CN110690460B - Cathode material and preparation method thereof, bioelectricity Fenton system and construction method thereof - Google Patents
Cathode material and preparation method thereof, bioelectricity Fenton system and construction 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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/005—Combined electrochemical biological processes
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8605—Porous electrodes
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- 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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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8673—Electrically conductive fillers
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
- H01M2004/8689—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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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
- Y02E60/50—Fuel cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention specifically relates to a cathode material and a preparation method thereof, and the preparation method comprises the following steps: firstly, cutting a magnetic sponge material to be used as a framework material; secondly, carrying out ultrasonic treatment on the graphite oxide suspension to obtain a uniformly dispersed graphene oxide solution; thirdly, soaking the framework material in a graphene oxide solution; fourthly, extruding out the excessive graphene oxide solution in the framework material obtained in the third step, airing, and repeating the third step for 1-5 times; fifthly, placing the product obtained in the step four in FeCl2Heating in water bath, and cooling to room temperature; sixthly, dropwise adding ammonia water into the solution obtained in the step five, adjusting the pH value, and heating in a water bath under a sealing condition; and seventhly, cooling the obtained product in the step six to room temperature, and washing the product with distilled water to obtain the cathode material. In addition, the invention also provides a bioelectricity Fenton system and a construction method thereof. Compared with the prior art, the cathode system in the bioelectricity Fenton system has strong catalytic oxidation capability and strong capability of removing refractory organic matters.
Description
Technical Field
The invention belongs to the technical field of bioelectricity Fenton systems, and particularly relates to a cathode material and a preparation method thereof, and a bioelectricity Fenton system and a construction method thereof.
Background
With the rapid development of economic society, the population number is continuously increased, the living standard is increasingly improved, and the energy demand is also increasingly larger, especially the energy required in the sewage treatment process, such as aeration tanks, sludge pumps, plug-flow devices and other devices, however, the sewage and the sludge contain rich organic matters, namely biomass energy. Microbial Fuel Cells (MFCs) are a new technology that can degrade organic pollutants and convert biomass energy stored in organic matters into electric energy by the catalytic action of anaerobic microorganisms, and realize the output of electric energy. MFCs can be classified into dual chamber MFCs, air cathode MFCs, membrane-less MFCs, flat plate MFCs, deposition MFCs, and the like, according to their structures. Deposition-type MFCs, i.e., bio-electro-fenton systems, greatly reduce the manufacturing and operating costs of MFCs because they do not use proton exchange membranes.
The bioelectricity Fenton system is characterized in that a biological anode is buried in a sediment, a cathode material is exposed in the air or aerated, oxygen is used as an electron acceptor, and the sediment and sewage on the upper layer of the bioelectricity Fenton system form a solid-liquid interface, so that an anaerobic environment and an aerobic environment are formed. Protons generated in the anode deposit are transferred to the cathode chamber through the solid-liquid interface, and extracellular electrons generated at the same time reach the cathode material through an external circuit; on the surface of the cathode material, oxygen and protons and electrons undergo redox reactions, which can be divided into four-electron processes (shown in equation a) and two-electron processes (shown in equation b) according to the reaction mechanism. Wherein, the two-electron process can generate peroxide radical ions which can degrade part of pollutants difficult to degrade, if ferrous ions exist in the system, the two-electron process and the generated peroxide radical ions can form a Fenton system, thereby improving the degradation capability of the cathode to the pollutants.
O2+4H++4e-→2H2O Eθ＝1.229V(vs SHE) (a)
O2+H2O+2e-→HO- 2+OH- Eθ＝－0.065V(vs SHE) (b)
At present, carbon materials such as graphite blocks, graphite felts, carbon brushes and carbon fibers are mostly adopted as cathode materials of the bioelectricity Fenton system. The cathode materials can promote the cathode redox reaction to generate a four-electron process, but cannot generate enough peroxyhydrogen radical ions, namely, the catalytic oxidation capacity of a cathode system is weak, and the capacity of removing difficultly degraded organic matters is poor.
Disclosure of Invention
One of the objects of the present invention is: aiming at the defects of the prior art, the preparation method of the cathode material is provided, and is simple to operate and low in cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a cathode material comprises the following steps:
cutting a magnetic sponge material into a square with the side length of 1-5 cm, and taking the square as a framework material;
step two, carrying out ultrasonic treatment on the graphite oxide suspension to obtain a uniformly dispersed graphene oxide solution;
step three, placing the framework material cut in the step one into the graphene oxide solution prepared in the step two for soaking;
extruding out excessive graphene oxide solution in the framework material obtained in the step three, airing, and repeating the step three for 1-5 times;
step five, placing the obtained product in FeCl2Heating the solution in a water bath at the temperature of 70-95 ℃ for 6-24 hours, and cooling to room temperature;
step six, dropwise adding ammonia water into the solution obtained in the step five, slowly stirring and adjusting the pH value to 9-12, and heating the solution in a water bath at the temperature of 60-95 ℃ for 0.5-6 h under a sealed condition;
and step seven, cooling the obtained material in the step six to room temperature, and cleaning the material with distilled water to obtain the graphite phase nitrogen modified and ferroferric oxide doped magnetic sponge cathode material.
The addition of the magnetic sponge material not only improves the conductivity of the cathode material, but also increases the biocompatibility of the cathode material; the ammonia water not only provides an alkaline environment for the formation of the magnetic sponge material, but also provides a precursor for the modification of graphite phase nitrogen.
As an improvement of the preparation method of the cathode material, the magnetic sponge material is polyurethane sponge or foamed nickel.
In the second step, the content of graphene oxide in the graphite oxide suspension is 2-8 mg/mL.
In the third step, the soaking time is 30-120 min.
As an improvement of the preparation method of the cathode material, in step five, the FeCl is2The concentration of the solution is 0.1-1 mol/L.
The second purpose of the invention is: provides a cathode material with strong catalytic oxidation capability, which is prepared by the preparation method described in any section of the specification.
The third purpose of the invention is that: there is provided a bioelectrofenson system for enhancing the ability of a cathode system to degrade contaminants, comprising a cathode material as described hereinbefore in the description. In the bioelectrochemical Fenton system, electrons from the anode material, hydrogen peroxide and Fe generated from the cathode material2+The electro-Fenton system is formed together, and the degradation capability of the cathode system on pollutants is improved.
The fourth purpose of the invention is that: there is provided a method of constructing the bioelectricity Fenton system described in the foregoing description, comprising the steps of:
taking sludge with the thickness of 5-20 cm as anode sediment, and burying an anode material at a position 0.5-15 cm above the bottom of the anode sediment;
slowly adding 100-1000 mL of sewage above the anode sediment to form a sewage layer, and placing the cathode material in the sewage layer;
thirdly, arranging aeration equipment 3-10 cm above a solid-liquid interface of the anode sediment and the sewage layer;
and step four, connecting the cathode material and the anode material through an external circuit, and connecting a resistor of 50-10000 omega in series as an external circuit load to form the bioelectricity Fenton system.
The improvement of the construction method of the bioelectricity Fenton system further comprises a fifth step of injecting 10-500 mL of 0.2-1.5 g/L sodium acetate solution into the anode sediment in each operation period after the bioelectricity Fenton system stably operates.
As an improvement of the construction method of the bioelectricity Fenton system, the anode material is graphite blocks or graphite felt.
Compared with the prior art, the invention has the beneficial effects that:
(1) the magnetic sponge cathode material modified by graphite phase nitrogen and doped with ferroferric oxide prepared by the invention has the advantages of simple preparation method and lower cost.
(2) In the preparation process of the cathode material, the addition of the magnetic sponge material not only improves the conductivity of the material, but also increases the biocompatibility of the material; the ammonia water not only provides an alkaline environment for the formation of the magnetic sponge material, but also provides a precursor for the modification of graphite phase nitrogen.
(4) In the bioelectrochemical Fenton system of the present invention, electrons from the anode material, hydrogen peroxide and Fe from the cathode material2+The electro-Fenton system is formed together, and the degradation capability of the cathode system on pollutants is improved.
Drawings
FIG. 1 is a schematic diagram showing the structure of the bioelectricity Fenton system of the present invention.
FIG. 2 is a graph showing the voltage change with time of the bioelectrochemical Fenton system in example 1.
FIG. 3 is a graph showing the voltage change with time of the bioelectrochemical Fenton system in example 2.
FIG. 4 is a graph showing the voltage change with time of the bioelectrochemical Fenton system in example 3.
FIG. 5 is a graph showing the relationship between voltage and current after the bioelectricity Fenton system of embodiments 1 to 3 is connected to resistors with different resistances.
FIG. 6 is a graph showing the relationship between the power density and the current after the bioelectricity Fenton system of embodiments 1 to 3 is connected to resistors with different resistance values.
FIG. 7 is a graph showing the time course of methyl orange concentration when the bio-electro-Fenton system of examples 1 to 3 and comparative examples 1 to 3 is used for removing methyl orange.
Wherein: 1-anode sediment, 2-anode material, 3-sewage layer, 4-cathode material, 5-aeration equipment and 6-external circuit load.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and the accompanying drawings, but the embodiments of the invention are not limited thereto.
Example 1
Preparing a cathode material:
1) cutting the polyurethane resin sponge into a square with the side length of 3cm as a framework material;
2) carrying out ultrasonic treatment on the graphite oxide suspension liquid of 2mg/mL for 60min by using an ultrasonic cleaning machine to obtain a uniformly dispersed graphene oxide solution;
3) placing the cut framework material in the step 1) into the graphene oxide solution prepared in the step 2) to be soaked for 60 min;
4) extruding an excessive graphene oxide solution in the framework material, airing, and repeating the step 3) for 1-5 times;
5) placing the FeCl obtained in the step 4) at 0.5mol/L2Heating in water bath at 80 deg.C for 12 hr, and cooling to room temperature;
6) dropwise adding ammonia water obtained in the step 5), adjusting the pH to 11, and heating in a water bath at 90 ℃ for 5 hours under a sealed condition;
7) and cooling to room temperature, opening the reactor in a fume hood, and washing the reactor for a plurality of times by using distilled water to obtain the graphite-phase nitrogen-modified ferroferric oxide-doped magnetic sponge cathode material.
Construction of bioelectricity Fenton System:
1) taking a layer of river bottom sludge or municipal sludge with the thickness of 15cm as an anode deposit 1, and burying an anode material 2 such as a graphite block or a graphite felt at a position 5cm above the bottom of the anode deposit 1;
2) slowly adding 500mL of sewage above the anode sediment 2 to form a sewage layer 3, and placing the cathode material 4 prepared above into the sewage layer 3;
3) 5cm above the solid-liquid interface of the anode sediment 1 and the sewage layer 3 is provided with an aeration device 5;
4) connecting the cathode material 4 and the anode material 2 through an external circuit, and connecting a 1000 omega resistor in series as an external circuit load 6 (shown in figure 1);
5) after the bioelectricity Fenton system is stably operated, 50mL of 0.5g/L sodium acetate solution is slowly injected into the anode sediment as a nutrient substance of the anode microorganisms in each operation period.
Example 2
In contrast to example 1, the preparation of the cathode material:
1) cutting the polyurethane resin sponge into a square with the side length of 3cm as a framework material;
2) carrying out ultrasonic treatment on the graphite oxide suspension liquid of 2mg/mL for 60min by using an ultrasonic cleaning machine to obtain a uniformly dispersed graphene oxide solution;
3) placing the cut framework material in the step 1) into the graphene oxide solution prepared in the step 2) to be soaked for 60 min;
4) extruding an excessive graphene oxide solution in the framework material, airing, and repeating the step 3) for 1-5 times;
5) placing the FeCl obtained in the step 4) at 1mol/L2Heating in water bath at 80 deg.C for 12 hr, and cooling to room temperature;
6) dropwise adding ammonia water obtained in the step 5), adjusting the pH to 11, and heating in a water bath at 90 ℃ for 5 hours under a sealed condition;
7) and cooling to room temperature, opening the reactor in a fume hood, and washing the reactor for a plurality of times by using distilled water to obtain the graphite-phase nitrogen-modified ferroferric oxide-doped magnetic sponge cathode material.
The rest is the same as embodiment 1, and the description is omitted here.
Example 3
In contrast to example 1, the preparation of the cathode material:
1) cutting the polyurethane resin sponge into a square with the side length of 3cm as a framework material;
2) carrying out ultrasonic treatment on the graphite oxide suspension liquid of 2mg/mL for 60min by using an ultrasonic cleaning machine to obtain a uniformly dispersed graphene oxide solution;
3) placing the cut framework material in the step 1) into the graphene oxide solution prepared in the step 2) to be soaked for 60 min;
4) extruding an excessive graphene oxide solution in the framework material, airing, and repeating the step 3) for 1-5 times;
5) placing the FeCl obtained in the step 4) at 1mol/L2Heating in water bath at 80 deg.C for 12 hr, and cooling to room temperature;
6) dropwise adding ammonia water obtained in the step 5), adjusting the pH to 10, and heating in a water bath at 90 ℃ for 5 hours under a sealed condition;
7) and cooling to room temperature, opening the reactor in a fume hood, and washing the reactor for a plurality of times by using distilled water to obtain the graphite-phase nitrogen-modified ferroferric oxide-doped magnetic sponge cathode material.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative examples 1 to 3
The difference from the embodiment 1-3 is the construction of the bioelectricity Fenton system:
1) taking a layer of river bottom sludge or municipal sludge with the thickness of 15cm as anode sediment, and burying anode materials such as graphite blocks or graphite felts and the like at a position 5cm above the bottom of the anode sediment;
2) slowly adding 500mL of sewage above the anode sediment to form a sewage layer, and placing the prepared cathode material in the sewage layer;
3) and 5cm above the solid-liquid interface of the anode sediment and the sewage layer is provided with an aeration device.
The rest are the same as embodiments 1 to 3, and are not described herein again.
Performance testing
1) In the stable operation of the bioelectricity Fenton system of examples 1-3, an external circuit was connected to a resistance of 1000 Ω, and voltage was collected every 1min, as shown in FIGS. 2-4. It is apparent that the power generation stabilization time is longest when the ferrous chloride concentration is 1mol/L and the pH is adjusted to 11 with ammonia (example 2), while the output voltage is reduced when the pH is adjusted to 10 with ammonia (example 3).
2) In the test of the power density of the bio-electro-Fenton system in examples 1-3, the method of changing the external resistance was used, and the maximum stable voltage and the power density of the bio-electro-Fenton system at resistances of 10000, 5000, 1000, 500, 250, 100 and 50 Ω were recorded, and the results are shown in FIGS. 5 and 6, respectively. Specifically, the maximum power density was obtained at a ferrous chloride concentration of 1mol/L in example 2, but the power density was reduced by influencing the generation of the magnetic material due to the decrease in pH in example 3.
The cathodes of the bioelectricity Fenton system in test examples 1-3 had good degradation capability for methyl orange, and the results are shown in FIG. 7. It is clear that the removal ability of the bioelectricity Fenton system connected to the external circuit is better than that of the non-connected circuit, and moreover, the removal ability of methyl orange is better than that of example 1 when the concentration of ferrous chloride is 1mol/L in example 2, whereas the removal ability of methyl orange is relatively low in example 3 because of the reduction of pH, a large amount of FeOOH is formed, and the bioelectricity Fenton system cannot be constructed.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (9)
1. The preparation method of the cathode material is characterized by comprising the following steps of:
cutting a sponge material into a square with the side length of 1-5 cm, and taking the square as a framework material; wherein the sponge material is polyurethane resin sponge or foam nickel;
step two, carrying out ultrasonic treatment on the graphite oxide suspension to obtain a uniformly dispersed graphene oxide solution;
step three, placing the framework material cut in the step one into the graphene oxide solution prepared in the step two for soaking;
extruding out excessive graphene oxide solution in the framework material obtained in the step three, airing, and repeating the step three for 1-5 times;
step five, placing the obtained product in FeCl2Heating the solution in a water bath at the temperature of 70-95 ℃ for 6-24 hours, and cooling to room temperature;
step six, dropwise adding ammonia water into the solution obtained in the step five, slowly stirring and adjusting the pH value to 9-12, and heating the solution in a water bath at the temperature of 60-95 ℃ for 0.5-6 h under a sealed condition;
and step seven, cooling the obtained material in the step six to room temperature, and cleaning the material with distilled water to obtain the graphite phase nitrogen modified and ferroferric oxide doped magnetic sponge cathode material.
2. The method for preparing the cathode material according to claim 1, wherein in the second step, the content of graphene oxide in the graphite oxide suspension is 2-8 mg/mL.
3. The method for preparing the cathode material according to claim 1, wherein the soaking time is 30-120 min in the third step.
4. The method for preparing cathode material according to claim 1, wherein in step five, the FeCl is2The concentration of the solution is 0.1-1 mol/L.
5. A cathode material prepared by the preparation method of any one of claims 1 to 4.
6. A bioelectrochemical Fenton system comprising the cathode material according to claim 5.
7. A construction method of the bioelectrical Fenton system according to claim 6, comprising the steps of:
taking sludge with the thickness of 5-20 cm as anode sediment, and burying an anode material at a position 0.5-15 cm above the bottom of the anode sediment;
slowly adding 100-1000 mL of sewage above the anode sediment to form a sewage layer, and placing the cathode material in the sewage layer;
thirdly, arranging aeration equipment 3-10 cm above a solid-liquid interface of the anode sediment and the sewage layer;
and step four, connecting the cathode material and the anode material through an external circuit, and connecting a resistor of 50-10000 omega in series as an external circuit load to form the bioelectricity Fenton system.
8. The method for constructing a bioelectricity Fenton system according to claim 7, further comprising a step five of injecting 10 to 500mL of 0.2 to 1.5g/L sodium acetate solution into the anode deposit every operation period after the bioelectricity Fenton system is stably operated.
9. The method of claim 7, wherein the anode material is graphite block or graphite felt.
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| CN112551681B (en) * | 2020-12-07 | 2023-03-17 | 上海海事大学 | Single-chamber type microbial electro-Fenton system and application thereof |
| CN113044930A (en) * | 2021-03-19 | 2021-06-29 | 西安建筑科技大学 | Tannic acid heterogeneous synergistic electro-Fenton method for catalytic degradation of phenolic organic wastewater |
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