CN109256566B - Electrode bar for microbial electrolysis cell anode and preparation method thereof - Google Patents

Electrode bar for microbial electrolysis cell anode and preparation method thereof Download PDF

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CN109256566B
CN109256566B CN201810990175.XA CN201810990175A CN109256566B CN 109256566 B CN109256566 B CN 109256566B CN 201810990175 A CN201810990175 A CN 201810990175A CN 109256566 B CN109256566 B CN 109256566B
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electrode
metal
rod
iron
anode
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CN109256566A (en
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蒋永荣
秦永丽
谢锦邦
熊昌勋
莫姗姗
韦巧艳
梁英
伍婵翠
张敏
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Guilin University of Electronic Technology
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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
    • H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
    • 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
    • H01M4/8803—Supports for the deposition of the catalytic active composition
    • 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
    • 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
    • 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
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Abstract

The invention discloses an electrode rod for an anode suitable for a microbial electrolytic cell and a preparation method thereof. On the premise of ensuring the conductivity, the electrode bar isolates the electrode from oxygen in air or solution, so that the corrosion speed of the electrode is reduced, and meanwhile, the existence of cement components increases the strength of the electrode, so that the electrode has better mechanical property, and the service life of the electrode in the microbial electrolysis cell is prolonged.

Description

Electrode bar for microbial electrolysis cell anode and preparation method thereof
Technical Field
The invention relates to the technical field of wastewater treatment and microbial electrolysis cells, in particular to an electrode bar used for an anode of a microbial electrolysis cell and a preparation method thereof.
Background
A Microbial Electrolysis Cell (MEC) is a system constructed on the basis of crossing and integrating the disciplines of electrochemistry, microbiology, process technology and the like. The basic principle of MEC is: in the anode chamber, the microorganism is used as a catalyst to carry out biocatalytic reaction, and the microorganism is oxidizedDissolving certain components (such as acetate, glucose and the like) in the matrix in the anode chamber to generate carbon dioxide, protons and electrons, transferring the generated electrons to the surface of the anode and then transferring the electrons to the surface of the cathode through an external circuit, and allowing the protons to reach the cathode chamber in a diffusion mode; in the cathode chamber, protons and electrons diffused to the surface of the cathode are combined to generate products such as hydrogen, methane, and the like. MEC is one of new technologies in the environmental frontier field because of its great potential for efficiently recovering biological energy from wastewater in principle, and at present MEC not only has good treatment effect on domestic sewage, industrial wastewater and refractory organic wastewater, but also can recover H2、CH4、H2O2Formic acid and the like.
The anode of the microbial electrolytic cell is used as a main forming place of a biological membrane, the influence on the attachment, growth, electron transfer and the like of microorganisms is particularly obvious, and an iron anode-microbial electrolytic cell system is mostly adopted in the currently disclosed technology for wastewater treatment and energy recovery. However, the iron anode-microbial electrolysis cell is easy to corrode iron electrodes in practical application, and the corrosion phenomenon of the iron electrodes is more serious along with the accumulation of time, so that the electrodes are hardened, and the electric conduction capability is seriously reduced, thereby greatly reducing the service life of the iron electrodes and limiting the popularization and application of the iron anode-microbial electrolysis system in the practical wastewater treatment. In order to alleviate the corrosion hardening problem of the iron electrode, some researchers adopt such relieving measures as doping other metal materials (forming alloy materials) into the iron electrode or placing the iron electrode in an anaerobic environment, and the like, and although the methods all slow down the corrosion speed of the iron electrode to a certain extent, the application of the iron electrode in a microbial electrolytic cell is limited to a certain extent due to high cost, strict requirements on the operating environment and the like.
Disclosure of Invention
The invention provides an electrode bar for an anode suitable for a microbial electrolysis cell, which is characterized in that a layer of anticorrosive layer prepared by mixing metal powder, cement and fine sand is wrapped outside a common electrode to form the electrode bar for the anode. On the premise of ensuring the conductivity, the electrode bar isolates the electrode from oxygen in air or solution, so that the corrosion speed of the electrode is reduced, and meanwhile, the existence of cement components increases the strength of the electrode, so that the electrode has better mechanical property, and the service life of the electrode in the microbial electrolysis cell is prolonged.
The material of the electrode can be any metal suitable for being used as an anode of the microbial electrolysis cell, and the metal powder in the anticorrosive layer is preferably prepared from metal with the same metal property as the material of the electrode, and can also be prepared from metal with different metal properties. The metal powder is preferably incorporated in an amount not to excessively lower the strength of the anticorrosive coating, and the particle size of the metal powder is smaller than that of the fine sand. The preferred proportion of the components of the anticorrosive layer material provided by the invention is as follows: the volume ratio of the cement to the fine sand to the metal powder is 3-5: 1: 1-3. In order to prevent the electrolytic cell solution from penetrating from the end of the electrode bar where the electrode wire is drawn out, the end may be blocked by covering it with a resin.
In addition, the invention also provides a preparation method of the electrode bar for the anode of the microbial electrolysis cell, which comprises the following steps: (1) mixing cement, fine sand and metal powder according to the volume ratio of 3-5: 1: 1-3 to prepare anticorrosive slurry; the cement may be a conventional construction cement. (2) And spirally winding the electrode wire on the metal rod to obtain the metal electrode body. (3) And suspending the metal electrode body in an inner hollow mold with an inner size larger than that of the metal electrode and an opening at one end, pouring the anticorrosive slurry from the opening end of the mold until the metal electrode is completely wrapped, and removing the mold after solidification is completed to obtain the anticorrosive electrode rod for the anode.
Drawings
Fig. 1 is a schematic structural view of the present invention.
FIG. 2 is a comparison of Tafel curves of an anti-corrosion iron electrode and a common iron electrode in an example of the present invention.
FIG. 3 is a graph showing the results of the test of the use of the corrosion-resistant iron electrode and the common iron electrode in the example of the present invention.
In the drawings: 1. an electrode wire; 2. a metal rod; 3. and (4) an anticorrosive layer.
Detailed Description
The technical scheme and the technical effects obtained by the technical scheme are described in detail by taking the iron as an example which is a relatively large amount of metal material, so that the technical effects can be better understood.
1. Preparing anticorrosive slurry: in this embodiment, 525 Portland cement with a 80 μm square-hole sieve residue of not more than 10%, fine sand with a particle size of 0.25-0.0625 mm, and iron powder sieved by a 100-mesh sieve are selected as materials for preparing the anticorrosive slurry. 80ml of 525 Portland cement, 20ml of fine sand and 60ml of iron powder are mixed according to the volume ratio of 4: 1: 3, 80ml of water is measured and added, and the mixture is fully and uniformly stirred to obtain the anti-corrosion slurry.
2. Preparing an iron electrode: selecting a cylindrical iron rod with the diameter of 13mm and the length of 13cm, polishing and removing an oxide layer on the surface of the iron rod by using sand paper, spirally winding a lead with the diameter of 1 mm from the bottom of the iron rod to the top end of the iron rod, and fixing the lead at the top end to obtain the iron electrode.
3. Wrapping the anticorrosive slurry on the outer layer of the iron electrode: and (3) manufacturing a hollow cylindrical mold with the diameter of 22mm and the length of 13cm by using an acrylic plate, placing the iron electrode obtained in the step (2) at the center of the mold, uniformly pouring the anticorrosive slurry obtained in the step (1) from one side of the upper end of the mold, and transferring to the other side for pouring after one side is filled with the anticorrosive slurry until the slurry uniformly fills the whole mold.
4. Electrode interface processing: and coating a proper amount of epoxy resin on the ports of the iron electrode and the lead covered with the anti-corrosion slurry.
5. Immobilized corrosion-resistant iron electrode: and (3) flatly placing the anticorrosive iron electrode obtained in the step (3) in a tray, placing the tray in a ventilated and dried place for curing for 3d at room temperature, and slightly removing the cylinder mould after the anticorrosive iron electrode is completely cured to obtain the anticorrosive iron electrode. A schematic cross-sectional view of the corrosion-resistant iron electrode is shown in fig. 1.
6. And (3) experimental test: the experiment is carried out in a three-electrode system, 2/3 volumes of clear water are added into 2 groups of organic glass reactors with the volume of 3L, the anti-corrosion iron electrode obtained in the step 5 is placed in the middle of one group of reactors, the iron electrode obtained in the step 2 is placed in the middle of the other group of reactors, the anti-corrosion iron electrode and the iron electrode are arranged as working electrodes, the auxiliary electrode is a Pt electrode, and the reference electrode is a saturated calomel electrode. Connecting electrode wires of the working electrode, the auxiliary electrode and the reference electrode with corresponding interfaces of an electrochemical workstation CHI604E, and measuring a Tafel curve, wherein the measuring scanning speed of the Tafel curve is 10 mv/s, and the scanning range is-2.0-0.2V.
FIG. 2 is a comparative graph of Taffer curves of an anticorrosive iron electrode and a common iron electrode in the embodiment of the present invention. The cathode and anode curves of the Tafel strong polarization region of these curves were fitted in the experiment and the results are shown in Table 1. As can be seen from FIG. 2, the corrosion potential E of the corrosion-protected iron electrodecorrCompared with the iron electrode, the corrosion resistance of the coated corrosion-resistant iron electrode is negative shift, the passivation interval of the corrosion-resistant iron electrode is more obvious than that of the common iron electrode, and meanwhile, the corrosion current I of the coated corrosion-resistant iron electrode can be seen from the table 1corrThe corrosion current is lower than that of the ordinary iron electrode without being coated, which shows that the corrosion resistance of the anti-corrosion iron electrode is obviously improved compared with the ordinary iron electrode. According to the classical theory of Tafel polarization curve, it is believed that the polarization of the electrode is the accumulation of charges at the electrode interface due to the reaction speed of the electrode not being equal to the electron moving speed. Degree of electrode polarization: (
Figure DEST_PATH_IMAGE002
) The derivative of the slope of the polarization curve represents the polarization tendency of the electrode and also reflects the magnitude of the reaction resistance of the electrode. The smaller the slope of the polarization curve is, the higher the polarization degree is, the stronger the polarization tendency of the electrode is, and the faster the electron movement rate of the electrode is; meanwhile, the higher the polarization degree is, the higher the reaction resistance of the electrode is, the difficulty in the electrode reaction process is high, and the electrode reaction rate is low. From Tafel parameter in Table 1, the slope beta of the anodic polarization curve of the corrosion-resistant iron electrode can be seenaAnd the slope beta of the cathodic polarization curvecAre all lower than those of common iron electrodes. Therefore, the polarization degree of the anticorrosive iron electrode is higher than that of a common iron electrode, the polarization tendency is stronger, the electron moving speed of the electrode is higher, and the conductivity is good; meanwhile, the reaction resistance of the anti-corrosion iron electrode is relatively high, and the corrosion rate of the electrode is relatively low, which is reflected by the corrosion current I of the anti-corrosion iron electrodecorrLess consistent. Therefore, the anticorrosive iron electrode formed by wrapping the iron electrode has stronger corrosion resistance than the common iron electrode, and simultaneously, the wrapping slurry contains a large amount of iron powder to strengthen the anticorrosive iron electrodeThe electron transfer rate of the microbial electrolytic cell can effectively prolong the service life of the microbial electrolytic cell while enhancing the electron transfer capacity of the microbial electrolytic cell.
7. And (3) testing the service life: based on the electrochemical test reaction system in the step 6, the experimental group uses the corrosion-resistant iron as the anode, the cathode is the Pt electrode, the control group uses the iron without being wrapped as the anode, and the cathode is the same as the experimental group. Meanwhile, 0.6V voltage is loaded at the two ends of the cathode and the anode of the experimental group and the control group to simulate the operating environment of the microbial electrolytic cell. With the operation of the electrolytic cell, it was found that the surface of the ordinary iron electrode of the control group was gradually corroded and the aqueous solution in the reactor was gradually turned yellow, while the surface of the corrosion-resistant iron electrode of the experimental group was not changed and the aqueous solution in the reactor was not turned yellow. With the continuous operation of the electrolytic cell system, when the system is operated for 3 months, the common iron electrode of the control group is seriously corroded and hardened, the diameter of the iron rod is obviously reduced (see figure 3 a), a layer of yellow rust is accumulated at the bottom of the electrode reactor, and the corrosion-resistant iron electrode of the experimental group is not obviously corroded (see figure 3 b). Therefore, the corrosion resistance of the prepared corrosion-resistant iron electrode is obvious, and the service life of the corrosion-resistant iron electrode in a microbial electrolytic cell can be effectively prolonged.
Table 1: tafel parameter data table of anti-corrosion iron electrode and iron electrode
Ecorr(V) Icorr(A) βa βc
Common iron electrode -0.379 5.578×10-7 5.719 7.161
Corrosion-resistant iron electrode -0.844 3.635×10-7 4.969 5.406

Claims (3)

1. The utility model provides an electrode bar for microbial electrolysis cell positive pole, is the metal bar body that is used for doing microbial electrolysis cell positive pole that heliciform winding is on the surface including the electrode line, its characterized in that: the outer surface of the metal rod body is further coated with a layer of anticorrosive material, and the anticorrosive material is a cement concrete solid material doped with metal powder; the metal powder is powder of a metal material used as an anode of the microbial electrolytic cell; the anticorrosive material comprises the following components in percentage by weight: the volume ratio of the cement to the fine sand to the metal powder is 3-5: 1: 1-3; the particle size of the metal powder is smaller than that of the fine sand.
2. The electrode rod according to claim 1, wherein the metal powder has the same material properties as the metal rod body.
3. A method of making an electrode rod according to claim 1, the method comprising the steps of:
(1) mixing cement, fine sand and metal powder according to the volume ratio of 3-5: 1: 1-3 to prepare anticorrosive slurry, wherein the metal powder is powder of a metal material used as an anode of a microbial electrolytic cell;
(2) spirally winding an electrode wire on a polished metal rod to obtain an electrode body, wherein the metal rod is a rod body made of a metal material used as an anode of the microbial electrolysis cell;
(3) suspending the electrode body in an inner hollow mold with an opening at one end and an inner size larger than that of the electrode body, pouring the anti-corrosion slurry from the opening end of the mold until the electrode body is completely wrapped, and removing the mold after solidification is completed to obtain the anti-corrosion electrode rod for the anode of the microbial electrolysis cell;
(4) and resin is coated and covered on the end part of the electrode rod with the electrode wire leading-out end.
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CN110098415B (en) * 2019-05-23 2022-02-18 中国船舶重工集团公司第七二五研究所 Anode material for sediment microbial fuel cell and preparation method thereof
CN111537817A (en) * 2020-05-09 2020-08-14 南京麦澜德医疗科技有限公司 Automatic testing tool and testing method for electrode aging life

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