CN114853125A - Preparation method of carbon-based adsorption electrode and three-electrode electric flocculation system - Google Patents
Preparation method of carbon-based adsorption electrode and three-electrode electric flocculation system Download PDFInfo
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- CN114853125A CN114853125A CN202210459828.8A CN202210459828A CN114853125A CN 114853125 A CN114853125 A CN 114853125A CN 202210459828 A CN202210459828 A CN 202210459828A CN 114853125 A CN114853125 A CN 114853125A
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/463—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrocoagulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
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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
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The application provides a preparation method of a carbon-based adsorption electrode and a three-electrode electric flocculation system, wherein the preparation method of the carbon-based adsorption electrode comprises the following steps: taking waste biomass powder, adding a pore-forming agent and water, uniformly mixing, and kneading until a bulk material is formed; placing the bulk material into an oven to be dried at a preset temperature, taking out the bulk material to continue kneading and exhausting, and cutting the kneaded and exhausted bulk material to obtain a carbon-based precursor; and placing the carbon-based precursor into a vacuum tube furnace, heating to 900 ℃ at a preset heating rate, and then preserving heat for 2h to obtain the carbon-based adsorption electrode. The carbon-based adsorption electrode prepared by the method has excellent conductivity and good adsorption capacity, can be used for rapidly treating water body pollution by being applied to a three-electrode electric flocculation system, has extremely strong adsorption capacity on particles in the polluted water body, does not cause secondary pollution, and is simple in manufacturing process and low in manufacturing cost, so that the carbon-based adsorption electrode is more suitable for an electric flocculation process.
Description
Technical Field
The application relates to the technical field of electrochemistry, in particular to a preparation method of a carbon-based adsorption electrode and a three-electrode electric flocculation system.
Background
In recent years, environmental problems have become more serious with the development of industry and agriculture. The excessive discharge of phosphorus in the sewage leads to water eutrophication, and meanwhile, the phosphorus is a non-renewable resource, so that the effective phosphorus recovery is realized and the concept of sustainable development is met, and therefore, the exploration of a technology for efficiently capturing and recovering the phosphorus in the sewage is imperative.
The current phosphorus removal means mainly comprise: adsorption, chemical precipitation and biological methods. The adsorption method is characterized in that some materials with large specific surface area and high porosity are used for removing phosphorus, so that the cost is high, and the phosphorus removal efficiency is low; the chemical precipitation method is characterized in that phosphorus is removed by adding a chemical reagent to precipitate the phosphate, the chemical phosphorus removal effect is influenced by various factors such as the type of the chemical reagent, the adding amount, the temperature, the sludge concentration and the like, and the method has certain limitation and complexity on phosphorus removal; the biological method is characterized in that bacteria are used for inducing and exciting cells to accumulate phosphorus polymerized in the cells and release phosphate radicals and bond energy under the alternate anaerobic and aerobic conditions, and then the phosphorus content in sewage is reduced through a series of conversions.
Compared with the traditional chemical method, biological method and adsorption method, the electric flocculation technology has the advantages of chemical coagulation and electrochemical method, and has simple and convenient operation, high pollutant removal rate and no need of adding extra chemical substances. The electric flocculation technology mainly utilizes the interaction of electrodes and electric energy to treat the wastewater. The electrode is the core part of the electrochemical treatment equipment, and the electrode material and the structural form play an important role in the performance of the electrochemical treatment equipment.
However, the electrodes commonly used in the electrocoagulation technology are often produced from nanomaterials such as activated carbon, carbon nanotubes, graphene and graphene composites, which often cause problems such as high cost and serious secondary pollution, and in addition, due to the high power consumption required by the electrocoagulation technology, the electrodes become an important reason for limiting the widespread use and popularization of the technology.
Disclosure of Invention
The application provides a preparation method of a carbon-based adsorption electrode and a three-electrode electric flocculation system, which can solve the problems that the electrode used in the existing electric flocculation technology has high cost and causes secondary pollution and the existing electric flocculation technology requires high electric energy consumption.
The first technical scheme of the application is a preparation method of a carbon-based adsorption electrode, which is used for preparing an electrode with ion migration capacity and adsorption function and comprises the following steps:
taking waste biomass powder, adding a pore-forming agent and water, uniformly mixing, and kneading until a bulk material is formed;
placing the dough-like material into an oven to be dried at a preset temperature, taking out the dough-like material to continue kneading and exhausting, and cutting the kneaded and exhausted dough-like material to obtain a carbon-based precursor;
and placing the carbon-based precursor into a vacuum tube furnace, heating to 900 ℃ at a preset heating rate, and then preserving heat for 2 hours to obtain the carbon-based adsorption electrode.
Optionally, the waste biomass powder is waste wheat flour or waste corn flour;
and the pore-forming agent can be yeast powder, baking soda, magnesium carbonate or calcium carbonate.
Optionally, the preset temperature is 30-40 ℃.
Optionally, the preset heating rate is 5-10 ℃/min.
A second technical aspect of the present application is a three-electrode electric flocculation system, comprising:
the reactor is formed by connecting a plurality of first insulating plate-shaped materials in a surrounding manner through second insulating plate-shaped materials, three electrode tanks arranged in the reactor, and a carbon-based adsorption electrode, a sacrificial anode and an inert metal plate which are all plate-shaped and are sequentially arranged in the three electrode tanks respectively.
Alternatively, the first insulating plate-like material may be a flat plate made of polymethyl methacrylate;
and the second insulating rod-shaped material may be a screw made of polytetrafluoroethylene.
Optionally, the sacrificial anode is mesh-shaped.
Optionally, a precipitation zone is provided at the sacrificial anode.
Optionally, the distance between the sacrificial anode and the inert metal plate is 1.5-3.5 cm.
Optionally, the electrode tank used in cooperation with the sacrificial anode is provided with an insertion groove for inserting and extracting the sacrificial anode;
when the sacrificial anode is inserted into the insertion groove, the electrode distance between the sacrificial anode and the carbon-based adsorption electrode is 0.5 cm.
To sum up, this application provides a preparation method of carbon base adsorption electrode at first for prepare the electrode that possesses ion mobility and adsorption function, compare in prior art, the carbon base adsorption electrode that this application was made has following advantage:
(1) the adsorption effect is achieved, the ion migration capacity is achieved through the change of the anode and the cathode, the electric flocculation process is more suitable for being used in the electric flocculation process, and the water body pollution can be rapidly treated;
(2) the conductive coating has excellent conductivity and good adsorption capacity, has extremely strong adsorption capacity on particles in a polluted water body, and cannot cause secondary pollution;
(3) the composite material has a unique three-dimensional structure, large particle aperture, large specific surface area, uniform distribution and stable structure, and has the characteristics of high total capacitance, large physical strength, large improvement space, strong bonding capability and long service life;
(4) the preparation process of the carbon-based adsorption electrode can use the binder, the conductive additive and the current collector according to actual needs, the preparation process is simple, and the cost for treating water pollution can be obviously reduced.
The application also provides a three-electrode electric flocculation system, compares in prior art, and the three-electrode electric flocculation system of this application has following advantage:
(5) the reactor is formed by enclosing a first insulating plate-shaped material such as a plate-shaped material of high-density polymer such as polymethyl methacrylate and connecting a second insulating rod-shaped material such as a polytetrafluoroethylene screw, so that unnecessary power consumption and potential safety hazard caused by using a metal connecting material are avoided;
(6) the modular stackable structure and the design of the plug-in electrode tank can meet the replacement requirement of the electrode and avoid the excessive consumption of the sacrificial anode material;
(7) the arrangement of the sedimentation area is convenient for discharging flocculent sediments generated in the electrocoagulation process in time in the past and simultaneously reducing the negative influence on the treatment efficiency of the electrocoagulation process;
(8) through the design of configuration, the regulation and control of operating parameters and the selection of electrode materials, the treatment time is greatly shortened, the treatment efficiency is improved, and the target ions in the low-concentration phosphate sewage are recovered with lower electric energy consumption, electrode material loss and higher treatment efficiency.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without any creative effort.
FIG. 1 is a schematic flow chart of a method for preparing a carbon-based adsorption electrode according to an embodiment of the present disclosure;
FIG. 2 is a mass flow diagram of a method of making a carbon-based adsorption electrode according to an embodiment of the present disclosure;
FIG. 3 is a schematic structural diagram of a three-electrode electric flocculation system in an embodiment of the present application;
FIG. 4 is a schematic diagram of a three-electrode electric flocculation system in an embodiment of the present application;
wherein, 1-electrode groove; 11-a rubber gasket; 2-carbon-based adsorption electrodes; 3-a sacrificial anode; 4-inert metal plate; 5-a precipitation zone.
Detailed Description
Reference will now be made in detail to embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following examples do not represent all embodiments consistent with the present application. But merely as exemplifications of systems and methods consistent with certain aspects of the application, as recited in the claims.
In a first aspect, the present application provides a method for preparing a carbon-based adsorption electrode, which is used for preparing an electrode having an ion migration adsorption function, as shown in fig. 1 and fig. 2, fig. 1 is a schematic flow diagram of a method for preparing a carbon-based adsorption electrode in an embodiment of the present application, fig. 2 is a material flow diagram of a method for preparing a carbon-based adsorption electrode in an embodiment of the present application, four diagrams from left to right in fig. 2 are respectively a waste biomass powder, a carbon-based precursor, a vacuum tube furnace, and a carbon-based adsorption electrode 2, and the method for preparing a carbon-based adsorption electrode 2 includes the following steps:
s1: taking waste biomass powder, adding a pore-forming agent and water, uniformly mixing, and kneading to form a dough-shaped material.
Specifically, the waste biomass powder can be waste wheat flour or waste corn flour, and the pore-forming agent can be yeast powder, baking soda, magnesium carbonate or calcium carbonate. In some embodiments, the waste biomass powder used is waste wheat flour with a mass of 400g, the pore former used is yeast powder with a mass of 4g, and the volume of water used is 250 mL.
S2: and placing the dough material into an oven to be dried at a preset temperature, taking out the dough material, continuously kneading and exhausting air, and cutting the kneaded and exhausted dough material to obtain the carbon-based precursor.
Specifically, the preset temperature may be 30-40 ℃.
S3: and placing the carbon-based precursor into a vacuum tube furnace, heating to 900 ℃ at a preset heating rate, and then preserving heat for 2 hours to obtain the carbon-based adsorption electrode 2.
Specifically, the preset temperature rise rate is 5-10 ℃/min and temperature rise can be started from room temperature.
In conclusion, the carbon-based adsorption electrode 2 prepared by the embodiment of the application has a unique three-dimensional structure, has ion migration and adsorption functions, has excellent conductivity, has a large specific surface area, and can be 700-1000m 2 The distribution is more uniform and the structure is more stable, and the capacitor has the characteristics of high total capacitance, high physical strength, large improvement space, strong bonding capability and long service life.
In practical application, the anode is connected with the inert metal plate in a three-electrode electrocoagulation system, and the cathode is connected with the carbon-based adsorption electrode 2 to enter a migration adsorption stage; then the negative electrode and the carbon-based adsorption electrode 2 are disconnected and connected to the inert metal plate 4, and the positive electrode and the sacrificial anode 3 are connected to enter an electric flocculation stage. By combining the target ions adsorbed in the migration and adsorption stage with the metal ions released by the sacrificial anode 3, the utilization efficiency of the sacrificial anode 3 material is improved, and the material and power consumption is reduced.
The preparation process of the carbon-based adsorption electrode 2 can use the binder, the conductive additive and the current collector according to actual needs, the preparation process is simple, and the cost for treating water pollution can be obviously reduced. The prepared electrode can rapidly treat water body pollution, has strong adsorption capacity to particles in the polluted water body, and cannot cause secondary pollution, so the electrode is more suitable for an electric flocculation process.
In a second aspect, the present application further provides a three-electrode electrocoagulation system for solving the problem that phosphorus in low-concentration phosphate sewage is difficult to remove, as shown in fig. 3, fig. 3 is a schematic structural diagram of the three-electrode electrocoagulation system in an embodiment of the present application, a schematic connection diagram of a plurality of electrode tanks 1 and a carbon-based adsorption electrode 2, a sacrificial anode 3 and an inert metal plate 4 is shown on the left side in fig. 3, a schematic connection diagram of the sacrificial anode 3 and a rubber gasket 11 is shown on the right side in fig. 3, and the system includes: the reactor comprises a reactor and at least three electrode tanks 1 arranged in the reactor, wherein the reactor is formed by enclosing a plurality of plate-shaped materials of first insulating plate-shaped materials such as polymethyl methacrylate and connecting the plate-shaped materials through second insulating rod-shaped materials such as polytetrafluoroethylene screws, and a carbon-based adsorption electrode 2, a sacrificial anode 3 and an inert metal plate 4 which are all plate-shaped and are respectively arranged in the three electrode tanks 1 in sequence are arranged.
Specifically, the reactor is surrounded by a first insulating plate-shaped material such as a plate-shaped material of high-density polymer such as polymethyl methacrylate and is formed by a second insulating rod-shaped material such as a connecting material of polytetrafluoroethylene screw, so that unnecessary power consumption and potential safety hazard caused by the use of a metal connecting material are avoided; the electrode tank 1 is provided with rubber gaskets 11 at the joints with the carbon-based adsorption electrode 2, the sacrificial anode 3 and the inert metal plate 4 respectively. In some embodiments, the sacrificial anode 3 is mesh-shaped.
In some embodiments, the polymethylmethacrylate plates surrounding the synthesis reactor are provided in dimensions of 0.5cm by 5cm by 8 cm. The polymethyl methacrylate plate of the electrode cell 1 used in cooperation with the sacrificial anode 3 was set to a size of 0.5cm × 3cm × 6 cm. And the size of the polymethyl methacrylate plate of the electrode tank 1 used in cooperation with the inert metal plate 4 is 0.1cm × 3cm × 7 cm.
The electrode bath 1 provided with the sacrificial anodes 3 is a sacrificial anode 3 insertion groove and is opened with an insertion groove into which the sacrificial anodes 3 are inserted and withdrawn, and a precipitation zone 5 is formed at the bottom ends of the sacrificial anodes 3 in a state where the sacrificial anodes 3 are inserted into the insertion groove. And the distance between the sacrificial anode 3 and the inert metal plate is 1.5-3.5cm, and the distance between the sacrificial anode 3 and the carbon-based adsorption electrode 2 is 0.5 cm. The proper electrode spacing is more beneficial to the transmission of electrons, the processing efficiency is improved, and the energy consumption is reduced.
Specifically, the sacrificial anode 3 is provided in an insertable and extractable form for the purpose of facilitating replacement of the sacrificial anode 3. The provision of the settling zone 5 avoids the problem of excessive consumption of the sacrificial anode 3 material.
The working principle is as follows: as shown in fig. 4, fig. 4 is a working schematic diagram of a three-electrode electrocoagulation system in the embodiment of the present application, and is different from a treatment mechanism of a conventional electrocoagulation technology, in the embodiment of the present application, a carbon-based adsorption electrode 2 and an inert metal plate 4 are connected by using a potentiostat, respectively, a cathode of the potentiostat is connected with the carbon-based adsorption electrode 2, an anode of the potentiostat is connected with the inert metal plate 4, at this time, anions in a solution will directionally move to the carbon-based adsorption electrode 2, and the carbon-based adsorption electrode 2 will enrich the anions.
Then, a lead connected with the carbon-based adsorption electrode 2 is disconnected and connected to the inert metal plate 4, the anode is connected to the sacrificial anode 3, iron ions are separated out from the sacrificial anode 3, and the separated iron ions are combined with anions enriched and released from the carbon-based adsorption electrode 2 to form precipitates, so that the precipitates enter an electrocoagulation working mode. The direction of an electric field is reversed by changing the connection of the anode and the cathode, the moving direction of target ions in a liquid phase is adjusted, charged ions are adsorbed on the carbon-based adsorption electrode 2 while generating a concentration gradient difference in a local liquid phase, the target ions are enriched near the sacrificial anode 3 as much as possible by adjusting the electrode spacing, the cathode of the potentiostat is connected with the inert metal plate 4 after entering an electric flocculation working mode, the anode of the potentiostat is connected with the sacrificial anode 3, and the carbon-based adsorption electrode 2 is combined with metal ions released by the sacrificial anode 3 while desorbing the target ions and forms flocculation precipitation near the sacrificial anode 3.
Experiments prove that the carbon-based adsorption electrode 2 prepared by the method has the characteristics of good electrical conductivity, high total capacitance and large specific surface area, wherein the specific surface area can be 700-1000m 2 (ii)/g, and has ion transfer and adsorption capabilities; the embodiments of the present application provideThe three-electrode electric flocculation system has the capability of efficiently recovering low-concentration phosphorus in sewage, and simultaneously, the required electric energy and material consumption are less. In 1-2.5mg/L phosphate solution, the lowest phosphate effluent concentration after a total treatment time of 200s (including a 100s migration adsorption stage and a 100s electroflocculation stage) can reach ≦
0.12 +/-0.03 mg/L, the removal rate can reach 90 percent, but the required energy consumption is only 0.004-0.006kWh/m 3 Compared with the traditional electric flocculation technology, the electric energy consumption can be reduced by 30-40%, and in addition, after the phosphorus-containing sewage is treated, a large amount of phosphorus flocculation sediment can be formed at the bottom of the reactor, so that the phosphorus-containing sewage is convenient to recycle.
In summary, the carbon-based adsorption electrode 2 material provided by the embodiment of the present application has the characteristics of simple preparation method, large specific surface area, good conductivity, large physical strength, large improvement space, strong binding capacity, long service life, and the like, and has ion migration and adsorption capacities. The three-electrode electric flocculation system provided by the embodiment of the application greatly shortens the treatment time of low-concentration phosphate recovery, improves the treatment efficiency, obtains high-efficiency recovery of phosphorus elements in low-concentration phosphorus-containing sewage with lower electric energy consumption and material loss through the design of system configuration, the regulation and control of operating parameters and the selection of electrode materials, and effectively solves the problem of phosphorus resource shortage.
The embodiments of the present application have been described in detail, but the present application is only a preferred embodiment of the present application and should not be construed as limiting the scope of the present application. All equivalent changes and modifications made within the scope of the present application shall fall within the scope of the present application.
Claims (10)
1. A preparation method of a carbon-based adsorption electrode is used for preparing an electrode with ion migration capacity and adsorption function, and is characterized by comprising the following steps:
taking waste biomass powder, adding a pore-forming agent and water, uniformly mixing, and kneading until a bulk material is formed;
placing the dough-like material into an oven to be dried at a preset temperature, taking out the dough-like material to continue kneading and exhausting, and cutting the kneaded and exhausted dough-like material to obtain a carbon-based precursor;
and placing the carbon-based precursor into a vacuum tube furnace, heating to 900 ℃ at a preset heating rate, and then preserving heat for 2 hours to obtain the carbon-based adsorption electrode.
2. The preparation method of the carbon-based adsorption electrode according to claim 1, wherein the waste biomass powder is waste wheat flour or waste corn flour;
and the pore-forming agent can be yeast powder, baking soda, magnesium carbonate or calcium carbonate.
3. The method according to claim 1, wherein the predetermined temperature is 30-40 ℃.
4. The method according to claim 1, wherein the predetermined temperature rise rate is 5-10 ℃/min.
5. A three-electrode electrocoagulation system, comprising:
the reactor is formed by connecting a plurality of first insulating plate-shaped materials in a surrounding manner through second insulating plate-shaped materials, three electrode tanks arranged in the reactor, and a carbon-based adsorption electrode, a sacrificial anode and an inert metal plate which are all plate-shaped and are sequentially arranged in the three electrode tanks respectively.
6. A three-electrode electroflocculation system as claimed in claim 5, wherein the first insulating sheet material is a flat sheet made of polymethylmethacrylate;
and the second insulating rod-shaped material may be a screw made of polytetrafluoroethylene.
7. A three-electrode electroflocculation system as claimed in claim 5, wherein the sacrificial anode is mesh-shaped.
8. A three-electrode electroflocculation system as claimed in claim 5, wherein a settling zone is provided at the sacrificial anode.
9. A three-electrode electroflocculation system as claimed in claim 5, wherein the distance between the sacrificial anode and the inert metal plate is 1.5-3.5 cm.
10. The system of claim 5, wherein the electrode tank used in cooperation with the sacrificial anode is provided with an insertion groove for insertion and extraction of the sacrificial anode; when the sacrificial anode is inserted into the insertion groove, the electrode distance between the sacrificial anode and the carbon-based adsorption electrode is 0.5 cm.
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