CN108767301B - Size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell and preparation method thereof - Google Patents
Size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell and preparation method thereof Download PDFInfo
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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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- 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
Abstract
The invention discloses a size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell and a preparation method thereof; a size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell comprising a cathode and an anode, characterized in that: the cathode adopts a carbonized algae tube, and the algae tube contains the protein nucleus chlorella powder; the inner surface of the algae tube is stuck with a separation film with the pore size less than 1 μm; the outer wall of the cathode is wound with a titanium wire, and the anode is inserted into the algae tube along the central axis direction of the algae tube; cover plates are respectively arranged at two ends of the algae pipe and fixed by bolts; one cover plate is provided with an electrolyte inlet, and the other cover plate is provided with an electrolyte outlet; the invention has the advantages of good performance, controllable size, low energy consumption, simple method, convenient operation and low cost, can be widely applied to the fields of energy, chemical industry, environmental protection and the like, and has good application prospect.
Description
Technical Field
The invention relates to a microbial fuel cell, in particular to a size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell and a preparation method thereof.
Background
In recent years, with the development of industrial society, energy crisis and water pollution become two major problems which plague the development of human beings, and therefore, the development and utilization of environmentally friendly renewable energy has become one of the important research directions in the field of energy research. As a novel Microbial energy conversion technology, Microbial Fuel Cells (MFCs) can generate electric energy while degrading organic substances in sewage, have unique environmental effects and economic benefits, contribute to reducing the cost of sewage treatment, and attract extensive attention of researchers in various countries around the world. In recent years, with the intensive research, the electricity generating performance of the microbial fuel cell is greatly improved, but the higher manufacturing and operating cost and the lower output power of the microbial fuel cell are still bottleneck factors limiting the expanded application of the microbial fuel cell. The cathode is an important component of the microbial fuel cell, and the manufacturing cost and the performance characteristics of the cathode have a crucial influence on the practical utilization of the MFC. The air cathode can significantly reduce the system operation cost compared with the traditional liquid cathode because the oxygen in the air is used as the electron acceptor of the cathode. However, most of the conventional catalysts for catalyzing oxygen reduction reaction are noble metal catalysts, and are not suitable for being applied to MFC. In recent years, carbon oxygen reduction air cathodes have attracted more and more attention due to their high performance and low cost. The pore structure and oxygen reduction catalytic activity of the air cathode catalytic layer have a significant effect on the performance of the cathode. Therefore, it is very important to find an air cathode with low cost, high catalytic activity, rich pore structure and controllable size.
The cathode of the current microbial fuel cell can be divided into a sheet air cathode and a three-dimensional tubular air cathode. The sheet air cathode is mainly prepared by taking structural materials such as carbon cloth, metal meshes and the like as a substrate, simultaneously taking adhesives such as Nafion membrane solution or Polytetrafluoroethylene (PTFE) and the like as catalyst adhesives, and adopting the modes of brushing, hot pressing and the like. But the catalyst is easy to be unevenly distributed by brushing, the preparation process is complex, and the catalyst is seriously wasted; the adhesive Nafion is expensive and has higher cost; PTFE has hydrophobicity, which is not beneficial to the material transmission in the catalytic layer; particularly, the sheet-shaped air cathode has limited catalyst loading capacity due to the electrode structure, and when the catalyst layer is too thick, the material transmission efficiency inside the catalyst layer is reduced, thereby affecting the electricity generation performance of the battery.
The three-dimensional tubular air cathode is more suitable for the expanded utilization of the MFC due to the good expandability of the three-dimensional tubular air cathode. The traditional tubular air cathode is manufactured by two methods: firstly, the flexible substrate is used for manufacturing a sheet-shaped air cathode, and then the air cathode is bent to be manufactured into a tubular shape. The tubular air cathode prepared by the method has no essential difference from the traditional sheet air cathode, and can not overcome the defects caused by the sheet air cathode; the other is a tubular cathode made of natural tubular materials, such as a bamboo charcoal tube, but the size and the structure of the tubular cathode are uncontrollable, the tubular cathode excessively depends on the structure of the materials, the oxygen reduction catalytic performance of the tubular cathode is poor, the bamboo has large difference, experiments are difficult to repeat, and the tubular cathode is difficult to use on a large scale. Therefore, the development of the tubular cathode with controllable size and excellent oxygen reduction performance has better practical application prospect.
Disclosure of Invention
The invention aims to provide a carbonaceous tubular oxygen reduction cathode microbial fuel cell and a preparation method thereof.
In order to solve the above technical problem, a first technical solution of the present invention is: the preparation method of the size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell is characterized by comprising the following steps of: the method comprises the following steps:
A. preparing a cathode material: putting deionized water into a beaker, and mixing the deionized water and the agar powder according to a mixing ratio of 1L: 80 g-1L: adding 90g of agar powder, heating and stirring to be viscous, adding fiber powder and chlorella pyrenoidosa powder, and stirring to be uniformly mixed; the ratio of the agar powder to the fiber powder to the chlorella pyrenoidosa powder is 4:1: 15-4.5: 1: 17; adding the mixed solution into a concentric cylindrical mold, wherein a central hole is formed in the concentric cylindrical mold; solidifying the mixed solution to form an algae tube, taking out the formed algae tube, and freeze-drying the algae tube in a freeze-drying box at the temperature of-20 to-25 ℃ for 12 to 18 hours for later use.
B. Carbonizing a cathode material: placing the cut algae tube in a high-temperature tube electric furnace, vacuumizing and filling nitrogen, heating to 900-950 ℃ at a heating rate of 8-10 ℃/min, and performing nitrogen atmosphere (nitrogen flow of 35 cm)3/min～40cm3Min) carbonizing for 2-2.5 hours, and then naturally cooling until the furnace temperature is reduced to be below 100 ℃ and taking out the algae tube.
C. Preparing a cathode: b, placing the algae tube obtained after the heat treatment in the step B in a 2M-2.2M hydrochloric acid solution for soaking for 24 hours to remove metal and nonmetal impurities in the algae tube; taking out, washing with deionized water and alcohol for several times, and drying; after the completion, a layer of separation membrane with the pore size less than 1 μm is pasted on the inner wall of the algae tube.
D. Assembling the battery: winding a titanium wire on the outer side of the cathode prepared in the step C, and inserting the anode into the algae tube along the central axis direction of the cathode; and two ends of the cathode are respectively provided with a cover plate and fixed by bolts, one cover plate is provided with an electrolyte inlet, and the other cover plate is provided with an electrolyte outlet, so that the tubular cathode microbial fuel cell is formed.
According to the preferable scheme of the preparation method of the size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell, the separation membrane is a polyether sulfone membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane or a glass fiber membrane.
The second technical scheme of the invention is that the size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell comprises a cathode and an anode, and is characterized in that: the cathode adopts a carbonized algae tube, and the algae tube contains the protein nucleus chlorella powder; the inner surface of the algae tube is stuck with a separation film with the pore size less than 1 μm; the outer wall of the cathode is wound with a titanium wire, and the anode is inserted into the algae tube along the longitudinal axis direction of the algae tube; cover plates are respectively arranged at two ends of the algae pipe and fixed by bolts; one of the cover plates is provided with an electrolyte inlet, and the other cover plate is provided with an electrolyte outlet.
According to the preferable scheme of the size-controllable carbonaceous tube type oxygen reduction cathode microbial fuel cell, the algae tube further comprises agar powder and fiber powder; and mixing the agar powder, the fiber powder and the globulina powder according to the ratio of 4:1: 15-4.5: 1: 17.
According to the preferable scheme of the size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell, the separation membrane is a polyether sulfone membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane or a glass fiber membrane.
The specific principle of the invention is as follows: firstly, the chlorella pyrenoidosa is used as a precursor and a structural basis of a cathode, and the chlorella pyrenoidosa is a nitrogen and phosphorus enrichment material. And (5) pouring and forming in the mold to obtain the algal tube structure preliminarily. The gel property of the agar ensures that the size structure of the electrode is fixed, and the acrylic fiber enhances the mechanical strength of the algae tube and the conductivity after carbonization. In the process of freeze-drying the algae tube, ice is sublimated to enable the algae tube to have an abundant communicated pore structure, and the dried algae tube is carbonized for 2 hours at 900 ℃ in a nitrogen atmosphere, so that the abundant communicated pore structure in the algae tube is fixed to ensure the transmission of substances in an electrode, and a carbon skeleton structure rich in nitrogen and phosphorus elements is obtained; the high temperature carbonization at 900 ℃ ensures that the carbonized material has lower ohmic internal resistance. The nitrogen-phosphorus-doped carbonaceous material has a large number of nitrogen-phosphorus-containing functional groups, can effectively perform oxygen adsorption and catalytic reaction, and has excellent catalytic performance. The inner wall of the air cathode is pasted with a layer of separating material with the pore diameter less than 1 mu m, so that the short circuit caused by direct contact between the cathode and the anode can be effectively prevented, and bacteria can be prevented from growing on the cathode, thereby avoiding the adverse effect of the biological film on the performance of the cathode.
According to the preferable scheme of the preparation method of the carbonaceous tubular oxygen reduction cathode microbial fuel cell, the separation membrane adopts a polyether sulfone membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane or a glass fiber membrane and the like.
According to a preferable scheme of the preparation method of the carbon tube type oxygen reduction cathode microbial fuel cell, an anode substrate of the microbial fuel cell is made of carbon cloth, carbon brushes, carbon paper, carbon felt, carbon rods or graphite sheets.
The size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell has the beneficial effects that: the invention adopts natural cheap materials as the precursor and the structural material, on one hand, the manufacturing and processing cost of the microbial fuel cell is greatly reduced, and meanwhile, the size is controllable, so that the cathode can meet the actual requirements of different degrees, and in addition, the tubular air cathode has rich interconnected pore structure, so that the material transmission is not limited; the chlorella pyrenoidosa is rich in nitrogen and phosphorus elements, so that a large amount of C-N and C-P chemical bonds are contained on the surface of the air cathode after carbonization, oxygen adsorption and catalytic reaction can be effectively carried out, the carbon cathode has better oxygen reduction performance, and the integral electricity production performance of the microbial fuel cell is improved; the invention has the advantages of good performance, controllable size, low energy consumption, simple method, convenient operation and low cost, can be widely applied to the fields of energy, chemical industry, environmental protection and the like, and has good application prospect.
Drawings
Fig. 1 is a schematic structural diagram of a size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell. FIGS. 2a, 2b, and 2c are photographs of a cross-section of a carbonaceous algal tube under a scanning electron microscope at different resolutions, respectively.
FIGS. 2d, 2e and 2f are photographs of the outer surface of a carbonaceous algal tube under a scanning electron microscope at different resolutions, respectively.
Fig. 3a is a power density curve of a microbial fuel cell according to the present invention.
FIG. 3b is a graph showing the polarization of the cathode and anode using the microbial fuel cell of the present invention.
Fig. 4a is an electrochemical ac impedance spectrum of a microbial fuel cell air cathode according to the present invention.
Fig. 4b is a graph comparing electrochemical ac impedance spectra of a microbial fuel cell of the present invention and a microbial fuel cell using Pt/C as a cathode catalyst.
Fig. 5 is a plot of a linear voltammetric scan of an air cathode of a microbial fuel cell according to the invention.
Detailed Description
The present invention will be further specifically described below with reference to examples, but the embodiments of the present invention are not limited thereto.
Referring to fig. 1, a method for preparing a size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell is characterized in that: the method comprises the following steps:
A. preparing a cathode material: putting deionized water into a beaker, and mixing the deionized water and the agar powder according to a mixing ratio of 1L: 80 g-1L: adding 90g of agar powder, heating and stirring to be viscous, adding fiber powder and chlorella pyrenoidosa powder, and stirring to be uniformly mixed; the ratio of the agar powder to the fiber powder to the chlorella pyrenoidosa powder is 4:1: 15-4.5: 1: 17; adding the mixed solution into a concentric cylindrical mold, wherein a central hole is formed in the concentric cylindrical mold; solidifying the mixed solution to form an algae tube, taking out the formed algae tube, and freeze-drying the algae tube in a freeze-drying box at the temperature of-20 to-25 ℃ for 12 to 18 hours for later use; the fiber powder is acrylic fiber powder.
B. Carbonizing a cathode material: placing the cut algae tube in a high-temperature tube electric furnace, vacuumizing and filling nitrogen, heating to 900-950 ℃ at the heating rate of 8-10 ℃/min, and keeping the nitrogen flow at 35cm under the nitrogen atmosphere3/min～40cm3And/min, carbonizing for 2-2.5 hours, naturally cooling, and taking out the algae tube when the furnace temperature is reduced to be below 100 ℃.
C. Preparing a cathode: b, placing the algae tube obtained after the heat treatment in the step B into a 2M-2.2M hydrochloric acid solution for soaking for 24 hours, taking out the algae tube, cleaning the algae tube for a plurality of times by using deionized water and alcohol, and drying the algae tube; after the completion, a layer of separation membrane with the pore size less than 1 μm is pasted on the inner wall of the algae tube.
D. Assembling the battery: winding a titanium wire on the outer side of the cathode prepared in the step C, and inserting the anode into the algae tube along the central axis direction of the cathode; and two ends of the cathode are respectively provided with a cover plate and fixed by bolts, one cover plate is provided with an electrolyte inlet, and the other cover plate is provided with an electrolyte outlet, so that the tubular cathode microbial fuel cell is formed.
In specific embodiments, the separation membrane is a polyethersulfone membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane or a glass fiber membrane.
The anode substrate of the microbial fuel cell adopts carbon cloth, carbon brushes, carbon paper, carbon felt, carbon rods or graphite sheets.
A size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell comprises a cathode 8 and an anode 5, wherein the cathode 8 adopts a carbonized algae tube, and the algae tube contains protein nucleus chlorella powder, agar powder and fiber powder; the algae tube is prepared by mixing deionized water, agar powder, fiber powder and protein core chlorella powder according to the weight ratio of 50: 4:1: 15-50: 4.5:1:17 ratio mixing and curing. The inner surface of the algae tube is stuck with a separation membrane 6 with the pore diameter less than 1 μm; the separation membrane adopts a polyether sulfone membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane or a glass fiber membrane. The anode substrate adopts carbon cloth, carbon brushes, carbon paper, carbon felt, carbon rods or graphite sheets. The titanium wire 3 is wound on the outer wall of the cathode 8, and the anode 5 is inserted into the algae tube along the central axis direction of the algae tube; two ends of the algae pipe are respectively provided with a cover plate 7, and the cover plates 7 are fixed by bolts 2 and screws 4; one of the cover plates is provided with an electrolyte inlet 9, and the other cover plate is provided with an electrolyte outlet 1.
Example 1: the size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell comprises the following preparation methods: the method comprises the following steps:
A. preparing a cathode structure: chlorella pyrenoidosa is used as a precursor. Adding 4g of agar powder into 50mL of deionized water in a beaker, heating and stirring the mixture to be viscous, adding 1g of fibers, adding 15g of chlorella pyrenoidosa algae powder after uniformly stirring, stirring the mixture until uniformly mixing, adding the mixed solution into a concentric cylindrical mold, wherein a central hole is formed in the concentric cylindrical mold, so that the mixed solution is solidified to form an algae tube, and the wall surface is ensured to be free of bubbles. Taking out the formed algae tube, freezing at-20 deg.C for 12 hr, drying in a freeze drying oven, and cutting to obtain algae tube with height of 4.9cm, inner diameter of 3.4cm and outer diameter of 4.5 cm.
B. Carbonizing a cathode material: placing the cut algae tube in a high-temperature tube electric furnace, vacuumizing and filling nitrogen, heating to 900 ℃ at a heating rate of 10 ℃/min, and controlling the nitrogen flow to be 40cm in the nitrogen atmosphere3Carbonizing for 2 hours at min, naturally cooling until the furnace temperature is reduced to below 100 ℃, and taking out. The carbonized algae tube is arranged under a scanning electron microscope to observe the microscopic characteristics of the algae tube, the carbonized algae tube can keep rich interconnected pore structures and provide a better channel for material transmission, and a picture under the scanning electron microscope is shown in figure 2.
C. Preparing a cathode: and D, polishing the sample obtained after the heat treatment in the step B from two ends of the pipe to form the algae pipe with the length of 2.5cm and a flat section. Soaking the algae tube in 2M hydrochloric acid solution for 24 hours, taking out, washing with deionized water and alcohol for several times, and drying. After finishing, a polytetrafluoroethylene film with the pore size smaller than 1 mu m is pasted on the inner wall of the tube.
D. Assembling the battery: and D, winding a titanium wire on the outer side of the cathode prepared in the step C, and inserting an anode carbon brush with the diameter of 0.8cm and the length of 2.1cm along the central axis direction of the cathode. The anode substrate adopts carbon cloth, carbon brushes, carbon paper, carbon felt, carbon rods or graphite sheets. And circular cover plates are respectively arranged at two ends of the tubular cathode and are fixed by bolts, an electrolyte inlet is reserved on one cover plate, and an electrolyte outlet is reserved on the other cover plate, so that the tubular cathode microbial fuel cell is formed.
EXAMPLES example 2
Example 2: the preparation method of the carbonaceous tubular oxygen reduction cathode microbial fuel cell is different from the preparation method of the embodiment 1 in that the proportion of deionized water, agar powder, fiber and chlorella pyrenoidosa powder is 50: 4.5:1: 17; the separation membrane is a glass fiber membrane. The assembled battery was started in batches under the condition of 50 Ω external resistance, and the performance curve was measured after 10 days of culture, as shown in fig. 3a and 3b, indicating that the battery had better output power of cathode performance. Wherein the 1500COD culture medium comprises the following components: 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 the microelement can be FeSO4·7H2O、ZnCl2、MnCl·4H2O、H3BO3、CaCl2·6H2O、CuCl2·2H2O，NiCl2·6H2O or NaMoO4·2H2O，CoCl2·6H2O, and the like.
In addition, the assembled cell was scanned using an electrochemical workstation under open circuit conditions, and the measured EIS curves are shown in fig. 4a and 4b, which shows that the cell has a small ohmic and mass transfer internal resistance.
Example 3: the preparation method of the size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell is different from the preparation method of the embodiment 1 in that the proportion of deionized water, agar powder, fiber and chlorella pyrenoidosa powder is 50: 4.2: 1: 16; the separation membrane is a polyvinylidene fluoride membrane, the cathode of the algae tube wound with titanium wires is immersed in a culture medium with 1500COD, 30min of saturated oxygen is introduced, a three-electrode system is adopted, an electrochemical workstation is used, scanning is carried out at a scanning speed of 10mV/s from 0.4V to-0.7V, and the measured LSV curve is shown in figure 5. In the three-electrode system, the working electrode is the cathode of the algae tube, the counter electrode is a platinum electrode, and the reference electrode is an Ag/AgCl electrode.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (4)
1. The preparation method of the size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell is characterized by comprising the following steps of: the method comprises the following steps:
A. preparing a cathode material: putting deionized water into a beaker, adding agar powder, heating and stirring to be viscous, adding fiber powder and globuline powder, and stirring to be uniformly mixed; adding the mixed solution into a concentric cylindrical mold, wherein a central hole is formed in the concentric cylindrical mold; solidifying the mixed solution to form an algae tube, taking out the formed algae tube, and placing the formed algae tube in a freeze drying box for freeze drying for later use;
B. carbonizing a cathode material: placing the algae tube in a high-temperature tube electric furnace, vacuumizing and filling nitrogen, heating to 900-950 ℃, carbonizing in the nitrogen atmosphere, and naturally cooling until the furnace temperature is reduced to below 100 ℃ and taking out the algae tube;
C. preparing a cathode: b, soaking the algae tube obtained after the heat treatment in the step B in a hydrochloric acid solution, taking out the algae tube, cleaning the algae tube for a plurality of times by using deionized water and alcohol, and drying the algae tube; after the completion, a layer of separation membrane (6) with pores smaller than 1 mu m is pasted on the inner wall of the algae pipe;
D. assembling the battery: winding a titanium wire on the outer side of the cathode prepared in the step C, and inserting the anode into the algae tube along the central axis direction of the cathode; and two ends of the cathode are respectively provided with a cover plate (7) and fixed by bolts (2), one cover plate is provided with an electrolyte inlet, and the other cover plate is provided with an electrolyte outlet, so that the tubular cathode microbial fuel cell is formed.
2. The method of making a dimensionally-controllable carbonaceous tubular oxygen-reducing cathode microbial fuel cell of claim 1, wherein: deionized water, agar powder, fiber powder and protein core chlorella powder in a mass ratio of 50: 4:1: 15-50: 4.5:1: and 17, mixing.
3. The method for preparing a size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell according to claim 1, wherein the separation membrane is a polyethersulfone membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane or a glass fiber membrane.
4. The carbonaceous tubular oxygen reduction cathode microbial fuel cell prepared by the size-controllable carbonaceous tubular oxygen reduction cathode microbial fuel cell preparation method according to claim 1, 2 or 3.
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| CN101385171A (en) * | 2005-08-31 | 2009-03-11 | 丰田自动车株式会社 | Method for producing tube fuel cell |
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