CN103367766A - Preparation method for graphene/ conductive polymer anode for microbial fuel cell - Google Patents
Preparation method for graphene/ conductive polymer anode for microbial fuel cell Download PDFInfo
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- CN103367766A CN103367766A CN2013103280724A CN201310328072A CN103367766A CN 103367766 A CN103367766 A CN 103367766A CN 2013103280724 A CN2013103280724 A CN 2013103280724A CN 201310328072 A CN201310328072 A CN 201310328072A CN 103367766 A CN103367766 A CN 103367766A
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Abstract
The invention discloses a preparation method for a graphene/ conductive polymer anode for a microbial fuel cell. The preparation method comprises the following steps: conductive polymer monomers and an aqueous suspension of graphene oxides are mixed, stirred at room temperature and subjected to ultrasonic treatment; by employing a constant voltage electroplating method, conductive polymer monomer/graphene oxide conductive composites are subjected to electrochemical polymerization and deposited on a surface of an anode; by employing a cyclic voltammetry, after situ electroreduction, a conductive polymer/electrochemical reduction graphene oxide modified anode is prepared on the electrode. The conductive polymer/electrochemical reduction graphene oxide modified anode is washed with deionized water and dried in the air at room temperature to prepare a graphene/ conductive polymer anode for a microbial fuel cell. Compared to traditional chemical modification methods, the preparation method reduces the usage of toxic reagents and cumbersome processes, lowers the preparation cost, and is easy to realize industrialization of electrode preparation. When the modified electrode is used for a cell, the electricity generation capacity of a microbial fuel cell is raised observably, and the development and application of a microbial fuel cell can be promoted.
Description
Technical field
The present invention relates to the microbiological fuel cell field, specifically a kind of microbiological fuel cell preparation method of Graphene/conducting polymer anode.
Background technology
Microbiological fuel cell (microbial fuel cell, be called for short MFC), be the fuel cell system that but chemical energy in the biological utilisation organic matter is converted into electric energy take microbe as catalyst, with its clean environment firendly, the advantage such as renewable, become gradually the study hotspot of emerging energy field and environmental area.But the electrogenesis power ratio fuel cell of MFC is low, and its main cause is subject on the one hand electrogenesis bacterium anode and transmits the indifferent of electronics, on the other hand because the ohmic loss in the MFC system is larger.And the material of anode and structure directly have influence on the oxidation of the adhering to of microbe, electronics transmission and substrate.Therefore, seeking the good high electrochemical activity anode of conductivity is an important directions will investigating at present.Carbon-based material, such as carbon paper, carbon cloth, carbon felt, foamy carbon owing to have good stability, high conductivity and high-ratio surface, are widely used as anode base material.Raising for the anode electrode performance, researchers have made extensive work, the type selecting of electrode mainly is divided into three major types, the one, use combination electrode material, such as CNT/PANI(carbon nano-tube/poly aniline) composite anode, so that anode characteristic area and charge transport ability are improved, improved significantly the electro-chemical activity of MFC anode reaction; The 2nd, to the electrode material of modification, as using Mn
4+The anode graphite anode of modifying utilizes ammonia to process and modifies the carbon paper anode, changes electrode N/C ratio content etc. by modifying the modes such as dimethylaniline, ammonia treatment, heating; The 3rd, nano-electrode material is as synthesizing MFC anode, the Au of decorated nanometer and Pd particle etc. on graphite electrode with carbon nano-tube.But the most processing cost of these methods is higher, and processing step is comparatively complicated, has greatly improved the cost of manufacture of electrode.Therefore, develop a kind of efficient, anode cheaply, to the making of microbiological fuel cell with and the expansion of commercial application be significant.
Summary of the invention
The object of the invention is to for the existing low deficiency of microbiological fuel cell efficiency of fuel cell generation, a kind of preparation method of composite graphite alkene anode of microbial fuel cell is provided, the present invention at carbon-based electrode substrates polypyrrole/electrochemical reduction graphene oxide composite membrane, prepares a kind of novel electrode by electrochemical method.
The present invention realizes that the technical scheme that purpose adopts comprises:
A kind of microbiological fuel cell comprises the steps: with the preparation method of Graphene/conducting polymer anode
(1) graphene oxide is dissolved in the deionized water, making concentration is 1 ~ 15 mgmL
-1Graphene oxide aqueous suspension solution, the conducting polymer monomer is joined in the graphene oxide aqueous suspension solution make mixed liquor again, the concentration of conducting polymer monomer in mixed liquor is 0.1 ~ 0.5 molL
-1, at room temperature behind magnetic agitation 5 ~ 30 min, and ultrasonic 5 ~ 30 min, make mixed electrolytic solution;
(2) utilize electrochemical workstation, adopt three-electrode system, with pretreated carbon-based material as work electrode, with platinum electrode as to electrode, with saturated calomel electrode or saturated silver chloride electrode as reference electrode, three electrodes are placed described mixed electrolytic solution, adopt the constant voltage galvanoplastic, it is 0.5 ~ 1 V that current potential is set, the plating amount is 5 ~ 120 C, and conducting polymer monomer and graphene oxide electrochemical polymerization are deposited on anode surface, then uses washed with de-ionized water, room temperature is dried, and obtains conducting polymer/graphene oxide modified anode;
(3) utilize electrochemical workstation, adopt three-electrode system, with the conducting polymer for preparing in (2)/graphene oxide modified anode as work electrode, with platinum electrode as to electrode, as reference electrode, three electrodes are placed 0.1 ~ 1 molL with saturated calomel electrode or saturated silver chloride electrode
-1In the electrolyte, adopt cyclic voltammetry, it is-1.0 ~ 0 V that reduction potential is set, sweeping speed is 5 mV/s, the reduction number of turns is 10 ~ 20 circles, and conducting polymer/graphene oxide modified anode is reduced to conducting polymer/electrochemical reduction graphene oxide modified anode, uses washed with de-ionized water, room temperature is dried, and namely makes microbiological fuel cell Graphene/conducting polymer anode.
In the above-mentioned preparation, the conducting polymer monomer comprises pyrroles, aniline or thiophene described in the step (1).
In the above-mentioned preparation, preliminary treatment described in the step (2) is at deionized water and 30% H with carbon-based material
2O
2Under 90 ℃, respectively heat 2 h in the aqueous solution.
In the above-mentioned preparation, electrolyte comprises aqueous sodium persulfate solution or the sodium perchlorate aqueous solution described in the step (3).
In the above-mentioned preparation, the described carbon-based material of step (2) comprises carbon felt or graphite felt.
The present invention by electrochemical method at carbon-based electrode substrates polypyrrole/electrochemical reduction graphene oxide composite membrane, prepare a kind of novel electrode, compare with the traditional chemical method, more environmental protection of advantage of the present invention, quick, cost is low, be easy to realize industrialization, the electrode obtained has good bio-compatible stability and electro-chemical activity, the electricity generation performance of the microbiological fuel cell that can significantly improve.
Description of drawings
Fig. 1 is the manufacturing process schematic diagram of galvanic anode of the present invention;
Fig. 2 is the position of galvanic anode of the present invention in battery and the structural representation of whole battery;
Fig. 3 is the output power density curve chart of the embodiment of the invention 1;
Fig. 4 is the output power density curve chart of the embodiment of the invention 2;
Fig. 5 is the output power density curve chart of the embodiment of the invention 3;
Fig. 6 is the output power density curve chart of the embodiment of the invention 4.
Embodiment
Below in conjunction with specific embodiment the present invention is done further concrete detailed description the in detail, but embodiments of the present invention are not limited to this, the technological parameter for not indicating especially can carry out with reference to routine techniques.
Embodiment 1:
As shown in Figure 1, the manufacturing process schematic diagram of galvanic anode, among the figure 1 be electrochemical workstation, 2 for to electrode, 3 for reference electrode, 4 for work electrode; Wherein, a refers to mixed solution (pyrrole monomer and graphene oxide aqueous suspension), and b refers to polypyrrole/graphene oxide composite membrane (constant voltage method electropolymerization), and c refers to polypyrrole/electrochemical reduction graphene oxide composite membrane (cyclic voltammetry reduction).Prepare according to the following steps anode:
(1) be that 200 mg graphene oxides are dissolved in the 40 mL deionized waters with quality, the concentration of system is 5mgmL
-1Graphene oxide aqueous suspension solution.Pyrrole monomer 8 mmol are joined in the graphene oxide aqueous suspension solution again and make mixed liquor, the concentration of conducting polymer monomer in mixed liquor is 0.2 molL
-1, at room temperature behind magnetic agitation 10 min, and ultrasonic 5 min, make mixed electrolytic solution;
(2) utilize electrochemical workstation, adopt three-electrode system, will be with deionized water and 30% H
2O
2The aqueous solution respectively heats the pretreated graphite felt anode of 2 h as work electrode under 90 ℃, with platinum electrode as to electrode, as reference electrode, three electrodes are placed mixed electrolytic solution with saturated calomel electrode, adopt the constant voltage galvanoplastic, it is 0.8 V that current potential is set, the plating amount is 30 C, pyrroles/graphene oxide electrically conductive composite electrochemical polymerization is deposited on anode surface, the electrode washed with de-ionized water after the modification, room temperature is dried, and obtains polypyrrole/graphene modified oxide anode;
(3) utilize electrochemical workstation, adopt three-electrode system, as work electrode, as to electrode, as reference electrode, three electrodes are placed 0.1 molL with saturated calomel electrode with platinum electrode with the anode after the modification for preparing in (2)
-1Na
2SO
4In the electrolyte, adopt cyclic voltammetry, it is-1.0 ~ 0 V that reduction potential is set, sweeping speed is 5 mV/s, the reduction number of turns is 20 circles, and polypyrrole/graphene modified oxide anode is reduced to polypyrrole/electrochemical reduction graphene oxide modified anode, will reduce the rear electrode washed with de-ionized water, room temperature is dried, and can make desired microorganisms fuel cell Graphene/conducting polymer anode.
The microbiological fuel cell (see figure 2) is comprised of battery filling opening 1, conduction titanium silk 2, amberplex 3, anode chamber's housing 4, modified anode 5, preliminary treatment graphite felt negative electrode 6, cathode chamber housing 7, shell holder 8 in the present embodiment.
Wherein the preparation method of negative electrode preliminary treatment graphite felt 2 is as follows: boil the hydrogen peroxide solution of graphite felt 10% 2 hours 90 ℃ of lower water-baths (1), then boiled 2 hours with the water-bath under same temperature of isopyknic deionized water, uses oven for drying again; (2) graphite felt is cut into (long 2cm * wide 3cm) size; (3) with the titanium silk graphite felt is put on.
Assembled battery: the anode for preparing is installed on the anode casing, and concrete grammar is as follows: (1) passes the titanium silk on the modified anode by interior outward from the anode casing aperture, and the modified anode plane is parallel with the anode casing board plane; (2) with AB glue titanium silk and anode casing aperture are glued, place and made its curing in about 5 minutes.(3) with pretreated negative electrode by (1) (2) method cathode chamber of packing into, again amberplex is pressed on the cathode chamber housing, then cathode shell, amberplex are fixed the screw nut of screwing at last with anode casing.Battery by Fig. 2 assemble complete after.(4) with 50 mmolL
-1Potassium ferricyanide solution join in the cathode casing by the negative electrode liquid filling hole, recycle silicon plug plug is good.(5) sodium lactate solution is joined (sodium lactate solution concentration is 10 mmol/L in the battery) in the anode cassette by the anode liquid filling hole, add again the pure bacterium of 2 ml Xi Washi, the phosphate buffer solution that adds at last pH=8.0, recycle silicon plug plug is good, and (4) (5) operation is all carried out at aseptic working platform.In external circuit, connect the resistance of 2000 Ω, connect data acquisition unit and carry out image data, image data is set is spaced apart collection in 1 minute once.By the time cell voltage reaches when stablizing, the start battery success.(sweeping speed is 1 mV s by linear scanning method
-1) measure the power density curve (see figure 3) of battery, the power density of battery maximum reaches 2143 mW/m
2(see figure 3).
Present embodiment as different from Example 1 anode constant voltage electroplates that the plating amount is 60 C in the polymerization modification.Other conditions are all identical with specific embodiment 1.This moment, the power density of battery maximum reached 3351 mW/m
2(see figure 4).
Present embodiment as different from Example 1 anode is the preliminary treatment graphite felt electrode of unmodified.Other conditions are all identical with specific embodiment 1.Anode of microbial fuel cell is identical with embodiment 1 in the present embodiment.This moment the battery maximum power density to reach only be 180 mW/m
2(see figure 5).
The present embodiment as different from Example 1 electroplate liquid of anode modification is the graphene oxide aqueous suspension that does not add pyrrole monomer.The present embodiment anode is prepared as follows: (1) is with 5 mgml
-1The graphene oxide aqueous suspension is at room temperature behind magnetic agitation 10 min, and ultrasonic 5 min; (2) utilize electrochemical workstation, adopt three-electrode system, with pretreated carbon-based material anode as work electrode, with platinum electrode as to electrode, as reference electrode, three electrodes are placed aaerosol solution with saturated calomel electrode, adopt and the voltage galvanoplastic, it is 0.8 V that current potential is set, the plating amount is 90 C, and the electrochemical polymerization of graphene oxide electrically conductive composite is deposited on anode surface, obtains the graphene oxide modified anode, electrode washed with de-ionized water after the modification, room temperature is dried; (3) utilize electrochemical workstation, adopt three-electrode system, as work electrode, as to electrode, as reference electrode, three electrodes are placed 0.1 molL with saturated calomel electrode with platinum electrode with the anode after the modification of preparation in (2)
-1Na
2SO
4In the electrolyte, adopt cyclic voltammetry, it is-1.0 ~ 0 V that reduction potential is set, sweeping speed is 5 mV/s, the reduction number of turns is 20 circles, and the graphene oxide modified anode is reduced to electrochemical reduction graphene oxide modified anode, will reduce the rear electrode washed with de-ionized water, room temperature is dried, and can make the desired microorganisms anode of fuel cell.Other conditions are all identical with specific embodiment 1.This moment, the maximum power density of battery was 854 mW/m
2(see figure 6).
Above-described embodiment is the better execution mode of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under Spirit Essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. microbiological fuel cell is characterized in that comprising the steps: with the preparation method of Graphene/conducting polymer anode
(1) graphene oxide is dissolved in the deionized water, making concentration is 1 ~ 15 mgmL
-1Graphene oxide aqueous suspension solution, the conducting polymer monomer is joined in the graphene oxide aqueous suspension solution make mixed liquor again, the concentration of conducting polymer monomer in mixed liquor is 0.1 ~ 0.5 molL
-1, at room temperature behind magnetic agitation 5 ~ 30 min, and ultrasonic 5 ~ 30 min, make mixed electrolytic solution;
(2) utilize electrochemical workstation, adopt three-electrode system, with pretreated carbon-based material as work electrode, with platinum electrode as to electrode, with saturated calomel electrode or saturated silver chloride electrode as reference electrode, three electrodes are placed described mixed electrolytic solution, adopt the constant voltage galvanoplastic, it is 0.5 ~ 1 V that current potential is set, the plating amount is 5 ~ 120 C, and conducting polymer monomer and graphene oxide electrochemical polymerization are deposited on anode surface, then uses washed with de-ionized water, room temperature is dried, and obtains conducting polymer/graphene oxide modified anode;
(3) utilize electrochemical workstation, adopt three-electrode system, with the conducting polymer for preparing in (2)/graphene oxide modified anode as work electrode, with platinum electrode as to electrode, as reference electrode, three electrodes are placed 0.1 ~ 1 molL with saturated calomel electrode or saturated silver chloride electrode
-1In the electrolyte, adopt cyclic voltammetry, it is-1.0 ~ 0 V that reduction potential is set, sweeping speed is 5 mV/s, the reduction number of turns is 10 ~ 20 circles, and conducting polymer/graphene oxide modified anode is reduced to conducting polymer/electrochemical reduction graphene oxide modified anode, uses washed with de-ionized water, room temperature is dried, and namely makes microbiological fuel cell Graphene/conducting polymer anode.
2. microbiological fuel cell according to claim 1 is characterized in that with the preparation method of Graphene/conducting polymer anode the conducting polymer monomer comprises pyrroles, aniline or thiophene described in the step (1).
3. microbiological fuel cell according to claim 1 is characterized in that with the preparation method of Graphene/conducting polymer anode preliminary treatment described in the step (2) is at deionized water and 30% H with carbon-based material
2O
2Under 90 ℃, respectively heat 2 h in the aqueous solution.
4. microbiological fuel cell according to claim 1 is characterized in that with the preparation method of Graphene/conducting polymer anode electrolyte comprises aqueous sodium persulfate solution or the sodium perchlorate aqueous solution described in the step (3).
5. microbiological fuel cell according to claim 1 is characterized in that with the preparation method of Graphene/conducting polymer anode the described carbon-based material of step (2) comprises carbon felt or graphite felt.
6. microbiological fuel cell is characterized in that with Graphene/conducting polymer anode, is prepared from by the described method of claim 1 to 5 any one.
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| CN111613802B (en) * | 2020-06-10 | 2022-04-22 | 中国船舶重工集团公司第七二五研究所 | Modified carbon brush electrode and preparation method thereof |
| CN115032253A (en) * | 2022-05-12 | 2022-09-09 | 北京理工大学 | Efficient electropolymerization L-arginine modified electrode and method for improving performance of microbial electrochemical system |
| CN115032253B (en) * | 2022-05-12 | 2023-05-05 | 北京理工大学 | High-efficiency electropolymerization L-arginine modified electrode and method for improving performance of microbial electrochemical system |
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