CN112062227A - Method for reducing scaling on cathode surface - Google Patents
Method for reducing scaling on cathode surface Download PDFInfo
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- CN112062227A CN112062227A CN202010795871.2A CN202010795871A CN112062227A CN 112062227 A CN112062227 A CN 112062227A CN 202010795871 A CN202010795871 A CN 202010795871A CN 112062227 A CN112062227 A CN 112062227A
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- 238000000034 method Methods 0.000 title claims abstract description 33
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- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 53
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- 239000000126 substance Substances 0.000 claims description 17
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011859 microparticle Substances 0.000 claims description 13
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- 229910021641 deionized water Inorganic materials 0.000 claims description 11
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- 238000002360 preparation method Methods 0.000 abstract description 2
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- 229910052739 hydrogen Inorganic materials 0.000 description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 12
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- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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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
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
-
- 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
- C02F1/4602—Treatment of water, waste water, or sewage by electrochemical methods for prevention or elimination of deposits
-
- 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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- 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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
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- Chemical & Material Sciences (AREA)
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention relates to a descaling method, in particular to a method for reducing scaling on the surface of a cathode, belonging to the technical fields of material preparation, environment and water treatment. The surface of the cathode material is coated with emulsion containing nano or micron organic matter particles, and a hydrophilic or hydrophobic nano particle structure layer is formed on the surface of the cathode, so that the scaling on the surface of the cathode in the electrolytic process is reduced. Exhibit superior electrode stability over conventional electrodes.
Description
Technical Field
The invention relates to a descaling method, in particular to a method for reducing scaling on the surface of a cathode, belonging to the technical fields of material preparation, environment and water treatment.
Background
In the process of production and living of human beings, a large amount of complex, stable and highly toxic degradation-resistant organic pollutants are generated, and the wastewater needs to be effectively treated, otherwise, the wastewater poses great threats to the ecological environment and human health.
The electrochemical advanced oxidation technology oxidizes water molecules to form hydroxyl free radicals (OH) with strong oxidizing property under the action of a catalyst on the surface of an anode, and the oxidation potential of the hydroxyl free radicals reaches 2.8eV, so that the hydroxyl free radicals can almost react with various refractory organic pollutants in the environment, and the electrochemical advanced oxidation technology is a high-efficiency water treatment technology. The electrochemical advanced oxidation has the advantages of mild reaction conditions, no need of adding chemicals, compact reactor structure, small occupied area, simple operation, easy expansion and the like, and is considered to have wide application prospect in the field of treating refractory organic wastewater.
In the electrochemical advanced oxidation treatment of wastewater, generally, an oxidation reaction of water occurs at the anode to generate active substances such as hydroxyl radicals, which oxidize pollutants in water and generate a hydrogen evolution reaction at the cathode. The efficiency of electrochemical advanced oxidation technology for treating wastewater is related to the performance of both the anode and the cathode. The cathode material is usually stainless steel plate or titanium plate. In the actual wastewater treatment process, calcium and magnesium ions in the wastewater can be deposited on the surface of a cathode material by carbonate and the like, so that the overpotential of cathode hydrogen evolution is increased, the treatment energy consumption is increased, and the system can not work normally in severe cases. At this point, the system needs to clean the electrode surface of deposits. At present, the methods for cleaning the deposit on the surface of the electrode mainly comprise acid washing and electrode reversal. Both of these methods, while effective in removing deposits from the electrode surface, require the processing system to be shut down and may cause secondary contamination. Therefore, reducing cathode fouling is the best option to reduce the complexity of the operating process and the operating cost.
Disclosure of Invention
The invention mainly solves the defects in the prior art and provides a method for reducing the scaling on the surface of a cathode, which seriously influences the working efficiency of an electrochemical advanced oxidation technology due to the scaling in the operation process of the cathode and needs to regularly remove the scaling.
The technical problem of the invention is mainly solved by the following technical scheme:
a method for reducing the scaling on the surface of a cathode comprises the following steps:
coating emulsion containing nano or micro organic particles on the surface of a cathode material to form a hydrophilic or hydrophobic nano particle structure layer on the surface of the cathode, so that the scale formation on the surface of the cathode in the electrolytic process is reduced;
the method is realized by the following steps:
firstly, preparing an emulsion containing 0.05-5% of nano or micro particles;
secondly, soaking the cathode sheet in 40 wt% NaOH solution at 80 ℃ for 30min, washing the cathode sheet with water, washing the surface of the cathode sheet with alcohol or acetone, coating the emulsion on the surface of the cathode, and finally drying the cathode sheet for 30min at room temperature;
and thirdly, placing the cathode sheet coated with the nano or micron particles in the step two into a heating furnace, and heating for 10-30 minutes at the temperature of 60-360 ℃ in the air atmosphere.
Preferably, in the step one: the nano or micro particle matter is one of polytetrafluoroethylene and perfluorosulfonic acid-polytetrafluoroethylene copolymer;
preparing a polytetrafluoroethylene emulsion: adding 3.3-330 mu L of 60% polytetrafluoroethylene emulsion into 96.7-100 mL of deionized water, wherein the particle size is 1 mu m-200 nm, and uniformly mixing to obtain 0.05-5% polytetrafluoroethylene emulsion by weight;
preparing perfluorosulfonic acid polytetrafluoroethylene emulsion: 1-10 mL of 5% perfluorosulfonic acid polytetrafluoroethylene emulsion is added into 90-99 mL of deionized water, the particle size is 1 mu m-200 nm, and the perfluorosulfonic acid polytetrafluoroethylene emulsion with the weight percentage of 0.05-5% is prepared after uniform mixing.
Preferably, in the step one: the particle size of the nano or micro particle matter is 1 mu m-200 nm.
Preferably, in the step one: the concentration of the nano or micro particle substances is 0.05-5% by weight percent, and the nano or micro particle substances are prepared by diluting with deionized water.
Preferably, in step two: the method for coating the emulsion on the surface of the cathode is an immersion method, the emulsion is coated on the surface of the cathode, and the time for immersing the cathode into the emulsion is 10-30 seconds.
Preferably, in the third step: the heating temperature of the cathode coated with the polytetrafluoroethylene is 340-360 ℃, and the heating temperature of the cathode coated with the perfluorosulfonic acid-polytetrafluoroethylene copolymer is 60-80 ℃.
A hydrophilic or hydrophobic layer consisting of micron and nano particles is deposited on the surface of a cathode, the micron or nano particle layer is uniformly distributed on the surface of the cathode, only part of the surface of the cathode is covered by the particles, the hydrogen evolution performance of the cathode is not influenced, but substances such as calcium carbonate and the like are prevented from forming compact and firm scales, a porous and loose layer is formed, self-desorption is easy to realize, and therefore scaling on the surface of the cathode is reduced or not required to be cleaned, and the operation stability of wastewater treatment by an advanced oxidation technology is improved.
According to the invention, a hydrophilic or hydrophobic layer consisting of micro-particles and nano-particles is deposited on the surface of the cathode, and the micro-particles or nano-particles are uniformly distributed on the surface of the cathode, so that hydrogen evolution sites on the surface of the cathode form a gas-liquid-solid three-phase reaction interface, the gas phase is favorable for hydrogen to leave the reaction interface, the liquid phase is favorable for hydrogen proton transmission, and the solid-phase cathode catalysis interface is favorable for catalytic hydrogen evolution reaction. Therefore, the hydrophilic or hydrophobic layer formed on the surface of the cathode can improve the hydrogen evolution performance of the cathode, meanwhile, hydrogen is precipitated in the cathode by micro bubbles, a pH change micro-area is formed on the surface of the cathode, and substances such as calcium carbonate and the like only form a porous loose layer on the cathode, so that the self-desorption is easy to realize, the scale formation on the surface of the cathode is reduced or not required to be cleaned, and the operation stability of the advanced oxidation technology for treating wastewater is improved.
In the present invention, the nano-or micro-particulate material is polytetrafluoroethylene and perfluorosulfonic acid-polytetrafluoroethylene copolymer. The polytetrafluoroethylene has strong hydrophobicity, and when nano or micron polytetrafluoroethylene particles are distributed on the surface of the cathode, hydrogen generated by the cathode is easily transmitted from the interface of the polytetrafluoroethylene particles and the solution. Due to the super hydrophobicity of the polytetrafluoroethylene, scale substances such as calcium carbonate and the like formed on the surface of the cathode are in a porous loose layer, and the binding force between the scale substances and the polytetrafluoroethylene is weak, so that the scale substances such as the calcium carbonate and the like easily fall off, the scale formation on the surface of the cathode is reduced or not required to be cleaned, and the wastewater treatment efficiency of the advanced oxidation technology is improved.
In the present invention, the nano-or microparticle perfluorosulfonic acid-polytetrafluoroethylene copolymer has a superhydrophobic polytetrafluoroethylene skeleton and hydrophilic sulfonic acid groups. The super hydrophobic polytetrafluoroethylene skeleton can play the same role as the super hydrophobic polytetrafluoroethylene, and the sulfonic acid group can promote the transmission of hydrogen protons. And meanwhile, scale substances such as calcium carbonate and the like formed on the surface of the cathode are in a porous loose layer, and the binding force between the scale substances and polytetrafluoroethylene is weak, so that the scale substances such as calcium carbonate and the like are easy to fall off, and the scale formation on the surface of the cathode is reduced or not required to be cleaned.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention provides a cathode surface modification method for preparing the cathode with reduced scale on the cathode surface, which is simple, green, environment-friendly and low in cost.
2) The performance of the prepared electrode can be regulated and controlled by factors such as the components, the proportion, the particle size, the heating temperature and the like of the cathode surface modification substance.
3) The modified electrode and modifier particles prepared by the method are uniformly and completely distributed on the surface, so that the cathode hydrogen evolution reaction is carried out on a gas phase, a solid phase and a liquid phase, the diffusion of gas and hydrogen protons is facilitated, and the cathode hydrogen evolution reaction is promoted to occur;
4) the electrode prepared by the method has high electrochemical activity and can provide more active sites in the electrochemical hydrogen evolution process; the hydrogen bubbles separated out on the cathode are tiny, so that the scaling substances are not easy to form massive compact scaling on the surface of the cathode.
5) The electrode prepared by the method has the advantages that the micron and nano particle layer is formed on the surface of the electrode, the combination with the scaling substances is weak, the scaling substances are in porous loose layers and are easy to fall off, and therefore the scaling on the surface of the cathode is reduced or not required to be cleaned. Exhibit superior electrode stability over conventional electrodes.
Drawings
FIG. 1 is an LSV curve of a Teflon-modified electrode in an embodiment;
FIG. 2 is the LSV curve of the perfluorosulfonic acid-polytetrafluoroethylene copolymer modified electrode in the specific example.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments and the accompanying drawings.
Example 1: polishing 20 × 0.65mm stainless steel sheet (#304) with 400-mesh and 800-mesh sandpaper in sequence, cleaning, soaking in 80 deg.C 40 wt% NaOH solution for 30min, cleaning with water, and cleaning with acetone or ethanol; preparing a polytetrafluoroethylene emulsion: adding 33 mu L of 60% polytetrafluoroethylene emulsion (with the particle size of 200nm) into 100mL of deionized water, and uniformly mixing to obtain the polytetrafluoroethylene emulsion with the weight percentage of 0.05%. And (3) putting the cleaned stainless steel sheet into 0.05% of polytetrafluoroethylene emulsion, taking out the stainless steel sheet after 30 seconds, airing the stainless steel sheet at normal temperature, and heating the stainless steel sheet in a heating furnace at 340 ℃ for 10 minutes. After the completion, the cathode was cooled to room temperature, and a cathode modified with 0.05% polytetrafluoroethylene was obtained.
Characterization of the prepared electrodes of this example:
the prepared electrode was subjected to linear polarization (LSV) curve measurement using an electrochemical workstation, the LSV curve of which is shown in fig. 1, showing that the modified cathode hydrogen evolution potential was higher than that of the untreated electrode.
Specific example 2:
polishing 20 × 0.65mm stainless steel mesh (80 mesh) with 400 mesh and 800 mesh sandpaper, cleaning, soaking in 80 deg.C 40 wt% NaOH solution for 30min, cleaning with water, and cleaning with acetone or ethanol; preparing a polytetrafluoroethylene emulsion: 330 mu L of 60 percent polytetrafluoroethylene emulsion (with the particle size of 50nm) is added into 99.5mL of deionized water and is evenly mixed to prepare the polytetrafluoroethylene emulsion with the weight percentage of 0.5 percent. And (3) putting the cleaned stainless steel sheet into 0.5% of polytetrafluoroethylene emulsion, taking out the stainless steel sheet after 20 seconds, airing the stainless steel sheet at normal temperature, and heating the stainless steel sheet in a heating furnace at 350 ℃ for 20 minutes. After the completion, the cathode was cooled to room temperature, and a cathode modified with 0.5% polytetrafluoroethylene was obtained.
Characterization of the prepared electrodes of this example:
the prepared electrode was subjected to linear polarization (LSV) curve measurement using an electrochemical workstation, the LSV curve of which is shown in fig. 1, showing that the modified cathode hydrogen evolution potential was higher than that of the untreated electrode.
Specific example 3:
polishing 20 × 0.65mm stainless steel sheet (80 mesh) with 400 mesh and 800 mesh sandpaper, cleaning, soaking in 80 deg.C 40 wt% NaOH solution for 30min, cleaning with water, and cleaning with acetone or ethanol; preparing a polytetrafluoroethylene emulsion: 3.3mL of 60% polytetrafluoroethylene emulsion (particle size 1 μm) was added to 96.7mL of deionized water and mixed well to obtain 5% weight percent polytetrafluoroethylene emulsion. And (3) putting the cleaned stainless steel sheet into 5% polytetrafluoroethylene emulsion, taking out the stainless steel sheet after 10 seconds, airing the stainless steel sheet at normal temperature, and heating the stainless steel sheet in a heating furnace at 360 ℃ for 30 minutes. And after the completion, cooling to room temperature to obtain the cathode modified by 5% of polytetrafluoroethylene.
Specific example 4:
polishing 20 × 0.65mm stainless steel sheet (80 mesh) with 400 mesh and 800 mesh sandpaper, cleaning, soaking in 80 deg.C 40 wt% NaOH solution for 30min, cleaning with water, and cleaning with acetone or ethanol; preparing perfluorosulfonic acid polytetrafluoroethylene emulsion: 1mL of 5% perfluorosulfonic acid polytetrafluoroethylene emulsion (with the particle size of 200nm) is added into 99mL of deionized water, and the perfluorosulfonic acid polytetrafluoroethylene emulsion with the weight percentage of 0.05% is prepared after uniform mixing. And (3) putting the cleaned stainless steel sheet into 0.05% perfluorosulfonic acid polytetrafluoroethylene emulsion, taking out the stainless steel sheet after 10 seconds, drying the stainless steel sheet at normal temperature, and heating the stainless steel sheet in a heating furnace at 60 ℃ for 30 minutes. After the completion, the cathode is cooled to room temperature, and the cathode modified by 0.05 percent of perfluorosulfonic acid polytetrafluoroethylene is obtained.
Characterization of the prepared electrodes of this example:
the electrode prepared was subjected to linear polarization (LSV) curve measurements using an electrochemical workstation, the LSV curve of which is shown in fig. 2, showing that the modified cathode hydrogen evolution potential was higher than the untreated electrode.
Specific example 5:
polishing 20 × 0.65mm stainless steel sheet (80 mesh) with 400 mesh and 800 mesh sandpaper, cleaning, soaking in 80 deg.C 40 wt% NaOH solution for 30min, cleaning with water, and cleaning with acetone or ethanol; preparing perfluorosulfonic acid polytetrafluoroethylene emulsion: 10mL of 5% perfluorosulfonic acid polytetrafluoroethylene emulsion (with the particle size of 200nm) is added into 90mL of deionized water, and the mixture is uniformly mixed to prepare the perfluorosulfonic acid polytetrafluoroethylene emulsion with the weight percentage of 0.5%. And (3) putting the cleaned stainless steel sheet into 0.5% perfluorosulfonic acid polytetrafluoroethylene emulsion, taking out the stainless steel sheet after 20 seconds, drying the stainless steel sheet at normal temperature, and heating the stainless steel sheet in a heating furnace at 70 ℃ for 20 minutes. After the completion, the cathode is cooled to room temperature, and the cathode modified by 0.5% perfluorosulfonic acid polytetrafluoroethylene is obtained.
Characterization of the prepared electrodes of this example:
the electrode prepared was subjected to linear polarization (LSV) curve measurements using an electrochemical workstation, the LSV curve of which is shown in fig. 2, showing that the modified cathode hydrogen evolution potential was higher than the untreated electrode.
Specific example 6:
polishing 20 × 0.65mm stainless steel sheet (80 mesh) with 400 mesh and 800 mesh sandpaper, cleaning, soaking in 80 deg.C 40 wt% NaOH solution for 30min, cleaning with water, and cleaning with acetone or ethanol; preparing perfluorosulfonic acid polytetrafluoroethylene emulsion: 10mL of a 5% perfluorosulfonic acid polytetrafluoroethylene emulsion (particle size 1 μm) was taken. And (3) putting the cleaned stainless steel sheet into 5% perfluorosulfonic acid polytetrafluoroethylene emulsion, taking out the stainless steel sheet after 30 seconds, airing the stainless steel sheet at normal temperature, and heating the stainless steel sheet in a heating furnace at the temperature of 80 ℃ for 30 minutes. And after the reaction is finished, cooling to room temperature to obtain the cathode modified by 5% perfluorosulfonic acid polytetrafluoroethylene.
Claims (6)
1. A method for reducing scaling on the surface of a cathode, comprising the steps of:
coating emulsion containing nano or micro organic particles on the surface of a cathode material to form a hydrophilic or hydrophobic nano particle structure layer on the surface of the cathode, so that the scale formation on the surface of the cathode in the electrolytic process is reduced;
the method is realized by the following steps:
firstly, preparing an emulsion containing 0.05-5% of nano or micro particles;
secondly, soaking the cathode sheet in 40 wt% NaOH solution at 80 ℃ for 30min, washing the cathode sheet with water, washing the surface of the cathode sheet with alcohol or acetone, coating the emulsion on the surface of the cathode, and finally drying the cathode sheet for 30min at room temperature;
and thirdly, placing the cathode sheet coated with the nano or micron particles in the step two into a heating furnace, and heating for 10-30 minutes at the temperature of 60-360 ℃ in the air atmosphere.
2. A method of reducing cathode surface fouling according to claim 1, wherein: in the first step: the nano or micro particle matter is one of polytetrafluoroethylene and perfluorosulfonic acid-polytetrafluoroethylene copolymer;
preparing a polytetrafluoroethylene emulsion: adding 3.3-330 mu L of 60% polytetrafluoroethylene emulsion into 96.7-100 mL of deionized water, wherein the particle size is 1 mu m-200 nm, and uniformly mixing to obtain 0.05-5% polytetrafluoroethylene emulsion by weight;
preparing perfluorosulfonic acid polytetrafluoroethylene emulsion: 1-10 mL of 5% perfluorosulfonic acid polytetrafluoroethylene emulsion is added into 90-99 mL of deionized water, the particle size is 1 mu m-200 nm, and the perfluorosulfonic acid polytetrafluoroethylene emulsion with the weight percentage of 0.05-5% is prepared after uniform mixing.
3. A method of reducing cathode surface fouling according to claim 2, wherein: in the first step: the particle size of the nano or micro particle matter is 1 mu m-200 nm.
4. A method of reducing cathode surface fouling according to claim 3, wherein: in the first step: the concentration of the nano or micro particle substances is 0.05-5% by weight percent, and the nano or micro particle substances are prepared by diluting with deionized water.
5. A method of reducing cathode surface fouling according to claim 3, wherein: in the second step: the method for coating the emulsion on the surface of the cathode is an immersion method, the emulsion is coated on the surface of the cathode, and the time for immersing the cathode into the emulsion is 10-30 seconds.
6. A method of reducing cathode surface fouling according to claim 3, wherein: in the third step: the heating temperature of the cathode coated with the polytetrafluoroethylene is 340-360 ℃, and the heating temperature of the cathode coated with the perfluorosulfonic acid-polytetrafluoroethylene copolymer is 60-80 ℃.
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