CN110854394A - Copper-based composite material used as immobilized anode of microbial fuel cell and preparation method thereof - Google Patents
Copper-based composite material used as immobilized anode of microbial fuel cell and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a copper-based composite material used as an immobilized anode of a microbial fuel cell and a preparation method thereof, belonging to the technical field of fuel cells, wherein sodium alginate, agar and activated carbon are mixed to be used as an immobilized solution, a standing and pulling method is adopted to carry out film coating on a copper net, and then the film coated copper net is crosslinked and gelatinized in a calcium chloride solution to obtain the copper-based composite material; and immersing the obtained copper-based composite material into bacterial liquid for adsorption and fixation to prepare the immobilized anode suitable for the microbial fuel cell. The copper-based composite material provided by the invention has good conductivity and biocompatibility, can be used for preparing an immobilized anode of a microbial fuel cell, can obviously improve the electricity generation performance of the microbial fuel cell, and has the advantages of simple preparation method, cheap raw materials and wide development prospect.
Description
Technical Field
The invention belongs to the technical field of fuel cells, relates to preparation of anode materials of microbial fuel cells, and particularly relates to a copper-based composite material used as an immobilized anode of a microbial fuel cell and a preparation method thereof.
Background
The waste water treatment consumes huge energy every year, and brings serious burden to the development of society and economy. Microbial Fuel Cells (MFCs) are an emerging technology that utilizes bacteria to degrade organic matter to produce bioelectrical energy. The wastewater contains a large amount of organic matters, and the microbial fuel cell can utilize the organic matters as electron donors to generate usable electric energy after conversion and decomposition of bacteria, so that the wastewater treatment is realized, and the energy contained in the wastewater is recovered. The MFC utilizes the characteristics of wastewater electricity generation and wastewater treatment, so that people generally think that once the MFC is industrialized, a revolution is brought to the field of sewage treatment, and immeasurable social, environmental and economic benefits are generated.
The productivity and consumption are two important evaluations of whether a technology is valuable, and therefore, increasing the power generation and reducing the cost are important to the industrialization of MFC. The anode is an important component of the microbial fuel cell, serves as a carrier for attachment of microbial electrogenic bacteria, and plays a significant role in the electron transfer process, so that the anode material is an important factor for restricting the electrogenic capability of the microbial fuel cell. Currently, the anode substrate of MFC is mainly carbon-based, such as graphite felt, graphite rod (sheet), carbon cloth, carbon paper, which have good biocompatibility, chemical and microbiological stability, but their electrical conductivity is several orders of magnitude lower than that of metals. An increase in MFC electrode resistivity results in a decrease in cell voltage and power generation, which may not be high for small experimental systems, but may lead to a complete breakdown of electrochemical performance for larger systems. Aiming at the problem, the invention takes the metal copper as the base material, and covers the gel film capable of fixing the microorganism on the basis of the copper mesh as the anode, thereby providing a new idea for the industrialized development of MFC.
Disclosure of Invention
The invention provides a copper-based composite material used as an immobilized anode of a microbial fuel cell and a preparation method thereof, aiming at the problems of low electricity generation performance and high manufacturing cost of the conventional microbial fuel cell.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a copper-based composite material used as an immobilized anode of a microbial fuel cell comprises the following steps:
1) stirring and dissolving sodium alginate in deionized water at 55 ℃, heating agar to 120 ℃ to dissolve the sodium alginate, cooling to 55 ℃, mixing the two solutions, adding activated carbon, stirring uniformly, and standing the obtained mixed solution in a water bath at 55 ℃ to remove bubbles;
2) immersing the pretreated copper mesh into the mixed solution obtained in the step 1), and standing and pulling to obtain a coated copper mesh;
3) adding the copper mesh coated with the film obtained in the step 2) into a calcium chloride solution for crosslinking and gelling, then taking out, washing and naturally drying in the air to obtain the copper-based composite material.
The mixed solution in the step 1) comprises the following raw materials in parts by weight: 2-6 parts of sodium alginate, 1-6 parts of agar, 1-18 parts of activated carbon and 100 parts of deionized water.
And 2) the pretreatment is to soak the copper mesh in acetone for 24 hours, then wash the copper mesh with deionized water, and then dry the copper mesh.
The mass concentration of the calcium chloride solution in the step 3) is 1-6%; the time of crosslinking gelation is 1-6 h.
In order to effectively fix the microorganisms, the invention adopts the compound of two natural polysaccharides of sodium alginate and agar as an immobilization material. Adopts sodium alginate for immobilization, has convenient formation, high enrichment degree on microbial cells and high priceThe gel is cheap, but the sodium alginate is crisp, the agar has the characteristics of toughness and high elasticity, and the sodium alginate and the agar are compounded to obtain the flexible immobilized gel with good biocompatibility. In order to ensure that the electrons generated by the microorganisms in the fuel cell can be more and more quickly transferred to the copper mesh through the anode, the invention particularly introduces the activated carbon with certain conductivity, which is used as a high-efficiency adsorbent on one hand, and the adhesion of the microorganisms on the anode is enhanced (the adsorption quantity of the microorganisms in the anode is characterized by testing the content of cell phospholipid contained in the anode, and the phospholipid content of the anode containing 1% of the activated carbon is 6.3433 +/-0.102 mu g/cm2The content of the anode phospholipid without the activated carbon is 3.9967 +/-0.047 mu g/cm2) On the other hand, the conductive network is formed inside the immobilized gel by utilizing the immobilized gel, so that the internal resistance of the anode is reduced.
The copper-based composite material prepared by the invention can be used as an immobilized anode of a microbial fuel cell for preparing the microbial fuel cell, and is specifically characterized in that the copper-based composite material is put into a bacterial liquid (mainly sulfate reducing bacteria) in an exponential growth phase for adsorbing for 8-72 h for immobilizing bacteria, so that the copper-based microbial immobilized anode is obtained.
The invention has the following remarkable advantages:
copper metal has higher conductivity than graphite material and is inexpensive. The invention combines the excellent conductivity of the metal copper with the good biocompatibility of the sodium alginate and the agar, and simultaneously utilizes the adsorbability of the activated carbon and the conductive network formed in the immobilized gel, thereby obviously improving the electricity generation performance of the microbial fuel cell.
The invention has simple preparation and low synthesis cost, and the microbial fuel cell formed by the invention has the characteristics of high electricity generation efficiency, long electricity generation period and the like, and can promote the industrialized application of the microbial fuel cell.
Drawings
FIG. 1 is an SEM image of a copper-based composite material obtained by the present invention.
FIG. 2 is an SEM image of the copper-based microorganism-immobilized anode prepared by adsorbing the bacterial liquid according to the present invention.
Fig. 3 is a cell power density curve of a microbial fuel cell prepared using the immobilized anodes obtained in example 1, comparative example 1 and comparative example 2.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
(1) Dissolving 3 g of sodium alginate solution in 55 ℃ and 50 ml of deionized water, stirring and dissolving, adding 2g of agar into 50 ml of deionized water, heating to about 120 ℃ to dissolve the agar, cooling to 55 ℃, mixing the two solutions, adding 6 g of activated carbon, stirring uniformly, and standing the obtained mixed solution in a water bath at 55 ℃ to remove bubbles;
(2) soaking the copper mesh in acetone for 24 hours to remove organic impurities, then washing with deionized water, drying, soaking into the mixed solution obtained in the step (1), and standing and pulling to obtain a coated copper mesh;
(3) adding the coated copper mesh into a 2% calcium chloride solution for crosslinking for 1h, then taking out, washing and naturally drying to obtain a copper-based composite material;
(4) and (3) placing the copper-based composite material after ultraviolet sterilization into sulfate reducing bacteria liquid in an exponential growth phase for adsorption for 24 hours to obtain the copper-based microorganism immobilized anode.
Comparative example 1
The procedure was exactly the same as in example 1 except that no activated carbon was added in step (1), to obtain a copper-based microorganism-immobilized anode containing no activated carbon.
Comparative example 2
And (3) placing the graphite felt after ultraviolet sterilization into sulfate reducing bacteria liquid in an exponential growth phase for adsorption for 24 hours, and then taking the graphite felt as the anode of the microbial fuel cell.
Assembling the microbial fuel cell: carbon felt as cathode electrode, 50mM K3(Fe(CN)6) The solution is used as catholyte and assembled with the obtained anode to prepare the microbial fuel cell with a double-chamber structure.
The anodes prepared in example 1, comparative example 1 and comparative example 2 were respectively installed in a microbial fuel cell reactor to operate, and the measured power density curve of the fuel cell is shown in fig. 3, and the obtained maximum power density is shown in table 1.
TABLE 1 comparison of maximum power densities of different anode materials
As can be seen from the table, when the copper-based composite material of example 1 was used as an anode of a microbial fuel cell, the maximum power density of the resulting fuel cell was significantly higher than that of a conventional microbial fuel cell (comparative example 2) in which a graphite felt was used as an anode. When the active carbon in the embodiment 1 is omitted (the comparative example 1), the maximum power density of the fuel cell is obviously reduced and even lower than that of the conventional microbial fuel cell (the comparative example 2), and the introduction of the active carbon plays a key role in obviously improving the electricity generation performance of the microbial fuel cell.
Example 2
(1) Dissolving 3 g of sodium alginate solution in 55 ℃ and 50 ml of deionized water, stirring and dissolving, adding 2g of agar into 50 ml of deionized water, heating to about 120 ℃ to dissolve the agar, cooling to 55 ℃, mixing the two solutions, adding 3 g of activated carbon, stirring uniformly, and standing the obtained mixed solution in a water bath at 55 ℃ to remove bubbles;
(2) soaking the copper mesh in acetone for 24 hours to remove organic impurities, then washing with deionized water, drying, soaking into the mixed solution obtained in the step (1), and standing and pulling to obtain a coated copper mesh;
(3) adding the coated copper mesh into a 4% calcium chloride solution for crosslinking for 2h, then taking out, washing and naturally drying to obtain a copper-based composite material;
(4) and (3) placing the copper-based composite material after ultraviolet sterilization into sulfate reducing bacteria liquid in an exponential growth phase for adsorption for 24 hours to obtain a copper-based microorganism immobilized anode, and further assembling to obtain the microbial fuel cell.
The immobilized anode is arranged in a microbial fuel cell reactor for operationThe maximum power density is 735 mW/m2。
Example 3
(1) Dissolving 3 g of sodium alginate solution in 55 ℃ and 50 ml of deionized water, stirring and dissolving, adding 2g of agar into 50 ml of deionized water, heating to about 120 ℃ to dissolve the agar, cooling to 55 ℃, mixing the two solutions, adding 18 g of activated carbon, stirring uniformly, and standing the obtained mixed solution in a water bath at 55 ℃ to remove bubbles;
(2) soaking the copper mesh in acetone for 24 hours to remove organic impurities, then washing with deionized water, drying, soaking into the mixed solution obtained in the step (1), and standing and pulling to obtain a coated copper mesh;
(3) adding the coated copper mesh into a 2% calcium chloride solution for crosslinking for 1h, then taking out, washing and naturally drying to obtain a copper-based composite material;
(4) and (3) placing the copper-based composite material after ultraviolet sterilization into sulfate reducing bacteria liquid in an exponential growth phase for adsorption for 24 hours to obtain a copper-based microorganism immobilized anode, and further assembling to obtain the microbial fuel cell.
The immobilized anode is arranged in a microbial fuel cell reactor to operate, and the maximum power density is 1089 mW/m2。
Example 4
(1) Dissolving 2g of sodium alginate solution in 55 ℃ and 50 ml of deionized water, stirring and dissolving, adding 4g of agar into 50 ml of deionized water, heating to about 120 ℃ to dissolve the agar, cooling to 55 ℃, mixing the two solutions, adding 6 g of activated carbon, stirring uniformly, and standing the obtained mixed solution in a water bath at 55 ℃ to remove bubbles;
(2) soaking the copper mesh in acetone for 24 hours to remove organic impurities, then washing with deionized water, drying, soaking into the mixed solution obtained in the step (1), and standing and pulling to obtain a coated copper mesh;
(3) adding the coated copper mesh into a 6% calcium chloride solution for crosslinking for 4 hours, then taking out, washing and naturally drying to obtain a copper-based composite material;
(4) and (3) placing the copper-based composite material after ultraviolet sterilization into sulfate reducing bacteria liquid in an exponential growth phase for adsorption for 72h to obtain a copper-based microorganism immobilized anode, and further assembling to obtain the microbial fuel cell.
The immobilized anode is arranged in a microbial fuel cell reactor to operate, and the maximum power density of 777 mW/m is obtained2。
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. A preparation method of a copper-based composite material used as an immobilized anode of a microbial fuel cell is characterized by comprising the following steps: the method comprises the following steps:
1) stirring and dissolving sodium alginate in deionized water at 55 ℃, heating agar to 120 ℃ to dissolve the sodium alginate, cooling to 55 ℃, mixing the two solutions, adding activated carbon, stirring uniformly, and standing the obtained mixed solution in a water bath at 55 ℃ to remove bubbles;
2) immersing the pretreated copper mesh into the mixed solution obtained in the step 1), and standing and pulling to obtain a coated copper mesh;
3) adding the copper mesh coated with the film obtained in the step 2) into a calcium chloride solution for crosslinking and gelling, then taking out, washing and naturally drying in the air to obtain the copper-based composite material.
2. The method for producing a copper-based composite material according to claim 1, characterized in that: the mixed solution in the step 1) comprises the following raw materials in parts by weight: 2-6 parts of sodium alginate, 1-6 parts of agar, 1-18 parts of activated carbon and 100 parts of deionized water.
3. The method for producing a copper-based composite material according to claim 1, characterized in that: and 2) the pretreatment is to soak the copper mesh in acetone, clean the copper mesh with deionized water and dry the copper mesh.
4. The method for producing a copper-based composite material according to claim 1, characterized in that: the mass concentration of the calcium chloride solution in the step 3) is 1-6%.
5. The method for producing a copper-based composite material according to claim 1, characterized in that: and 4) the time of crosslinking gelation in the step 4) is 1-6 h.
6. Use of a copper-based composite material prepared according to any one of claims 1 to 5 in a microbial fuel cell, characterized in that: and preparing the copper-based composite material into an immobilized anode of the microbial fuel cell, and further assembling to prepare the microbial fuel cell.
7. Use of a copper-based composite material according to claim 6 in a microbial fuel cell, wherein: the method for preparing the immobilized anode comprises the step of putting the copper-based composite material into free mixed bacterial liquid in an exponential growth phase for adsorption for 8-72 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114725404A (en) * | 2022-04-22 | 2022-07-08 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
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| CN114725404A (en) * | 2022-04-22 | 2022-07-08 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
| CN114725404B (en) * | 2022-04-22 | 2023-09-01 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
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