CN107706428A - A kind of carbon cloth electrode of polyaniline nano flower modification and its production and use - Google Patents
A kind of carbon cloth electrode of polyaniline nano flower modification and its production and use Download PDFInfo
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- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
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Abstract
The invention discloses the preparation method and purposes of a kind of carbon cloth electrode of polyaniline nano flower modification, belong to electrode material technical field；The present invention is using carbon cloth as matrix, and by controlling the ratio between aniline monomer and ammonium persulfate, the in-situ polymerization of polyaniline is carried out in carbon cloth surfaces, after washing is dried, obtains the carbon cloth electrode of polyaniline nano flower modification；The carbon cloth electrode for the polyaniline nano flower modification being prepared can be used for anode of microbial fuel cell, and obtain more unmodified carbon cloth electrode higher current density and power density；The preparation technology of the present invention is simple, and cost is low, and electricity generation performance of microbial fuel cell is good, and the practical application of microbiological fuel cell is had very important significance.
Description
Technical field
The present invention relates to a kind of novel electrode, and in particular to a kind of carbon cloth electrode of polyaniline nano flower modification and its preparation
Method and purposes, belong to electrode material technical field.
Background technology
Polyaniline (PANI) is a kind of highly important conducting polymer, is had due to the diversity of its pattern and structure
Extensive use.Meanwhile PANI had electrochemical redox activity, the biocompatibility become reconciled of electrocatalysis, in PANI
Quinoid structure can speed up the electronic transfer process of anode surface.Therefore, have using PANI progress electrode modifications huge
Application prospect.
Microbiological fuel cell (Microbial Fuel Cells, MFCs) is to produce electricity using microbial degradation organic matter
The technology of energy.This technology has wastewater treatment and the recoverable dual-use function of electricity, and its appearance is at traditional organic wastewater
The significant innovation of reason technology and idea, cause worldwide extensive concern.It is especially increasingly prominent in energy supply and demand contradiction
Go out, today of environmental pollution getting worse, MFCs more shows its superiority.But efficiency of fuel cell generation is relatively low to be hindered it and enters one
Step development.From the point of view of MFCs composition, the attachment of carrier, not only influence electricity-producing microorganism that anode adheres to as electricity-producing microorganism
Amount, and transmission of the electronics from microorganism to anode is influenceed, there is vital influence to improving MFCs electricity generation performances.Therefore,
From the electricity generation ability for improving MFCs, selection has potential anode material and conducted a research, the electricity generation ability to improving MFCs
Tool is of great significance.
At this stage, the commonly used anode material of MFCs technologies is the carbon cloth, carbon paper and glass using carbon material as base stock
Glass carbon etc..Particularly carbon cloth material, quality is soft, space is more, specific surface area is big, conductance is high and cheap and easy to get, most heavy
What is wanted is that active microorganism bacterium in anode chamber is adapted to superficial growth at them.However, studies have shown that if only with carbon cloth
For anode material, MFCs systems can only obtain relatively low power density.In order to improve MFCs electricity generation performance, Many researchers are all
It is directed to MFCs anode is modified and modified to reach the purpose (Electrochimica of its power output of increase
Acta 2017,231:609-616；Journal of Power Sources 2015,283:46-53).Polyaniline is because of its environment
It is friendly, cost is low, many advantages, such as being readily synthesized, adulterating and go doping process simple, be applied to microbiological fuel cell.
Lai et al. obtains adulterating HSO using electrochemical polymerization method4 -Polyaniline is used in microbiological fuel cell, due to Polyaniline-modified
Carbon cloth adds the roughness of anode, improves the electro-chemical activity of anode, reduces the overpotential of anode, polyaniline/carbon cloth
The maximum power density that anode obtains is 5.16W/m3, it is 2.66 times of unmodified carbon cloth, meanwhile, internal resistance is also under 261 Ω
Drop to 90 Ω.Further to improve the chemical property of conducting polymer, the controlledly synthesis to its pattern and structure is to grind at present
Study carefully one of problem the most popular.Because regular, special pattern would generally assign conducting polymer unique physicochemical property, because
And develop the method on morphology controllable synthesis nano structural conductive polymer, so as to improve its chemical property, and meet
Application in microbiological fuel cell field is the most important thing studied at present.Carbon cloth electricity on the modification of PANI nano wires at present
Pole has been reported (Bioresource Technology 2015,192:831-834).However, the carbon cloth of PANI nano flowers modification
Electrode and MFCs applications have no report.
The content of the invention
It is an object of the invention to provide the preparation method and purposes of a kind of carbon cloth electrode of polyaniline nano flower modification, system
The carbon cloth electrode of standby obtained polyaniline nano flower modification be used for microbiological fuel cell can obtain higher current density and
Power density.
Present invention firstly provides a kind of carbon cloth electrode of polyaniline nano flower modification, the electrode is using carbon cloth as matrix, so
Aniline monomer carries out in-situ polymerization in carbon cloth surfaces afterwards, after washing is dried, obtains the carbon cloth electrode of polyaniline nano flower modification.
The present invention also provides a kind of preparation method of the carbon cloth electrode of polyaniline nano flower modification, and it includes following preparation step
Suddenly：
(1) carbon cloth and titanium silk are assembled into carbon cloth electrode, immerses ultrasonic 30min in deionized water, drive surface gas away
Bubble；
(2) tartaric acid, aniline monomer, ammonium persulfate (APS) and deionized water are sequentially added into 20cm vials；Wherein
Tartaric acid, aniline, APS dosage are：0.8mmol:4mmol:1.6-3.2mmol；
(3) carbon cloth electrode that titanium silk is connected with step (1) is immersed in the solution of step (2), stands 12-16h；
(4) electrode of modified in step (3) is taken out, deionized water is washed three times, and air, which dries, to be obtained polyaniline and receive
The carbon cloth electrode of popped rice modification.
Step (1) is described to be ultrasonically treated using the ultrasonic processor that power is 300W.
Final solution volume described in step (2) is 16mL.
Step (3) described dwell temperature is 0~5 DEG C.
The present invention also provides a kind of application of carbon cloth electrode of polyaniline nano flower modification in microbiological fuel cell, tool
Body application process is：
The MFCs that this experiment uses, which is configured as dual chamber, membranous type, and anode chamber and cathode chamber dischargeable capacity are 32mL, middle
Separated by PEM.Titanium silk for connection cathode and anode wire, external 2 kilo-ohms of resistance, using Shewanella for produce electricity bacterium,
Negative electrode using carbon felt as microbiological fuel cell, potassium ferricyanide catholyte, the carbon cloth electrode modified is spent with the polyaniline nano
For anode, the mixed solution of M9 and LB culture mediums is anolyte.Data acquisition device is connected to external resistance both ends, and output voltage is certainly
It is dynamic to recorded in computer, that is, complete the assembling of microbiological fuel cell.The carbon felt specification is 2cm × 3cm；The M9 and LB
Volume ratio 95:5.
Beneficial effect：
The carbon cloth electrode of conductive polyaniline nanometer flower modification provided by the invention and its MFCs applications, are built upon this patent
On the basis of the polyaniline nano flower of method synthesis has higher electro-chemical activity, prepare in acid condition has at present
The nano flower-like polyaniline of electric conductivity there is no pertinent literature to report；Due to using most common, most simple and easy original
Position chemical polymerization, so electrode cost is cheap, is easy to large-scale production；The 3 D stereo nano flower of rule has higher table
Face enhancement effect, adhesion amount of the Shewanella in anode electrode surface can be effectively improved, and then greatly improve MFC property
Energy.According to the electrode prepared by the inventive method, MFCs ceiling voltages are 520.9mV, maximum power density 388.6mWm-
2, maximum current density 2.01Am-2, it is 2.56 times, 6.55 times and 4.29 times of carbon cloth electrode respectively, polyaniline more in recent years
Modified electrode in terms of MFCs performance boosts to having greater advantage (see table 1).To sum up, electrical-conductive nanometer of the invention flower modified electrode
Synthetic method is simple, electrode novel in shape, excellent performance, is had a clear superiority in terms of MFC performance boosts, real to promoting MFC
Border is using significant.
Brief description of the drawings
Fig. 1 is the infrared spectrum for the carbon cloth electrode that embodiment 3 prepares gained polyaniline nano flower modification.
Fig. 2 is the Raman spectrogram for the carbon cloth electrode that embodiment 3 prepares gained polyaniline nano flower modification.
Fig. 3 is the scanning electron microscope (SEM) photograph for the carbon cloth electrode that embodiment 3 prepares gained polyaniline nano flower modification.
Fig. 4 is that embodiment 3 prepares cyclic voltammetric of the carbon cloth electrode of gained polyaniline nano flower modification in 0.5M sulfuric acid
Curve.
Fig. 5 is the cell voltage of the microbiological fuel cell a cycle of embodiment 4.
Fig. 6 is the polarization curve and power curve of the microbiological fuel cell of embodiment 4.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but therefore protection scope of the present invention is not confined to
Following embodiments, but limited by description and claims of this specification.
Embodiment 1：
The preparation of the carbon cloth electrode of polyaniline nano flower modification：
The business carbon cloth of purchase is cut into 1cm × 2cm specifications, is then assembled into electrode with 12cm titanium silks, immersion go from
Ultrasonic 30min in sub- water, drive the bubble on surface away.Aqueous tartaric acid solution (0.8mmol/9mL is sequentially added into 20cm vials
Water) and aniline monomer (5mL, 0.8M, 4mmol) is straight by ammonium persulfate (APS) aqueous solution (2mL, 0.8M, 1.6mmol) under ice bath
Connect and add above-mentioned solution.Then the carbon cloth that sonicated titanium silk connects quickly is immersed in above-mentioned vial, finally the glass
0 DEG C of glass bottle, stand 12h.The carbon cloth through modification is taken out, deionized water is washed three times, and air naturally dry is polyaniline nano
The carbon cloth electrode of flower modification.
Embodiment 2：
The business carbon cloth of purchase is cut into 1cm × 2cm specifications, is then assembled into electrode with 12cm titanium silks, immersion go from
Ultrasonic 30min in sub- water, drive the bubble on surface away.Aqueous tartaric acid solution (0.8mmol/8mL is sequentially added into 20cm vials
Water) and aniline monomer (5mL, 0.8M, 4mmol) is straight by ammonium persulfate (APS) aqueous solution (3mL, 0.8M, 2.4mmol) under ice bath
Connect and add above-mentioned solution.Then the carbon cloth that sonicated titanium silk connects quickly is immersed in above-mentioned vial, finally the glass
5 DEG C of glass bottle, stand 14h.The carbon cloth through modification is taken out, deionized water is washed three times, and air naturally dry is polyaniline nano
The carbon cloth electrode of flower modification.
Embodiment 3：
The business carbon cloth of purchase is cut into 1cm × 2cm specifications, is then assembled into electrode with 12cm titanium silks, immersion go from
Ultrasonic 30min in sub- water, drive the bubble on surface away.Aqueous tartaric acid solution (0.8mmol/7mL is sequentially added into 20cm vials
Water) and aniline monomer (5mL, 0.8M, 4mmol) is straight by ammonium persulfate (APS) aqueous solution (4mL, 0.8M, 3.2mmol) under ice bath
Connect and add above-mentioned solution.Then the carbon cloth that sonicated titanium silk connects quickly is immersed in above-mentioned vial, finally the glass
0 DEG C of glass bottle, stand 16h.The carbon cloth through modification is taken out, deionized water is washed three times, and air naturally dry is polyaniline nano
The carbon cloth electrode of flower modification.
Infrared (such as Fig. 1) is carried out to prepared polyaniline nano flower to characterize, and is as a result shown, what electrically conductive polyaniline was included
Functional group occurs in relevant position, such as 1302 and 1495cm-1Indicate the presence of benzene formula structure, and 1142and 1570cm-1
It is the characteristic absorption peak of quinoid structure.Raman (such as Fig. 2) analysis is carried out to prepared polyaniline nano flower, shown, preparation
Polyaniline is existing in the form of emeraldine salt.Electronic Speculum is scanned to the carbon cloth of prepared polyaniline nano flower modification
Morphology characterization (such as Fig. 3), shows, flower-shaped regular-scattered is presented in carbon cloth electrode surface in the polyaniline of preparation.Prepared is gathered
The carbon cloth electrode of aniline nano flower modification carries out CV tests (such as Fig. 4)：Electrolyte is 0.5M H2SO4, it is 10mV S to sweep speed-1.Survey
To take temperature bright, there are two pairs of symmetrical redox peaks in CV curves, not only show that polyaniline is successfully attached to carbon cloth electrode surface, and
And imply that the electrode containing polyaniline nano flower has higher electro-chemical activity.
Embodiment 4：
The application of the carbon cloth electrode of polyaniline nano flower modification and the performance comparision with traditional carbon cloth electrode：
The MFCs that this experiment uses, which is configured as dual chamber, membranous type, and anode chamber and cathode chamber dischargeable capacity are 32mL, middle
Separated by PEM.In superclean bench, Shewanella (OD600 ,~2.5) is added to sterile M9 and LB and cultivated
In base (30mL, V/V=95/5), sterile sodium lactate (98.2 μ L), Ca are added successively2+(30 μ L) and Mg2+(30 μ L), with reality
The carbon cloth electrode for applying the polyaniline nano flower modification being prepared in example 3 is anode (superclean bench ultraviolet irradiation sterilizing
30min).Negative electrode using 2cm × 3cm carbon felts as microbiological fuel cell, the potassium ferricyanide and potassium chloride catholyte (30mL).Titanium silk
To connect the wire of cathode and anode, external 2 kilo-ohms of resistance.Data acquisition device is connected to external resistance both ends, and output voltage is automatic
It recorded in computer, that is, complete the assembling of microbiological fuel cell.As a result as shown in figure 5, to be prepared in embodiment 3
The carbon cloth electrode of polyaniline nano flower modification is that the MFCs ceiling voltages of anode are 520.9mV, and the MFCs of traditional carbon cloth electrode is most
High voltage is only 146.2mV.Compared with traditional carbon cloth electrode, the carbon cloth electrode of polyaniline nano of the invention flower modification makes
MFCs voltage outputs improve 2.56 times.Fig. 6 is that the electrode is bent as the cell polarization curves figure and power density of MFCs anodes
Line chart, maximum power density 388.6mWm-2, maximum current density 2.01Am-2, and the maximum of traditional carbon cloth electrode
Power density only has 51.5mWm-2, maximum current density 0.38Am-2.Compared with traditional carbon cloth electrode, the present invention
Polyaniline nano flower modification carbon cloth electrode MFCs power densities and current density is improved 6.55 times and 4.29 times respectively.
Result above shows that polyaniline nano flower unique surface appearance and excellent chemical property are to strengthening MFC anode biological electricity
Stream generates important actively impact.
The present embodiment also spends the polyaniline nano of the present invention carbon cloth electrode of modification and disclosed traditional carbon cloth electrode
Performance has carried out comparative analysis, specifically illustrates see table 1, table 1, and the carbon cloth electrode of polyaniline nano of the invention flower modification is in shape
With currently known and differ in terms of looks, prepared by the present invention is the flower-shaped regular-scattered of polyaniline presentation in carbon cloth electrode table
Face；The multiple that power density improves improves much compared to existing, possesses obvious advantage.
Comparative analysis result of the anode electrode of the Polyaniline-modified in recent years of table 1. in MFC
aFor compared to blank control, MFC maximum power density growth rates.
Claims (8)
1. a kind of carbon cloth electrode of polyaniline nano flower modification, it is characterised in that the electrode shows that flower-shaped distribution is presented, described
Flower-shaped regular-scattered is presented in carbon cloth electrode surface in polyaniline.
2. a kind of preparation method of the carbon cloth electrode of polyaniline nano flower modification, it is characterised in that made in accordance with the following steps
It is standby：
Carbon cloth and titanium silk are assembled into carbon cloth electrode, ultrasound in deionized water is immersed, drives blibbing away；
Tartaric acid, aniline monomer, ammonium persulfate and deionized water are sequentially added into vial；
By step（1）In be connected with titanium silk carbon cloth electrode immerse step（2）Solution in, stand a period of time；
Take out step（3）The electrode of middle modified, deionized water washing, air dry the carbon for obtaining polyaniline nano flower modification
Cloth electrode.
3. preparation method according to claim 2, it is characterised in that step（1）The supersound process is using power
For 300W ultrasonic processor, the min of ultrasonic time 30.
4. preparation method according to claim 2, it is characterised in that step（1）The carbon cloth is cut into the cm of 1 cm × 2
Specification, titanium silk specification are 12 cm.
5. preparation method according to claim 2, it is characterised in that step（2）The tartaric acid, aniline, ammonium persulfate
Dosage be：0.8 mmol: 4 mmol: 1.6-3.2 mmol；Described final solution volume is 16 mL.
6. preparation method according to claim 2, it is characterised in that step（3）The dwell temperature is 0 ~ 5 DEG C；Stand
Time is 12-16 h.
A kind of 7. application of carbon cloth electrode of polyaniline nano flower modification in microbiological fuel cell.
8. application according to claim 7, it is characterised in that in the microbiological fuel cell, titanium silk is connection yin, yang
The wire of pole, using Shewanella as electricity production bacterium, the negative electrode using carbon felt as microbiological fuel cell, potassium ferricyanide catholyte, with institute
The carbon cloth electrode for stating polyaniline nano flower modification is anode, and the mixed solution of M9 and LB culture mediums is anolyte；Data acquisition fills
Put and be connected to external resistance both ends, output voltage is automatically logged into computer, that is, completes the assembling of microbiological fuel cell.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244479A (en) * | 2018-08-06 | 2019-01-18 | 江苏大学 | Netted nitrogen-doped carbon cladding manganese dioxide carbon cloth electrode and preparation method and application |
| CN109873171A (en) * | 2019-03-04 | 2019-06-11 | 中国科学技术大学 | A kind of microorganism electrochemical system combination electrode and preparation method thereof |
| CN109962249A (en) * | 2019-04-04 | 2019-07-02 | 湖南师范大学 | Carbon-based anode of microbial fuel cell of polyaminophenylboronic acid and preparation method thereof |
| CN110429286A (en) * | 2019-08-16 | 2019-11-08 | 哈尔滨工业大学 | Application of the titanium nitride nano stick array in anode of microbial fuel cell |
| CN110729487A (en) * | 2019-10-14 | 2020-01-24 | 东莞理工学院城市学院 | Microbial fuel cell based on molybdenum disulfide composite material as anode |
| CN112002946A (en) * | 2020-08-06 | 2020-11-27 | 山东科技大学 | Preparation method and application of polyaniline zinc ion battery of high-voltage platform |
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| CN105837053A (en) * | 2015-01-13 | 2016-08-10 | 广东工业大学 | Titanium dioxide/polyaniline nano-composite structure and preparation method thereof |
| CN106920971A (en) * | 2017-02-16 | 2017-07-04 | 江苏大学 | A kind of cluster polyaniline nano fiber composite carbon electrode and preparation method and purposes |
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- 2017-09-25 CN CN201710875837.4A patent/CN107706428B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837053A (en) * | 2015-01-13 | 2016-08-10 | 广东工业大学 | Titanium dioxide/polyaniline nano-composite structure and preparation method thereof |
| CN106920971A (en) * | 2017-02-16 | 2017-07-04 | 江苏大学 | A kind of cluster polyaniline nano fiber composite carbon electrode and preparation method and purposes |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244479A (en) * | 2018-08-06 | 2019-01-18 | 江苏大学 | Netted nitrogen-doped carbon cladding manganese dioxide carbon cloth electrode and preparation method and application |
| CN109873171A (en) * | 2019-03-04 | 2019-06-11 | 中国科学技术大学 | A kind of microorganism electrochemical system combination electrode and preparation method thereof |
| CN109962249A (en) * | 2019-04-04 | 2019-07-02 | 湖南师范大学 | Carbon-based anode of microbial fuel cell of polyaminophenylboronic acid and preparation method thereof |
| CN109962249B (en) * | 2019-04-04 | 2020-11-20 | 湖南师范大学 | Carbon-based microbial fuel cell anode of poly (m-aminobenzoic acid) boric acid and preparation method thereof |
| CN110429286A (en) * | 2019-08-16 | 2019-11-08 | 哈尔滨工业大学 | Application of the titanium nitride nano stick array in anode of microbial fuel cell |
| CN110729487A (en) * | 2019-10-14 | 2020-01-24 | 东莞理工学院城市学院 | Microbial fuel cell based on molybdenum disulfide composite material as anode |
| CN112002946A (en) * | 2020-08-06 | 2020-11-27 | 山东科技大学 | Preparation method and application of polyaniline zinc ion battery of high-voltage platform |
| CN112002946B (en) * | 2020-08-06 | 2022-04-15 | 山东科技大学 | Preparation method and application of polyaniline zinc ion battery of high-voltage platform |
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