CN111916808A - SmFCs for strengthening electrogenesis decontamination of cobaltosic oxide photocathode and preparation method thereof - Google Patents
SmFCs for strengthening electrogenesis decontamination of cobaltosic oxide photocathode 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
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- 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
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Abstract
The invention discloses SMFCs for strengthening electrogenesis decontamination of a cobaltosic oxide photocathode and a preparation method thereof. The method comprises the following steps: (1) dissolving cobalt nitrate in a methanol solution, and adding deionized water to obtain a red solution; (2) adding sodium dodecyl benzene sulfonate into the step 1 to obtain a red solution; (3) placing the suspension in TeflonHeating the dragon-lined stainless steel autoclave in an oven, and cooling to room temperature to obtain a cobaltosic oxide precursor loaded on the graphite felt; (4) washing the obtained precursor with ethanol and deionized water respectively, and drying in an oven after washing; (5) calcining in a muffle furnace to obtain Co3O4A photocathode. Co with oxygen generating characteristics3O4The photocatalyst supported carbon-based electrode is an SMFC photocathode. Effectively improves the oxygen reduction reaction rate of the cathode and reduces the recombination of photo-generated electron hole pairs.
Description
Technical Field
The invention belongs to the environmental protection industry, in particular relates to a deposit type microbial fuel cell (SMFCs) taking Co3O4 photocatalytic material as an oxygen-producing photocathode to strengthen the electricity production and decontamination, and also relates to a Co3O4 photocatalytic material3O4The preparation method of photoelectric cathode uses solar radiation as driving force and adopts Co3O4The photocatalysis material load electrode is used as a photoelectric cathode to strengthen the sediment type microbial fuel cell to repair the endogenous pollution and the electricity generation performance of the lake.
Background
The sediment is an important component of a fresh water environment ecosystem and is a special ecological environment which integrates a large number of microorganisms and chemical substances. The microorganisms are the main driving force of water-sediment material circulation, play an important role in the material circulation, and utilize the natural metabolic activity of the microorganisms in the sediment to carry out bioremediation, which is widely accepted as a feasible selection, but the efficiency is relatively low, the controllability is poor, and the application of the microorganisms is severely restricted. In this regard, there is a study that suggests the concept that electrochemical methods can be an effective means to stimulate the bioremediation of deposits.
Sediment Microbial Fuel Cells (SMFCs) are electrochemical devices based on Sediment environment systems, provide electron acceptors for Sediment layers by utilizing the potential energy gradient of a mud-water interface naturally existing in the environment, directly convert chemical energy in organic matters into electric energy by utilizing the catalytic action of microorganisms in the Sediment layers, and realize in-situ remediation of Sediment and simultaneously generate electric energy.
Current research on SMFCs focuses on electricity generation and bioremediation, but due to mass transfer limitations, the bioavailability of macromolecular organic matter, and the rate of cathodic Oxygen reduction (ORR) reaction, SMFCs are still less efficient in degradation than most chemical enhancement processes, and have low output power. The oxygen is the optimal electron acceptor of the SMFCs cathode, and researches show that the cathode properly performs surface aeration to increase the concentration of dissolved oxygen in overlying water, so that the electric energy output of the SMFCs can be improved, and the degradation rate of organic matters in sediments can be improved. In order to increase the cathode ORR rate, a noble metal such as Pt is usually introduced as the MFC cathode ORR catalyst to increase the output of the system. However, due to the high cost and susceptibility to poisoning of Pt, alternative electrocatalysts are currently under investigation.
Co3O4Is a p-type semiconductor, has the characteristics of higher thermal stability, chemical stability, low solubility, electrocatalytic performance and the like, and is widely researched for generating O by photolysis catalysis due to excellent oxidizing ability, strong absorption capacity to visible light and lower energy band gap (2.1eV)2。Co3O4The electrocatalyst is applied to the MFCs electrode in a role, and due to the ORR catalytic activity, the ORR on the surface of the electrode can be accelerated, and the cathode resistance is obviously reduced, so that the internal resistance of the whole system is obviously reduced, and the performance of the MFCs system is improved. But with respect to Co3O4The application of the photocatalyst in SMFCs is not reported.
Disclosure of Invention
The invention aims to provide a deposited microbial fuel cell which uses cobaltosic oxide photocatalytic material as an oxygen-producing photoelectric cathode to strengthen electrogenesis decontamination, has simple structure and convenient use, and the cathode of the deposited microbial fuel cell adopts Co with oxygen-producing characteristic3O4The photocatalyst supported carbon-based material electrode is used as a photocathode of the SMFC. By Co3O4The composite material is compounded with a carbon-containing material, so that the photocatalytic performance of the composite material is improved, photo-generated electrons and holes are generated under the condition of sunlight irradiation, and water can be photolyzed to generate oxygenThe gas provides an electron acceptor for the cathode region of the Sediment microbial fuel cell, can also promote the cathode oxygen reduction reaction of the SMFCs, and promotes the transfer of electrons from the anode to the cathode of the Sediment Microbial Fuel Cell (SMFCs), thereby enhancing the pollutant removal capacity and the electricity generation performance of the SMFCs system.
The invention also aims to provide a preparation method of the cobaltosic oxide photocathode, which is easy to implement and simple and convenient to operate, effectively improves the oxygen reduction reaction rate of the cathode, and reduces the recombination of photo-generated electron-hole pairs.
In order to achieve the purpose, the invention adopts the following technical measures:
cobaltosic oxide (Co)3O4) The deposit type microbial fuel cell using photocatalysis material as oxygen-producing photoelectric cathode to intensify electricity-producing decontamination is irradiated by sunlight and cobaltosic oxide (Co)3O4The following are the same) photocathode, biological anode, upper water covering layer, sediment layer, muddy water interface, outer wire, external resistor constitute its characterized in that: outer leads are respectively connected with Co3O4The photocathode is connected with an external resistor, the biological anode is connected with the external resistor, a sediment layer (5-10 cm thick) is arranged on the biological anode, and an overlying water layer (10-20 cm thick) is arranged on the sediment layer. Co having oxygen generating characteristics3O4Photocatalysts are combined with cathode materials to serve as photocathodes of Sediment Microbial Fuel Cells (SMFCs), and the Co is combined with the cathode materials to serve as photocathodes of the SMFCs3O4The preparation method of the photocathode adopts a solvothermal method. The electricity generation process comprises the following steps; mixing Co3O4The photoelectric cathode floats on the water surface, the biological anode is embedded with the sediment layer, the biological anode and the sediment layer are connected by an external lead, and an external resistor forms a closed loop. An aerobic cathode region of the sediment microbial fuel cell is arranged above the mud-water interface, and an anaerobic or anoxic cathode region of the sediment microbial fuel cell is arranged below the mud-water interface.
Solves the problems of poor electricity generation effect caused by the oxygen deficiency of the cathode region of the sediment microbial fuel cell, low reaction efficiency of cathode oxygen reduction and the likeAnd the pollutant removal rate is low. By using cheap Co in cathode3O4The photoelectric catalyst replaces noble metal catalysts such as Pt and the like, and the photoelectric cathode is prepared by adopting a simple solvothermal method together with a carbon-based electrode, so that the technical cost is further reduced, and meanwhile, the electricity generation performance of a Sediment microbial fuel cell (SMFCs, the same as below) and the purification effect on water quality and bottom mud are improved. Co3O4Not only the electrocatalytic effect but also the photocatalytic oxygen production and the decomposition of organic pollutants are shown in the SMFCs.
A preparation method of a cobaltosic oxide photocathode comprises the following steps:
(1) mixing cobalt nitrate (Co (NO)3)26H2O, the same below) was dissolved in a methanol solution and deionized water was added to form a red solution;
(2) adding sodium dodecyl benzene sulfonate into the step 1 to obtain a red solution, and performing ultrasonic treatment on the red solution to form a suspension;
(3) putting the suspension obtained in the step 2 into a Teflon (Teflon) lined stainless steel autoclave, putting the pretreated electrode with a proper size (matched with the size of the actual SMFCs) into the autoclave, sealing, heating in an oven at the temperature of 130-200 ℃ for 4-6h, taking out after treatment, and cooling to room temperature (20-25 ℃) to obtain Co loaded on a graphite felt3O4A precursor;
(4) washing the precursor obtained in the step 3 with 75% ethanol and deionized water for 3-5 times, drying in an oven after washing, controlling the temperature at 45-60 ℃ and the time at 22-26 h to obtain a clean and impurity-free precursor;
(5) calcining the product obtained in the step 4 in a muffle furnace at the temperature of 300-350 ℃ for 2-4h to obtain Co3O4A photocathode.
As a preferred aspect of the above technical means, the Co provided by the present invention3O4The preparation method of the photocathode material further comprises part or all of the following technical characteristics:
as an improvement of the above technical solutionIn the step 1, cobalt nitrate (Co (NO)3)2·6H2The mass volume ratio (w (g) v (mL)) of the O to the methanol solution is 1:30-1:20, and the volume ratio of the methanol to the deionized water is 10:1-30: 1.
As an improvement of the technical proposal, in the step 2, the mass-to-volume ratio of the sodium dodecyl benzene sulfonate to the red solution (w (g): v (mL)) is 1:14-1: 16.
As an improvement of the technical scheme, in the step 2, the ultrasonic treatment time is 20-30 min.
As an improvement of the above technical scheme, in the step 3, the temperature of the oven is controlled to be 130-200 ℃, and the treatment time of the oven is controlled to be 4-6 h.
As an improvement of the above technical solution, in the step 3, the electrode material is one of carbon cloth, a carbon fiber brush, a carbon felt, an activated carbon fiber felt, graphene, or a graphite felt.
As an improvement of the technical scheme, in the step 4, the temperature of the oven is controlled to be 45-60 ℃, and the drying time is controlled to be 22-26 h.
As an improvement of the technical scheme, in the step 5, the temperature of the muffle furnace is controlled to be 300-350 ℃, and the calcining time is controlled to be 2-4 h.
The structure of the sediment type microbial fuel cell comprises Co3O4A photocathode, a carbon cloth, a carbon felt, a graphite felt or an activated carbon fiber felt anode, an electrode support, an external lead and an external resistor of 100-1000 omega.
Through the technical measures of the five steps:
the hydrothermal reaction taking place in the reaction kettle and the calcination process in the muffle furnace are key steps of the technology.
Solves the technical problems and difficulties that noble metal catalysts such as Pt and the like are expensive, the SMFCs cathode oxygen reduction reaction rate is low, the output power is low, the pollutant degradation efficiency is low and the like.
According to the invention, the cheap Co3O4 photoelectric catalyst is used for replacing Pt and other noble metal catalysts on the cathode, and the photoelectric cathode and the carbon-based electrode are prepared by adopting a simple solvothermal method, so that the technical cost is further reduced, and the electricity generation performance of SMFCs and the purification effect of water quality and bottom mud are obviously improved.
Co is much studied in the prior art3O4Application of Co in MFCs as electrocatalyst3O4Not only shows the electrocatalytic effect, but also has the functions of photocatalytic oxygen generation and organic pollutant decomposition.
Co3O4Compared with the conventional SMFCs, the application of the photocathode in the SMFCs has the advantages that the electricity generation amount is improved by 10-50%, and the COD removal rate of the overlying water is improved by 25-45%.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention has the functions of photocatalytic oxygen generation and electrocatalysis of Co3O4The photocathode is arranged in the overlying water of the lake, the anode is arranged in the sediment or municipal sludge, and Co is used3O4Is located at a valence band position lower than H2Oxidation potential of O, Co3O4The photocathode generates photo-generated electrons after absorbing the energy of incident light through sunlight irradiation, the generated photo-generated electrons are mainly used for two parts, one part is combined with a photo-generated hole again, the energy carried by the electrons is consumed in different forms such as heat, and the other part moves to the surface of the catalyst to participate in cathode ORR of the SMFCs, so that the pollutant processing capacity and the electricity generation performance of the SMFCs are enhanced. Meanwhile, except for a part of strong oxidative photogenerated holes left at the position of the valence band and recombined with electrons, the rest holes move to the surface of the catalyst to oxidize water to generate O2Or oxidatively degrading other organic pollutants in the overlying water to continuously provide electron donor O for SMFCs cathode2And the stability and the performance of SMFCs are further improved.
Drawings
FIG. 1 is a Co3O4The photocatalysis material is used as the sediment type microbial fuel cell for strengthening the electrogenesis decontamination of the oxygen-generating photocathode.
In the figure: 1-irradiation by sunlight; 2-Co3O4A photocathode; 3-a bioanode; 4-upper water layer; 5-sediment layer (seriously polluted lake sediment); 6-mud-water interface; 7-outerA wire; 8-external resistor (1000 Ω).
Detailed Description
Example 1:
a cobaltosic oxide photocatalytic material is used as a sediment type microbial fuel cell for strengthening electrogenesis decontamination of an oxygen-producing photocathode, which consists of sunlight irradiation 1, a cobaltosic oxide photocathode 2, a biological anode 3, an upper water-covering layer 4, a sediment layer 5, a muddy water interface 6, an outer lead 7 and an external resistor 8, and is characterized in that: the external lead 7 is respectively connected with the cobaltosic oxide photocathode 2 and the external resistor 8, the biological anode 3 is connected with the external resistor 8, a sediment layer 5 (about 8cm in thickness) is arranged on the biological anode 3, and an upper water coating layer 4 (about 12cm in thickness) is arranged on the sediment layer 5. The electricity generation process comprises the following steps; mixing cobaltosic oxide (Co)3O4) The photoelectric cathode floats on the water surface, the biological anode is embedded with the sediment layer, the biological anode and the sediment layer are connected by an external lead, and an external resistor forms a closed loop. The aerobic cathode area of the sediment microbial fuel cell is arranged above the mud-water interface, and the anaerobic or anoxic area of the sediment microbial fuel cell is arranged below the mud-water interface.
The problems of low efficiency, poor controllability and the like of biological repair by utilizing natural metabolic activity of microorganisms in the sediment are solved through the connection and the position relation among the components, a proper electron acceptor can be provided for the microorganisms in the sediment through the connection of the biological anode and the photoelectric cathode, and the biological repair of the sediment is enhanced by utilizing an electrochemical method. Furthermore, Co3O4The photocathode is used as a photoelectrocatalysis material, on one hand, the oxygen reduction rate of the cathode can be enhanced, on the other hand, photo-generated electrons and holes can be generated after solar radiation is absorbed, the degradation efficiency of organic pollutants in a cathode region is enhanced, and oxygen generated by photolysis of water is used as a cathode electron acceptor, so that the electricity generation efficiency and the pollutant removal performance of SMFCs are further enhanced. Compared with the conventional SMFCs, the power generation amount is improved by 10-50%, and the COD removal rate of the overlying water is improved by 25-45%.
Example 2:
cobaltosic oxide (Co)3O4) Method for preparing photocathode, its stepsThe method comprises the following steps:
(1) 1.5g of Co (NO)3)2·6H2O was dissolved in 40mL of methanol and 3.0mL of deionized water was added to form a red solution, Co (NO)3)2·6H2The mass volume ratio of O to the methanol solution (w (g) v (mL)) is 1:27, and the volume ratio of methanol to deionized water is 13: 1;
(2) adding 3.0g of sodium dodecyl benzene sulfonate into the step 1 to obtain a red solution, and carrying out ultrasonic treatment on the red solution to form a suspension, wherein the mass-to-volume ratio (w (g): v (mL)) of the sodium dodecyl benzene sulfonate to the red solution is 1:14, and the ultrasonic treatment time is 25 min;
(3) putting the suspension obtained in the step 2 into a stainless steel autoclave with a Teflon (Teflon) lining, putting a graphite felt electrode which is 6cm in diameter and is pretreated into the autoclave, sealing the autoclave, heating the graphite felt electrode in a drying oven (150 ℃, 4 hours), taking out the graphite felt electrode, and cooling the graphite felt electrode to room temperature (20-25 ℃) to obtain Co loaded on the graphite felt3O4A precursor; the electrode material is one of carbon cloth, carbon fiber brushes, carbon felts, activated carbon fiber felts, graphene or graphite felts;
(4) and (3) washing the precursor obtained in the step (3) with 75% ethanol and deionized water for 3-5 times respectively, and drying in an oven after washing, wherein the temperature of the oven is controlled at 60 ℃, and the drying time is 24 hours. Obtaining a clean and impurity-free precursor;
(5) calcining the product obtained in the step 4 in a muffle furnace to obtain Co3O4And the temperature of the photoelectric cathode in a muffle furnace is 300 ℃, and the calcining time is 3 h.
The cathode material with the photoelectrocatalysis performance is obtained through the specific steps, the cathode oxygen reduction rate can be effectively improved, the cathode resistance is reduced, meanwhile, under the illumination condition, water is photolyzed to generate oxygen, and a continuous electron acceptor can be provided for the cathode.
Claims (4)
1. A cobaltosic oxide photocatalytic material is used as a sediment type microbial fuel cell for strengthening electrogenesis decontamination of an oxygen-producing photocathode, which comprises a cobaltosic oxide photocathode (2), a biological anode (3), an upper water-covering layer (4), a sediment layer (5), an outer lead (7) and an external resistor (8), and is characterized in that: the external lead (7) is respectively connected with the cobaltosic oxide photocathode (2) and the external resistor (8), the biological anode (3) is connected with the external resistor (8), the biological anode (3) is provided with a sediment layer (5), and the sediment layer (5) is provided with an upper water coating layer (4).
2. The method for preparing a cobaltosic oxide photocathode according to claim 1, which comprises the steps of:
(1) dissolving cobalt nitrate in a methanol solution, and adding deionized water to form a red solution, wherein the mass volume ratio of the cobalt nitrate to the methanol solution is 1:30-1:20, and the volume ratio of the methanol to the deionized water is 10:1-30: 1;
(2) adding sodium dodecyl benzene sulfonate into the step (1) to obtain a red solution, and performing ultrasonic treatment on the red solution to form a suspension, wherein the mass-to-volume ratio of the sodium dodecyl benzene sulfonate to the red solution is 1:14-1: 16;
(3) placing the suspension obtained in the step (2) in a Teflon lining stainless steel autoclave, sealing the pretreated electrode after entering the autoclave, heating in an oven at the temperature of 130-200 ℃ for 4-6h, taking out the pretreated electrode after treatment, cooling to room temperature to obtain a cobaltosic oxide precursor loaded on a graphite felt, controlling the temperature of the oven at 130-200 ℃ and controlling the treatment time of the oven at 4-6 h;
(4) washing the precursor obtained in the step (3) with 75% ethanol and deionized water for 3-5 times respectively, drying in an oven after washing, controlling the temperature at 45-60 ℃ and the time at 22-26 h to obtain a clean and impurity-free precursor, controlling the temperature of the oven at 45-60 ℃ and the drying time at 22-26 h;
(5) calcining the product obtained in the step (4) in a muffle furnace at the temperature of 300-350 ℃ for 2-4h to obtain Co3O4The temperature of the photoelectric cathode and the muffle furnace is controlled at 350 ℃ and the calcination time is controlled at 2-4 h.
3. The method of claim 2, wherein the method comprises the following steps: the ultrasonic treatment time in the step (2) is 20-30 min.
4. The method of claim 2, wherein the method comprises the following steps: in the step (3), the electrode material is one of carbon cloth, carbon fiber brush, carbon felt, activated carbon fiber felt, graphene or graphite felt.
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Application publication date: 20201110 |