CN110655151A - Preparation method of titanium-based titanium suboxide porous electrode - Google Patents
Preparation method of titanium-based titanium suboxide porous electrode Download PDFInfo
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- CN110655151A CN110655151A CN201910951902.6A CN201910951902A CN110655151A CN 110655151 A CN110655151 A CN 110655151A CN 201910951902 A CN201910951902 A CN 201910951902A CN 110655151 A CN110655151 A CN 110655151A
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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
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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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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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
- C02F1/46104—Devices therefor; Their operating or servicing
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- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
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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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46152—Electrodes characterised by the shape or form
- C02F2001/46157—Perforated or foraminous electrodes
- C02F2001/46161—Porous electrodes
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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
Abstract
A preparation method of a titanium-based titanium protoxide porous electrode comprises the steps of cleaning the surface of a titanium sheet, anodizing the titanium sheet, preparing the titanium-based titanium dioxide electrode and preparing the titanium-based titanium protoxide electrode. According to the invention, the porous structure is prepared by adopting an anodic oxidation method, the contact area between the electrode and organic pollutants is increased, the effect of degrading the organic pollutants is improved, the titanium dioxide is reduced into the titanium suboxide at a lower temperature by adopting a gas phase reduction method, the stress generated in the cooling process is reduced, the surface microcracks are reduced, and the bonding strength of the titanium suboxide and the substrate is improved. The electrochemical oxidation activity of the prepared titanium-based titanium protoxide porous electrode is tested by degrading organic matters in the simulated wastewater, and the result shows that the prepared titanium-based titanium protoxide porous electrode has higher activity of electrochemically oxidizing and degrading organic matters.
Description
Technical Field
The invention relates to a preparation method of a titanium-based titanium suboxide porous electrode, belonging to the technical field of electrochemistry.
Background
The waste water containing organic pollutants is difficult to naturally degrade, the discharge of the organic waste water seriously pollutes the ecological environment, the organic pollutants are required to be degraded in the treatment of the organic waste water, and the degradation of the organic pollutants with high efficiency and low consumption is a development trend of organic waste water treatment. The electrochemical oxidation method has the advantages of high efficiency, low consumption and no secondary pollution in the aspect of treating organic wastewater, so that the electrochemical oxidation method has development prospect in the field of organic wastewater degradation.
The electrochemical oxidation method is to electrochemically oxidize and decompose organic pollutants on the surface of an anode and degrade the organic pollutants into harmless inorganic matters. The degradation effect is related to the anode material, and the anode material with good effect needs higher electrochemical activity. Titanium (Ti) suboxide4O7Has higher conductivity than graphite. Ti4O7Has higher oxygen evolution potential, which leads to higher electrochemical activity. Further, Ti4O7Has higher electrochemical stability and stronger corrosion resistance, which is beneficial to prolonging Ti4O7The service life of (2). Thus, Ti4O7Is an ideal electrochemical oxidation anode material.
In the process of degrading organic pollutants by adopting an electrochemical oxidation method, the organic pollutants are in Ti4O7The surface of the electrode is oxidized and decomposed to increase organic pollutants and Ti4O7The contact area of the electrode can improve the efficiency of degrading organic matters and promote Ti4O7The electrode has the effect of degrading organic matters. In the preparation of Ti4O7In the electrode process, due to Ti4O7High temperature reduction of TiO, different from the thermal expansion coefficient of the substrate titanium2Ti may be generated during the cooling process4O7Stress is generated on the surface, which results in Ti4O7The surface is micro-cracked, which makes Ti4O7Easy to fall off and the service life is reduced.
Disclosure of Invention
The object of the present invention is to increase Ti4O7The contact area of the electrode and the organic pollutants is increased, and Ti is improved4O7The electrode has the effect of degrading organic matters; simultaneously, the preparation of Ti by a hydrogen reduction method is reduced4O7Temperature during electrode process, reduction of Ti4O7Microcrack on the surface of the electrode, and provides a preparation method of a titanium-based titanium protoxide porous electrode.
The technical scheme of the invention is as follows: a preparation method of a titanium-based titanium suboxide porous electrode adopts an anodic oxidation method to prepare a titanium-based TiO with a porous structure from a titanium sheet2An electrode; TiO is treated at lower temperature by adopting a microwave hydrogen plasma method2Reduction to Ti4O7To obtain Ti-based Ti4O7And an electrode.
A preparation method of a titanium-based titanium protoxide porous electrode comprises the following steps:
(1) cleaning the surface of a titanium sheet, putting the titanium sheet into a metal degreasing agent, and ultrasonically cleaning for 1h at 90 ℃; then putting the titanium sheet into deionized water, ultrasonically cleaning the titanium sheet for 0.5h at 90 ℃, and then drying the titanium sheet for 6h at 60 ℃ in vacuum;
(2) anodizing the titanium sheet, namely putting the cleaned titanium sheet into electrolyte for anodizing; the cathode is a platinum electrode; the electrolyte is ethylene glycol containing ammonium fluoride and water, wherein the mass percentages of the ammonium fluoride and the water are 0.25 percent and 2 percent respectively, the anodic oxidation voltage is 50-60V, and the anodic oxidation time is 2-4 h;
(3) titanium-based TiO2Preparing an electrode, namely heating the titanium sheet after anodic oxidation at 450 ℃ for 2h in an air atmosphere to obtain titanium-based TiO2An electrode;
(4) ti-based Ti4O7Preparation of electrode by gas phase reduction of TiO2Reduction to Ti4O7To obtain Ti-based Ti4O7And an electrode.
The gas phase reduction method is a microwave hydrogen plasma reduction method.
The microwave power in the gas phase reduction method is 600-700W.
The hydrogen flow rate in the gas phase reduction method is 120-140 mL/min.
The working pressure in the gas phase reduction method is 14-16 kPa.
The treatment time in the gas-phase reduction method is 30-50 min.
To obtain Ti4O7After the porous electrode is used, organic matters in the simulated organic wastewater are degraded by using the porous electrode, and the electrochemical oxidation activity of the porous electrode is tested.
The invention has the beneficial effect that the invention adopts the microwave hydrogen plasma method to react TiO at lower temperature2Reduction to Ti4O7Lower temperature is favorable for reducing Ti4O7Internal stress of the layer, reduction of surface microcracks, and improvement of Ti4O7The bonding strength of the layers. The invention adopts an anodic oxidation method to prepare the electrode with a porous structure, and the porous structure is beneficial to increasing the contact area between the electrode and organic wastewater and improving the effect of treating the organic wastewater.
Drawings
FIG. 1 is a flow chart of the present invention for preparing a titanium-based titanium suboxide porous electrode;
FIG. 2 shows Ti prepared in example 1 of the present invention4O7Graph of porous electrode degradation of phenol.
Detailed Description
The specific embodiment of the present invention is shown in the preparation scheme of fig. 1.
Example 1
Putting the titanium sheet into a metal degreasing agent, ultrasonically cleaning the titanium sheet for 1h at 90 ℃, then putting the titanium sheet into deionized water, ultrasonically cleaning the titanium sheet for 0.5h at 90 ℃, and then drying the titanium sheet for 6h in vacuum at 60 ℃. Dissolving ammonium fluoride and water in ethylene glycol, wherein the mass percentages of the ammonium fluoride and the water are respectively 0.25% and 2%, and preparing the ethylene glycol electrolyte. And (3) putting the titanium sheet into ethylene glycol electrolyte for anodic oxidation, wherein a cathode is a platinum electrode, the anodic oxidation voltage is 55V, and the anodic oxidation time is 3 h. Heating the titanium sheet after anodic oxidation at 450 ℃ for 2h in the atmosphere of air to obtain the titanium-based TiO2And an electrode.
TiO of titanium base2Putting the electrode into a microwave plasma device, vacuumizing by using a mechanical vacuum pump, introducing hydrogen when the air pressure is reduced to 10Pa, wherein the hydrogen flow is 130mL/min, adjusting the working air pressure to 15kPa, then starting a microwave power supply, adjusting the microwave power to 650W, generating hydrogen plasma, and treating the titanium-based TiO by using the hydrogen plasma2Electrode for 40min to obtain Ti-based Ti4O7And an electrode.
Dissolving phenol and sodium sulfate in water to obtain the moldThe concentrations of the pseudo-organic wastewater, phenol and sodium sulfate were 90mg/L and 14.2g/L, respectively. The current density in electrochemical oxidation is 1.2mA/cm2And testing the chemical oxygen consumption of the simulated organic wastewater every 0.5 h.
The chemical oxygen demand corresponds to the content of organic matters in the simulated organic wastewater, the curve of the chemical oxygen demand of the simulated organic wastewater changing with time is shown in figure 2, the initial chemical oxygen demand of the simulated organic wastewater is 203mg/L, the chemical oxygen demand of the simulated organic wastewater after electrochemical oxidation for 3h is 39mg/L, the removal rate of the chemical oxygen demand is 80.8 percent, and the prepared titanium-based Ti is prepared4O7The porous electrode has high electrochemical oxidation activity.
Example 2
Putting the titanium sheet into a metal degreasing agent, ultrasonically cleaning the titanium sheet for 1h at 90 ℃, then putting the titanium sheet into deionized water, ultrasonically cleaning the titanium sheet for 0.5h at 90 ℃, and then drying the titanium sheet for 6h in vacuum at 60 ℃. Dissolving ammonium fluoride and water in ethylene glycol, wherein the mass percentages of the ammonium fluoride and the water are respectively 0.25% and 2%, and preparing the ethylene glycol electrolyte. And (3) putting the titanium sheet into ethylene glycol electrolyte for anodic oxidation, wherein a cathode is a platinum electrode, the anodic oxidation voltage is 60V, and the anodic oxidation time is 2 h. Heating the titanium sheet after anodic oxidation at 450 ℃ for 2h in the atmosphere of air to obtain the titanium-based TiO2And an electrode.
TiO of titanium base2Putting the electrode into a microwave plasma device, vacuumizing by using a mechanical vacuum pump, introducing hydrogen when the air pressure is reduced to 10Pa, wherein the hydrogen flow is 120mL/min, adjusting the working air pressure to 14kPa, then starting a microwave power supply, adjusting the microwave power to 600W, generating hydrogen plasma, and treating the titanium-based TiO by using the hydrogen plasma2Electrode for 30min to obtain Ti-based Ti4O7And an electrode.
Phenol and sodium sulfate were dissolved in water to prepare a simulated organic wastewater, the concentrations of phenol and sodium sulfate being 90mg/L and 14.2g/L, respectively. The current density in electrochemical oxidation is 1.2mA/cm2And testing the chemical oxygen consumption of the simulated organic wastewater every 0.5 h.
The test result shows that the initial chemical oxygen consumption of the simulated organic wastewater is 203mg/L, and the electrochemical reaction is carried outAfter 3 hours of chemical oxidation, the chemical oxygen consumption of the simulated organic wastewater is 44mg/L, the removal rate of the chemical oxygen consumption is 78.3 percent, and the prepared titanium-based Ti is4O7The electrochemical oxidation activity of the porous electrode is higher.
Example 3
Putting the titanium sheet into a metal degreasing agent, ultrasonically cleaning the titanium sheet for 1h at 90 ℃, then putting the titanium sheet into deionized water, ultrasonically cleaning the titanium sheet for 0.5h at 90 ℃, and then drying the titanium sheet for 6h in vacuum at 60 ℃. Dissolving ammonium fluoride and water in ethylene glycol, wherein the mass percentages of the ammonium fluoride and the water are respectively 0.25% and 2%, and preparing the ethylene glycol electrolyte. And (3) putting the titanium sheet into ethylene glycol electrolyte for anodic oxidation, wherein a cathode is a platinum electrode, the anodic oxidation voltage is 50V, and the anodic oxidation time is 4 h. Heating the titanium sheet after anodic oxidation at 450 ℃ for 2h in the atmosphere of air to obtain the titanium-based TiO2And an electrode.
TiO of titanium base2Putting the electrode into a microwave plasma device, vacuumizing by using a mechanical vacuum pump, introducing hydrogen when the air pressure is reduced to 10Pa, wherein the hydrogen flow is 140mL/min, adjusting the working air pressure to 16kPa, then starting a microwave power supply, adjusting the microwave power to 700W, generating hydrogen plasma, and treating the titanium-based TiO by using the hydrogen plasma2Electrode for 50min to obtain Ti-based Ti4O7And an electrode.
Phenol and sodium sulfate were dissolved in water to prepare a simulated organic wastewater, the concentrations of phenol and sodium sulfate being 90mg/L and 14.2g/L, respectively. The current density in electrochemical oxidation is 1.2mA/cm2And testing the chemical oxygen consumption of the simulated organic wastewater every 0.5 h.
Test results show that the initial chemical oxygen consumption of the simulated organic wastewater is 203mg/L, the chemical oxygen consumption of the simulated organic wastewater after 3 hours of electrochemical oxidation is 42mg/L, the removal rate of the chemical oxygen consumption is 79.3 percent, and the prepared titanium-based Ti is prepared4O7The electrochemical oxidation activity of the porous electrode is higher.
Claims (7)
1. The preparation method of the titanium-based titanium protoxide porous electrode is characterized in that the titanium sheet is prepared into the titanium-based TiO porous electrode with a porous structure by adopting an anodic oxidation method2An electrode; TiO is treated at lower temperature by adopting a microwave hydrogen plasma method2Reduction to Ti4O7To obtain Ti-based Ti4O7And an electrode.
2. The method for preparing a titanium-based titanium monoxide porous electrode as claimed in claim 1, wherein the method comprises the following steps:
(1) cleaning the surface of a titanium sheet, putting the titanium sheet into a metal degreasing agent, and ultrasonically cleaning for 1h at 90 ℃; then putting the titanium sheet into deionized water, ultrasonically cleaning the titanium sheet for 0.5h at 90 ℃, and then drying the titanium sheet for 6h at 60 ℃ in vacuum;
(2) anodizing the titanium sheet, namely putting the cleaned titanium sheet into electrolyte for anodizing; the cathode is a platinum electrode; the electrolyte is ethylene glycol containing ammonium fluoride and water, wherein the mass percentages of the ammonium fluoride and the water are 0.25 percent and 2 percent respectively, the anodic oxidation voltage is 50-60V, and the anodic oxidation time is 2-4 h;
(3) titanium-based TiO2Preparing an electrode, namely heating the titanium sheet after anodic oxidation at 450 ℃ for 2h in an air atmosphere to obtain titanium-based TiO2An electrode;
(4) ti-based Ti4O7Preparation of electrode by gas phase reduction of TiO2Reduction to Ti4O7To obtain Ti-based Ti4O7And an electrode.
3. The method for preparing the titanium-based titanium protoxide porous electrode according to claim 2, wherein the gas phase reduction method is a microwave hydrogen plasma reduction method.
4. The method as claimed in claim 2, wherein the microwave power in the gas phase reduction method is 600-700W.
5. The method as claimed in claim 2, wherein the hydrogen flow rate in the gas phase reduction method is 120-140 mL/min.
6. The method of claim 2, wherein the working gas pressure in the gas phase reduction method is 14 to 16 kPa.
7. The method for preparing a porous titanium-based titanium monoxide electrode as claimed in claim 2, wherein the treatment time in the gas phase reduction method is 30-50 min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111592078A (en) * | 2020-05-09 | 2020-08-28 | 哈尔滨工业大学 | Device and method for treating chlorophenol wastewater by using ultrasonic-assisted active membrane electrode |
| CN112250145A (en) * | 2020-10-30 | 2021-01-22 | 南京理工大学 | Preparation and application of porous titanium-based titanium suboxide nanotube lead dioxide electrode |
| CN112870931A (en) * | 2021-01-11 | 2021-06-01 | 深圳市普瑞美泰环保科技有限公司 | Device and method for degrading gaseous organic pollutants by electrochemical method |
| CN114180683A (en) * | 2021-12-22 | 2022-03-15 | 东莞理工学院 | To enhance TiO2Magneli phase Ti with nanotube array as interlayer4O7Electrode, its preparation and application |
| CN115947419A (en) * | 2022-06-09 | 2023-04-11 | 松山湖材料实验室 | Titanium suboxide porous ceramic coating electrode and preparation method, application and electric equipment thereof |
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