CN114105258A - Manufacturing method of electrode for electrocatalytic degradation of pyridine, product and application thereof - Google Patents
Manufacturing method of electrode for electrocatalytic degradation of pyridine, product and application thereof Download PDFInfo
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- CN114105258A CN114105258A CN202111363521.XA CN202111363521A CN114105258A CN 114105258 A CN114105258 A CN 114105258A CN 202111363521 A CN202111363521 A CN 202111363521A CN 114105258 A CN114105258 A CN 114105258A
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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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- 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
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Abstract
The invention discloses a manufacturing method of a high-stability electrode for electrocatalytic degradation of pyridine, and a product and application thereof, wherein the manufacturing method comprises the steps of preparing a precursor solution containing antimony Sb and tin Sn; preparing Sb-SnO antimony-doped tin dioxide on the surface of a titanium sheet by using the titanium sheet as a substrate and utilizing a thermal decomposition method2Obtaining Ti/Sb-SnO as an electrode material2An electrode; by a constant current method, using Ti/Sb-SnO2A working electrode, a Pt sheet as a counter electrode, and nickel nitrate Ni (NO)3)2The solution is electrolyte solution, and electrochemical deposition is carried out to obtain Ti/Sb-SnO modified by nickel2And an electrode. The electrode obtained by the method takes a titanium sheet as a substrate and Sb-SnO2NiO or Ni (OH)2The composite material is an electrode material and shows higher activity and stability of electrochemical degradation of pyridine.
Description
Technical Field
The invention belongs to the technical field of catalytic environment protection, and particularly relates to a manufacturing method of an electrode for degrading pyridine through electrocatalysis, and a product and application thereof.
Background
High concentrations of organic and harmful pollutants emitted in industrial production pose great harm to human health and the environment. In particular, nitrogen-containing heterocyclic compounds are difficult to degrade and have inhibitory or toxic effects on biochemical reactions. Pyridine, a typical nitrogen-containing heterocyclic compound, is harmful to human health and ecological environment due to its high toxicity and teratogenicity, and it is difficult to treat such waste water by conventional methods due to its recalcitrance. Therefore, the development of a rapid and efficient pyridine degradation method is urgently needed. The electrochemical oxidation has the advantages of mild reaction conditions, environmental friendliness, strong oxidation capacity and the like, and is a hotspot of current research. Electrochemical oxidation is therefore considered a promising wastewater treatment technology and has attracted considerable attention in water treatment research.
The Ti/SnO2-Sb electrode has high oxygen evolution potential and electrocatalytic activity, so that the Ti/SnO2-Sb electrode is widely researched in the field of electrochemical catalysis, but the Ti/SnO2-Sb electrode has the problems of easy peeling of a coating, short service life and the like, and practical application is limited. The construction of the protective layer can improve the stability of the electrode on one hand, thereby achieving the purpose of prolonging the service life of the electrode, and on the other hand, the proper protective layer can effectively improve the electron transmission rate of the electrode, promote the surface diffusion of ions, and thereby effectively improve the catalytic oxidation capability of the electrode.
Disclosure of Invention
In order to realize the efficient removal of pyridine, the invention aims to provide a manufacturing method of an electrode for electrocatalytic degradation of pyridine.
Yet another object of the present invention is to: provides an electrode product for electrocatalytic degradation of pyridine prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a method for manufacturing an electrode for electrochemically degrading pyridine, wherein the electrode is a nickel-modified antimony-doped tin dioxide/titanium sheet electrode, and comprises the following manufacturing steps:
(1) preparing a precursor solution containing antimony Sb and tin Sn: respectively preparing SnCl with the concentration of 1mol/L4˙5H2O n-Butanol solution, 1mol/L SbCl3N-butyl alcohol solution, according to the doping proportion of antimony of 5% -10%, taking two solutions, and carrying out ultrasonic treatment for 5min is mixed evenly to obtain mixed solution;
(2) uniformly coating the mixed solution obtained in the step (1) on a titanium sheet, and standing at room temperature for 1 h;
(3) taking a titanium sheet as a substrate, placing the titanium sheet obtained in the step (2) in a muffle furnace, and preparing antimony-doped tin dioxide Sb-SnO on the surface of the titanium sheet by adopting a thermal decomposition method2The catalyst is used for obtaining the antimony doped stannic oxide/titanium sheet electrode Ti/Sb-SnO2;
(4) With Ti/Sb-SnO2A working electrode, a Pt sheet as a counter electrode, and nickel nitrate (Ni (NO)3)2) And performing electrochemical deposition by adopting a constant current method to obtain the nickel-modified antimony-doped tin dioxide/titanium plate electrode.
On the basis of the scheme, in the step (2), the titanium sheet is a titanium sheet with the thickness of 0.1-0.2 mm and the size of 2 x 3 cm, and the titanium sheet is pretreated, and the method comprises the following steps:
1) soaking the titanium sheet in 40% sodium hydroxide solution, and keeping the temperature at 80 ℃ for 1 h;
2) soaking the titanium sheet obtained in the step 1) in 6M HCl solution, and reacting for 2h at 90 ℃;
3) washing the titanium sheet obtained in the step 2) with deionized water for several times, and finally soaking in absolute ethyl alcohol for later use.
In the step (3), the titanium sheet is placed in a muffle furnace, roasted for 2 hours at the heating rate of 3 ℃/min to 550 ℃, and finally naturally cooled to room temperature to obtain Ti/Sb-SnO2And an electrode.
In the step (4), the concentration of the nickel nitrate solution is 0.1-0.5 mol/L, the constant current is-1 to-5 mA, and the electrodeposition time is 0.5-1 h.
Further, 200. mu.l of the mixed solution obtained in the step (1) was uniformly coated on the pretreated titanium plate and left at room temperature for 1 hour.
The invention also provides an electrode for electrochemically degrading pyridine, which is manufactured according to any one of the methods and specifically comprises the following steps: a titanium sheet substrate; the titanium sheet substrate is covered with an antimony-doped tin dioxide catalyst; and a nickel hydroxide or nickel oxide protective layer is deposited on the surface of the antimony-doped tin dioxide catalyst, namely the nickel-modified antimony-doped tin dioxide/titanium plate electrode.
The invention also provides an application of the electrode for electrochemically degrading pyridine as an electrode in electrocatalytic degradation of pyridine at normal temperature.
The invention provides a method for manufacturing a high-stability electrode for electrocatalytic degradation of pyridine. The electrode takes a titanium sheet as a substrate and Sb-SnO as well as Sb-SnO2NiO or Ni (OH)2The composite material is an electrode material and shows higher activity and stability of electrochemical degradation of pyridine. On the one hand, NiO or Ni (OH) is added due to the fact that the nickel-based material has stronger electron transport capacity2And Sb-SnO2The electrode is compounded, so that the Sb-SnO is effectively improved2Charge transfer capability of the surface. On the other hand, a nickel-based material is adhered to Sb-SnO as a protective layer2The surface of (2) effectively improves the stability of the electrode.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
An electrode for electrochemically degrading pyridine is a nickel-modified antimony-doped tin dioxide/titanium sheet electrode and is manufactured according to the following steps:
(1) pretreating a titanium sheet: soaking a titanium sheet with the thickness of 0.1mm and the size of 2 multiplied by 3 cm in a 40 percent sodium hydroxide solution, and keeping the temperature at 80 ℃ for 1 h; then soaking the mixture in 6M HCl, and reacting for 2 hours at 90 ℃; taking out, washing with deionized water for several times, and soaking in absolute ethyl alcohol to obtain a pretreated titanium sheet for later use;
(2) preparing a precursor solution containing antimony Sb and tin Sn: weighing SnCl4˙5H2O1.75 g is dissolved in 5ml of n-butanol solution as a tin-containing precursor solution; weighing SbCl31.15g of this was dissolved in 5ml of n-butanol solution as a solution containingTaking 900 mu l of tin-containing precursor solution and 100 mu l of antimony-containing precursor solution according to the doping proportion of antimony, and carrying out ultrasonic 5 min to uniformly mix to obtain a mixed solution;
(3) uniformly coating 200 mu l of the mixed solution obtained in the step (2) on a pre-sheet titanium sheet, and standing at room temperature for 1 h; then, the user can use the device to perform the operation,
(4) placing the titanium sheet obtained in the step (3) in a muffle furnace, controlling the heating rate to be 3 ℃/min, roasting at 550 ℃ for 2h, and finally naturally cooling to room temperature to obtain the antimony-doped tin dioxide/titanium sheet electrode Ti/Sb-SnO2;
(5) With Ti/Sb-SnO2As a working electrode, a Pt sheet as a counter electrode, and 50ml of 0.1M nickel nitrate (Ni (NO)3)2) And performing electrochemical deposition by adopting a constant current method with constant current of-1 mA and electrodeposition time of 0.5h to obtain the nickel-modified antimony-doped tin dioxide/titanium plate electrode.
The electrode is taken as a working electrode, a Pt sheet is taken as a counter electrode, Ag/AgCl is taken as a reference electrode, 50ml of 100mg/L pyridine is taken as a solution to be degraded, 0.71g of anhydrous sodium sulfate containing electrolyte, and the degradation rate of the pyridine is 100% after 2h under the voltage of 3V. The electrode is recycled for three times, and the pyridine degradation rate is still over 90% after 2 hours.
Example 2
An electrode for electrochemically degrading pyridine, similar to the procedure of example 1, was fabricated by the following steps:
(1) pretreating a titanium sheet: soaking a titanium sheet with the thickness of 0.1mm and the size of 2 multiplied by 3 cm in 40 percent sodium hydroxide solution, and keeping the titanium sheet at 80 ℃ for 1 h; then soaking the mixture in 6M HCl, and reacting for 2 hours at 90 ℃; taking out, washing with deionized water for several times, and soaking in absolute ethyl alcohol to obtain a pretreated titanium sheet for later use;
(2) preparing a precursor solution containing antimony Sb and tin Sn: weighing SnCl4˙5H2O1.75 g is dissolved in 5ml of n-butanol solution as a tin-containing precursor solution; weighing SbCl31.15g of antimony-containing precursor solution was dissolved in 5ml of n-butanol solution; according to the doping proportion of antimony, taking 900 mu l of tin-containing precursor solution and 100 mu l of antimony-containing precursor solution, and carrying out ultrasonic 5 min to uniformly mix to obtain a mixed solution;
(3) uniformly coating 200 mu l of the mixed solution obtained in the step (2) on a pre-treated titanium sheet, and standing at room temperature for 1 h; then, the user can use the device to perform the operation,
(4) placing the titanium sheet obtained in the step (3) in a muffle furnace, controlling the heating rate to be 3 ℃/min, roasting at 550 ℃ for 2h, and finally, naturally cooling to room temperature to obtain the antimony-doped tin dioxide/titanium sheet electrode Ti/Sb-SnO2;
(5) Thereby Ti/Sb-SnO2The electrode is a working electrode, the Pt sheet is a counter electrode, 50ml of 0.1M nickel nitrate solution is used as an electrolyte solution, electrochemical deposition is carried out by adopting a constant current method, the constant current is-1 mA, and the electrodeposition time is 1h, so that the nickel-modified antimony-doped tin dioxide/titanium sheet electrode is obtained.
The electrode is taken as a working electrode, a Pt sheet is taken as a counter electrode, Ag/AgCl is taken as a reference electrode, 50ml of 100mg/L pyridine is taken as a solution to be degraded, 0.71g of anhydrous sodium sulfate containing electrolyte, and the degradation rate of the pyridine is 100% after 2h under the voltage of 3V. The electrode is recycled for three times, and the pyridine degradation rate is still over 90% after 2 hours.
Example 3
An electrode for electrochemically degrading pyridine, similar to the procedure of example 1, was fabricated by the following steps:
(1) pretreating a titanium sheet: soaking a titanium sheet with the thickness of 0.2mm and the size of 2 multiplied by 3 cm in 40 percent sodium hydroxide solution, and keeping the titanium sheet at 80 ℃ for 1 h; then soaking the mixture in 6M HCl, and reacting for 2 hours at 90 ℃; taking out, washing with deionized water for several times, and soaking in absolute ethyl alcohol to obtain a pretreated titanium sheet for later use;
(2) preparing a precursor solution containing antimony Sb and tin Sn: weighing SnCl4˙5H2O1.75 g was dissolved in 5ml of n-butanol solution as a tin-containing precursor solution, and SbCl was weighed31.15g of antimony-containing precursor solution was dissolved in 5ml of n-butanol solution; according to the doping proportion of antimony, taking 950 mul of tin-containing precursor solution and 50 mul of antimony-containing precursor solution, and uniformly mixing to obtain a mixed solution;
(3) uniformly coating 200 mu l of the mixed solution obtained in the step (2) on a pre-treated titanium sheet, and standing at room temperature for 1 h; then, the user can use the device to perform the operation,
(4) subjecting the product obtained in step (3)The titanium sheet is placed in a muffle furnace, the heating rate is controlled to be 3 ℃/min, the titanium sheet is roasted for 2h at the temperature of 550 ℃, and finally the titanium sheet is naturally cooled to the room temperature to obtain the antimony doped tin dioxide/titanium sheet electrode Ti/Sb-SnO2;
(5) Thereby Ti/Sb-SnO2The electrode is a working electrode, the Pt sheet is a counter electrode, 0.5M 50ml of nickel nitrate solution is used as electrolyte solution, electrochemical deposition is carried out by adopting a constant current method, the constant current is-1 mA, and the electrodeposition time is 0.5h, so that the nickel-modified antimony-doped tin dioxide/titanium sheet electrode is obtained.
The electrode is taken as a working electrode, a Pt sheet is taken as a counter electrode, Ag/AgCl is taken as a reference electrode, 50ml of 100mg/L pyridine is taken as a solution to be degraded, 0.71g of anhydrous sodium sulfate containing electrolyte is adopted, and the pyridine degradation rate is 100% after 2 hours under the voltage of 3V. The electrode is recycled for three times, and the pyridine degradation rate is still over 90% after 2 hours.
Comparative example:
an electrode for electrochemically degrading pyridine, which was fabricated in the same manner as in steps (1) to (3) of example 3, by the following steps:
(1) pretreating a titanium sheet: soaking a titanium sheet with the thickness of 0.2mm and the size of 2 multiplied by 3 cm in 40 percent sodium hydroxide solution, and keeping the titanium sheet at 80 ℃ for 1 h; then soaking the mixture in 6M HCl, and reacting for 2 hours at 90 ℃; taking out, washing with deionized water for several times, and soaking in absolute ethyl alcohol to obtain a pretreated titanium sheet for later use;
(2) preparing a precursor solution containing antimony Sb and tin Sn: weighing SnCl4˙5H2O1.75 g was dissolved in 5ml of n-butanol solution as a tin-containing precursor solution, and SbCl was weighed31.15g of antimony-containing precursor solution was dissolved in 5ml of n-butanol solution; according to the doping proportion of antimony, taking 950 mul of tin-containing precursor solution and 50 mul of antimony-containing precursor solution, and uniformly mixing to obtain a mixed solution;
(3) uniformly coating 200 mu l of the mixed solution obtained in the step (2) on a pre-treated titanium sheet, and standing at room temperature for 1 h; then, the user can use the device to perform the operation,
(4) placing the titanium sheet obtained in the step (3) in a muffle furnace, controlling the heating rate to be 3 ℃/min, roasting at 550 ℃ for 2h, and finally naturally cooling to room temperature to obtain the antimony-doped tin dioxide/titanium sheet electrode Ti/Sb-SnO2。
Thereby Ti/Sb-SnO2The electrode is a working electrode, the Pt sheet is a counter electrode, Ag/AgCl is a reference electrode, 50ml of 100mg/L pyridine is a solution to be degraded, 0.71g of anhydrous sodium sulfate containing electrolyte, and the pyridine degradation rate is 90% after 2 hours under the voltage of 3V. The electrode is recycled for three times, and the pyridine degradation rate is 50% after 2 hours.
The electrodes of examples 1 to 3 for electrochemically degrading pyridine had stable types, as compared to the comparative example.
Claims (9)
1. A method for manufacturing an electrode for electrochemically degrading pyridine is characterized in that the electrode is a nickel-modified antimony-doped tin dioxide/titanium sheet electrode, and comprises the following manufacturing steps:
(1) preparing a precursor solution containing antimony Sb and tin Sn: respectively preparing SnCl with the concentration of 1mol/L4˙5H2O n-Butanol solution, 1mol/L SbCl3The n-butyl alcohol solution is prepared by taking two solutions according to the doping proportion of 5-10% of antimony, and uniformly mixing the two solutions by ultrasonic treatment for 5 min to obtain a mixed solution;
(2) uniformly coating 200 mu l of the mixed solution in the step (1) on a titanium sheet, and standing at room temperature for 1 h;
(3) taking a titanium sheet as a substrate, placing the titanium sheet obtained in the step (2) in a muffle furnace, and preparing antimony-doped tin dioxide Sb-SnO on the surface of the titanium sheet by adopting a thermal decomposition method2The catalyst is used for obtaining the antimony doped stannic oxide/titanium sheet electrode Ti/Sb-SnO2;
(4) With Ti/Sb-SnO2A working electrode, a Pt sheet as a counter electrode, and nickel nitrate (Ni (NO)3)2) And performing electrochemical deposition by adopting a constant current method to obtain the nickel-modified antimony-doped tin dioxide/titanium plate electrode.
2. The method for manufacturing an electrode for the electrocatalytic degradation of pyridine according to claim 1, wherein in the step (2), the titanium sheet is a titanium sheet with a thickness of 0.1-0.2 mm and a size of 2 x 3 cm, and the pretreatment is performed on the titanium sheet, comprising the following steps:
1) soaking the titanium sheet in 40% sodium hydroxide solution, and keeping the temperature at 80 ℃ for 1 h;
2) soaking the titanium sheet obtained in the step 1) in 6M HCl solution, and reacting for 2h at 90 ℃;
3) washing the titanium sheet obtained in the step 2) with deionized water for several times, and finally soaking in absolute ethyl alcohol for later use.
3. The method for manufacturing the electrode for the electrocatalytic degradation of pyridine according to claim 1, wherein in the step (3), the titanium sheet is placed in a muffle furnace, roasted for 2 hours at a heating rate of 3 ℃/min to 550 ℃, and finally naturally cooled to room temperature to obtain Ti/Sb-SnO2And an electrode.
4. The method for manufacturing the electrode for the electrocatalytic degradation of pyridine according to claim 1, wherein in the step (4), the concentration of the nickel nitrate solution is 0.1-0.5 mol/L, the constant current is-1 to-5 mA, and the electrodeposition time is 0.5-1 h.
5. The method for manufacturing an electrode for the electrocatalytic degradation of pyridine according to any one of claims 1 to 4, characterized by comprising the steps of:
(1) pretreating a titanium sheet: soaking a titanium sheet with the thickness of 0.1mm and the size of 2 multiplied by 3 cm in a 40 percent sodium hydroxide solution, and keeping the temperature at 80 ℃ for 1 h; then soaking the mixture in 6M HCl, and reacting for 2 hours at 90 ℃; taking out, washing with deionized water for several times, and soaking in absolute ethyl alcohol to obtain a pretreated titanium sheet for later use;
(2) preparing a precursor solution containing antimony Sb and tin Sn: weighing SnCl4˙5H2O1.75 g is dissolved in 5ml of n-butanol solution as a tin-containing precursor solution; weighing SbCl3Dissolving 1.15g of the mixed solution in 5ml of n-butyl alcohol solution to be used as an antimony-containing precursor solution, taking 900 mu l of the tin-containing precursor solution and 100 mu l of the antimony-containing precursor solution according to the doping proportion of antimony, and uniformly mixing by ultrasonic treatment for 5 min to obtain a mixed solution;
(3) uniformly coating 200 mu l of the mixed solution obtained in the step (2) on a pre-sheet titanium sheet, and standing at room temperature for 1 h; then, the user can use the device to perform the operation,
(4) placing the titanium sheet obtained in the step (3) in a muffle furnace, controlling the heating rate to be 3 ℃/min, roasting at 550 ℃ for 2h, and finally naturally cooling to room temperature to obtain the antimony-doped tin dioxide/titanium sheet electrode Ti/Sb-SnO2;
(5) With Ti/Sb-SnO2As a working electrode, a Pt sheet as a counter electrode, and 50ml of 0.1M nickel nitrate (Ni (NO)3)2) And performing electrochemical deposition by adopting a constant current method with constant current of-1 mA and electrodeposition time of 0.5h to obtain the nickel-modified antimony-doped tin dioxide/titanium plate electrode.
6. The method for manufacturing an electrode for the electrocatalytic degradation of pyridine according to any one of claims 1 to 4, characterized by comprising the steps of:
(1) pretreating a titanium sheet: soaking a titanium sheet with the thickness of 0.1mm and the size of 2 multiplied by 3 cm in 40 percent sodium hydroxide solution, and keeping the titanium sheet at 80 ℃ for 1 h; then soaking the mixture in 6M HCl, and reacting for 2 hours at 90 ℃; taking out, washing with deionized water for several times, and soaking in absolute ethyl alcohol to obtain a pretreated titanium sheet for later use;
(2) preparing a precursor solution containing antimony Sb and tin Sn: weighing SnCl4˙5H2O1.75 g is dissolved in 5ml of n-butanol solution as a tin-containing precursor solution; weighing SbCl31.15g of antimony-containing precursor solution was dissolved in 5ml of n-butanol solution; according to the doping proportion of antimony, taking 900 mu l of tin-containing precursor solution and 100 mu l of antimony-containing precursor solution, and carrying out ultrasonic 5 min to uniformly mix to obtain a mixed solution;
(3) uniformly coating 200 mu l of the mixed solution obtained in the step (2) on a pre-treated titanium sheet, and standing at room temperature for 1 h; then, the user can use the device to perform the operation,
(4) placing the titanium sheet obtained in the step (3) in a muffle furnace, controlling the heating rate to be 3 ℃/min, roasting at 550 ℃ for 2h, and finally, naturally cooling to room temperature to obtain the antimony-doped tin dioxide/titanium sheet electrode Ti/Sb-SnO2;
(5) Thereby Ti/Sb-SnO2The electrode is a working electrode, the Pt sheet is a counter electrode, and 50ml of 0.1M nickel nitrate solution is used as an electrolyte solutionAnd performing electrochemical deposition by a constant current method, wherein the constant current is-1 mA, and the electrodeposition time is 1h to obtain the nickel-modified antimony-doped tin dioxide/titanium plate electrode.
7. The method for manufacturing an electrode for the electrocatalytic degradation of pyridine according to any one of claims 1 to 4, characterized by comprising the steps of:
(1) pretreating a titanium sheet: soaking a titanium sheet with the thickness of 0.2mm and the size of 2 multiplied by 3 cm in 40 percent sodium hydroxide solution, and keeping the titanium sheet at 80 ℃ for 1 h; then soaking the mixture in 6M HCl, and reacting for 2 hours at 90 ℃; taking out, washing with deionized water for several times, and soaking in absolute ethyl alcohol to obtain a pretreated titanium sheet for later use;
(2) preparing a precursor solution containing antimony Sb and tin Sn: weighing SnCl4˙5H2O1.75 g was dissolved in 5ml of n-butanol solution as a tin-containing precursor solution, and SbCl was weighed31.15g of antimony-containing precursor solution was dissolved in 5ml of n-butanol solution; according to the doping proportion of antimony, taking 950 mul of tin-containing precursor solution and 50 mul of antimony-containing precursor solution, and uniformly mixing to obtain a mixed solution;
(3) uniformly coating 200 mu l of the mixed solution obtained in the step (2) on a pre-treated titanium sheet, and standing at room temperature for 1 h; then, the user can use the device to perform the operation,
(4) placing the titanium sheet obtained in the step (3) in a muffle furnace, controlling the heating rate to be 3 ℃/min, roasting at 550 ℃ for 2h, and finally naturally cooling to room temperature to obtain the antimony-doped tin dioxide/titanium sheet electrode Ti/Sb-SnO2;
(5) Thereby Ti/Sb-SnO2The electrode is a working electrode, the Pt sheet is a counter electrode, 0.5M 50ml of nickel nitrate solution is used as electrolyte solution, electrochemical deposition is carried out by adopting a constant current method, the constant current is-1 mA, and the electrodeposition time is 0.5h, so that the nickel-modified antimony-doped tin dioxide/titanium sheet electrode is obtained.
8. An electrode for electrochemically degrading pyridine, characterized by being manufactured according to the method of any one of claims 1 to 7, and specifically comprising: a titanium sheet substrate; the titanium sheet substrate is covered with an antimony-doped tin dioxide catalyst; and a nickel hydroxide or nickel oxide protective layer is deposited on the surface of the antimony-doped tin dioxide catalyst.
9. Use of the electrode for electrochemically degrading pyridine according to claim 8 as an electrode in electrocatalytic degradation of pyridine at normal temperature.
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CN115259295A (en) * | 2022-08-12 | 2022-11-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Electrode manufacturing method for degrading resorcinol by electrocatalysis, product and application |
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