etc..
According to a kind of preferred side of carbonaceous tubular type oxygen reduction cathode microbiological fuel cell preparation method of the present invention
Case, the anode substrate of the microbiological fuel cell use carbon cloth, carbon brush, carbon paper, carbon felt, carbon-point or graphite flake.
The present invention second technical scheme be：Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell, including anode and
Negative electrode, it is characterised in that：The negative electrode uses bamboo carbon pipe；The outer surface of the bamboo carbon pipe is coated with poly- four that concentration is 5~10%
PVF emulsion, the inner surface of the bamboo carbon pipe are pasted with the separation membrane that hole is less than 1 μm；Cathode outer side winds titanium silk, anode edge
In bamboo charcoal tube axial direction insertion bamboo charcoal tube, anode uses carbon cloth, carbon brush, carbon paper, carbon felt, carbon-point or graphite flake；In negative electrode
Both ends are respectively arranged with end plate, and end plate is bolted；Electrolyte inlet is provided with an end plate wherein, another end plate
On be provided with electrolyte outlet.
According to a kind of preferred scheme of carbonaceous tubular type oxygen reduction cathode microbiological fuel cell of the present invention, described point
Barrier film uses poly (ether sulfone) film, poly tetrafluoroethylene, polyvinylidene fluoride film or glass fibre membrane.
The beneficial effect of carbonaceous tubular type oxygen reduction cathode microbiological fuel cell of the present invention and preparation method is：This
Invention, as presoma and structural material, on the one hand greatly reduces microbiological fuel cell using natural cheap porous material
Making and processing cost, while tubular structure provides preferable architecture basics for the amplification and scale of battery；Due to
The enrichment of this material nitrogen phosphorus, substantial amounts of C-N and C-P chemical bonds are made it have, there is more aerobic absorption for oxygen reduction reaction
And catalytic action so that carbonaceous cathodes have preferable hydrogen reduction performance, so as to improve the performance of microbiological fuel cell；This
Invention energy consumption is low, and method is simple, easy to operate, and cost is low, has a good application prospect.
Brief description of the drawings
Fig. 1 is carbonaceous tubular type oxygen reduction cathode principle of microbial fuel cells figure and pictorial diagram.
Fig. 2 is the photo that carbonaceous bamboo trunk carbon cloth is placed under SEM.
Fig. 3 is the microbiological fuel cell performance map obtained using the present invention.
Fig. 4 is COD clearances and coulombic efficiency under the conditions of different COD.
Fig. 5 is COD clearances and coulombic efficiency under the conditions of different extrernal resistances.
Embodiment
The present invention is further described specifically with reference to embodiment, but the implementation of the present invention is not limited to this.
With reference to figure 1, carbonaceous tubular type oxygen reduction cathode microbiological fuel cell, including anode 4 and negative electrode 3；The negative electrode 3 is adopted
With bamboo carbon pipe；The outer surface of the bamboo carbon pipe is coated with the ptfe emulsion that concentration is 5~10%, the inner surface of the bamboo carbon pipe
The separation membrane 5 that hole is less than 1 μm is pasted with, the separation membrane is using poly (ether sulfone) film, poly tetrafluoroethylene, polyvinylidene fluoride film
Or glass fibre membrane；The outer wall winding titanium silk 1 of bamboo carbon pipe, anode 4 is inserted in bamboo charcoal tube along bamboo charcoal tube axial direction, anode 4
Carbon cloth, carbon brush, carbon paper, carbon felt, carbon-point or graphite flake can be used；End plate 6 is respectively arranged with the both ends of negative electrode 3, end plate 6 uses
Poly (methyl methacrylate) plate；Electrolyte inlet 7 is set on an end plate wherein, electrolyte outlet 8 is set on another end plate；End plate 6
Fixed by bolt 2.
Embodiment 1：Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell preparation method, comprises the following steps：
A. cathode material is carbonized：Among ready fresh bamboo trunk is positioned over into baking oven, 7 are toasted at a temperature of 80 DEG C
My god, it is ensured that bamboo trunk is dehydrated completely；Dry bamboo charcoal is positioned over high-temperature atmosphere furnace again, vacuumizes, fill nitrogen afterwards with 1
~3 DEG C/min of heating rate is heated to 900 DEG C, under nitrogen atmosphere, with nitrogen flow 300cm3/ min is carbonized 2 hours, will
Furnace temperature is down to less than 100 DEG C taking-up bamboo trunks；Bamboo trunk is positioned under air ambient again, it is small that 2 are carried out among 350 DEG C of temperature baking ovens
When be heat-treated, then the inner surface of heat treated bamboo trunk and outer surface are polished, it is about 2~3mm to obtain wall thickness, length
Certain bamboo charcoal tube.
B. prepared by negative electrode：It is 8% by the concentration prepared after bamboo charcoal tube is cleaned and dried with deionized water
Ptfe emulsion is uniformly brushed in bamboo charcoal pipe outer wall, and is heated 30 minutes and dried under the conditions of 330 DEG C；Four paintings are carried out altogether
Brush；After polytetrafluoroethylene (PTFE) brushing is completed, separation membrane of the one layer of hole less than 1 μm is mounted in inside pipe wall, separation membrane uses polyethers
Sulfone PES films.
C. battery assembles：Titanium silk 1 is wrapped with negative electrode outer wall, diameter is less than the carbon brush anode 3 of bamboo charcoal bore along bamboo
In charcoal pipe y direction insertion bamboo charcoal tube；Load onto end plate 6 respectively at bamboo charcoal tube both ends, blending bolt 2 is fixed；End plate 6, which uses, to be had
Machine glass plate；Electrolyte inlet 7 is set on an end plate wherein, electrolyte outlet 8 is set on another end plate；Form carbonaceous
Tubular type oxygen reduction cathode microbiological fuel cell.
Embodiment 2
Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell preparation method, comprises the following steps：
A. cathode material is carbonized：Using fresh bamboo trunk as presoma.By ready fresh bamboo trunk be positioned over baking oven it
In, bamboo trunk internal diameter 5cm, length 12cm, toasted 3 days under the conditions of being toasted 2 days, 80 DEG C under the conditions of 40 DEG C, it is ensured that bamboo trunk is complete
Full dehydration.Dry bamboo charcoal is positioned over high-temperature atmosphere furnace, vacuumizes, fill nitrogen afterwards with 1.5 DEG C/min of heating rate
1000 DEG C are heated to, under nitrogen atmosphere, nitrogen flow 250cm3/ min is carbonized 2.5 hours, treats that furnace temperature is down to less than 100 DEG C and taken
Go out bamboo trunk；Bamboo trunk after being carbonized is arranged under SEM and observes its microscopic characteristics, is found after being carbonized
Bamboo charcoal can keep abundant porous, provide preferable passage for mass transfer, the photo under SEM is shown in
Fig. 2.
B. prepared by negative electrode：The bamboo charcoal tube that step A has been carbonized is positioned under air conditionses, and 330 DEG C of temperature are carried out 2.5 hours
Heat treatment；Then by heat treated bamboo charcoal tube, inner surface and outer surface are polished respectively, and it is about 3mm to form wall thickness, long
The bamboo charcoal tube for 6cm is spent, and is cleaned with deionized water.Complete after cleaning and drying, be 5% by the concentration prepared
Ptfe emulsion is uniformly brushed in pipe outer wall, and is heated 25 minutes under the conditions of 360 DEG C；Brushed three times altogether；Poly- four
PVF brushing is less than 1 μm of separation membrane in inside pipe wall one layer of hole of attachment after completing, separation membrane is glass fibre membrane.
C. battery assembles：The negative electrode outer wall prepared in stepb is wrapped with titanium silk, and diameter is less than into bamboo charcoal bore, long
Spend and inserted for 4cm carbon-point anode along bamboo charcoal tube y direction in bamboo charcoal tube.Load onto end plate 6 respectively at bamboo charcoal tube both ends, and
Fixed with bolt 2, electrolyte inlet 7 is set on an end plate wherein, electrolyte outlet 8 is set on another end plate；Formed
Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell.
D. by the battery assembled, continuous stream starts under the conditions of 1000 Ω extrernal resistances, and its property is measured after carrying out the culture of 10 days
Energy curve, as shown in figure 3, experiment shows that this battery has preferable power output.Wherein nutrient media components is：3.38~
10.14g/L CH3COONa,6g/L Na2HPO4,1.5g/L KH2PO4,0.05g/L NH4Cl,0.5g/L NaCl,0.1g/L
MgSO4·7H2O,15mg/L CaCl2·2H2O and 1.6mg/L trace elements；Wherein trace element can use FeSO4·
7H2O、ZnCl2、MnCl·4H2O、H3BO3、CaCl2·6H2O、CuCl2·2H2O,NiCl2·6H2O or NaMoO4·2H2O,
CoCl2·6H2O etc..
Embodiment 3：Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell preparation method, this method are different from embodiment 2
Be that separation membrane is poly tetrafluoroethylene.After preparing in this way and assembling battery, respectively handle 200COD, 500COD,
1000COD, 1500COD waste water, its COD removal efficiency and coulombic efficiency are as shown in Figure 4.In the case of COD, this carbonaceous tubular type
Oxygen reduction cathode microbiological fuel cell can realize higher COD clearances, have preferable waste treatment capacity.
Embodiment 4：Carbonaceous tubular type oxygen reduction cathode microbiological fuel cell preparation method, this method are different from embodiment 2
Be that separation membrane is polyvinylidene fluoride film, and be respectively adopted 600 ohm, 200 ohm, 100 ohm, 50 ohm in outer meeting resistance
In the case of, test this carbonaceous tubular type oxygen reduction cathode microbiological fuel cell COD removal efficiency and coulombic efficiency.Such as Fig. 5 institutes
Show, illustrate in the case of different extrernal resistances, this carbonaceous tubular type oxygen reduction cathode microbiological fuel cell can be realized higher
COD clearances, there is preferable waste treatment capacity.And under certain loading condition, this single chamber MFC, which also has, more may be used
The coulombic efficiency of sight, show that the battery can realize preferable energy regenerating.
Claims (4)
1. carbonaceous tubular type oxygen reduction cathode microbiological fuel cell preparation method, it is characterised in that：Comprise the following steps：
A. cathode material is carbonized：Among fresh bamboo trunk is positioned over into baking oven, 3~7 are toasted in the baking oven of 80~105 DEG C of temperature
My god, then dry bamboo trunk is positioned over high-temperature atmosphere furnace, after high-temperature atmosphere stove evacuation, filling nitrogen, with 1~3 DEG C/
The heating rate of minute is heated to 900~1000 DEG C, under nitrogen atmosphere, 100~300cm of nitrogen flow3/ min, carbonization 2~3
Hour, furnace temperature is down to less than 100 DEG C taking-up bamboo trunks；Bamboo trunk is positioned under air ambient again, entered in 330~350 DEG C of temperature
Row is heat-treated for 2~3 hours, obtains bamboo charcoal tube；
B. prepared by negative electrode：Bamboo charcoal tube is cleaned with deionized water, then dried；It is 5~10wt%'s by the concentration prepared
Ptfe emulsion uniformly brushes the outer wall in bamboo charcoal tube, and is heated 20~30 minutes under the conditions of 330~370 DEG C；Then
Again separation membrane (5) of the one layer of hole less than 1 μm is mounted in bamboo charcoal inside pipe wall；
C. battery assembles：Anode (4) is inserted in bamboo charcoal tube along bamboo charcoal tube axial direction；End is loaded onto respectively at bamboo charcoal tube both ends
Plate (6), blending bolt (2) are fixed；Electrolyte inlet is left on an end plate wherein, leaving electrolyte on another end plate goes out
Mouthful, form carbonaceous tubular type oxygen reduction cathode microbiological fuel cell.
2. carbonaceous tubular type oxygen reduction cathode microbiological fuel cell preparation method according to claim 1, it is characterised in that：
The separation membrane uses poly (ether sulfone) film, poly tetrafluoroethylene, polyvinylidene fluoride film or glass fibre membrane.
3. carbonaceous tubular type oxygen reduction cathode microbiological fuel cell, including anode (4) and negative electrode (3), it is characterised in that：Described the moon
Pole (3) uses bamboo charcoal tube；The outer surface of the bamboo charcoal tube is coated with the ptfe emulsion that concentration is 5~10wt%, the bamboo carbon
The inner surface of pipe is pasted with the separation membrane (5) that hole is less than 1 μm；Negative electrode outer wall winding titanium silk (1), anode (4) is along bamboo charcoal tube
In y direction insertion bamboo charcoal tube；End plate (6) is respectively arranged with bamboo charcoal tube both ends, end plate (6) is fixed by bolt (2)；At it
In be provided with electrolyte inlet on an end plate, be provided with electrolyte outlet on another end plate.
4. carbonaceous tubular type oxygen reduction cathode microbiological fuel cell according to claim 3, it is characterised in that：The separation
Film uses poly (ether sulfone) film, poly tetrafluoroethylene, polyvinylidene fluoride film or glass fibre membrane.
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| CN106505233B (en) * | 2016-11-10 | 2019-03-19 | 重庆大学 | A kind of microbiological fuel cell of bamboo charcoal bundled tube bubbling air cathode construction |
| CN108574105A (en) * | 2018-05-21 | 2018-09-25 | 西交利物浦大学 | A kind of air cathode of microbiological fuel cell |
| CN108767301B (en) * | 2018-05-28 | 2021-03-12 | 重庆大学 | Size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell and preparation method thereof |
| CN108649251B (en) * | 2018-05-28 | 2021-07-06 | 重庆大学 | Preparation method of membrane-free formic acid fuel cell based on integral carbonaceous self-breathing cathode |
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| CN103296278A (en) * | 2013-06-24 | 2013-09-11 | 西南大学 | Preparation method of plant material based energy conversion catalyst |
| CN104617309A (en) * | 2015-01-13 | 2015-05-13 | 上海理工大学 | Carbon-based oxygen reduction electrode material and preparation method thereof |
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