CN117303511A - Preparation method and application of leaf-like Sn-Ni electrocatalytic oxidation electrode - Google Patents
Preparation method and application of leaf-like Sn-Ni electrocatalytic oxidation electrode Download PDFInfo
- Publication number
- CN117303511A CN117303511A CN202311159699.1A CN202311159699A CN117303511A CN 117303511 A CN117303511 A CN 117303511A CN 202311159699 A CN202311159699 A CN 202311159699A CN 117303511 A CN117303511 A CN 117303511A
- Authority
- CN
- China
- Prior art keywords
- electrode
- electrocatalytic oxidation
- leaf
- substrate
- recl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910020938 Sn-Ni Inorganic materials 0.000 title claims abstract description 24
- 229910008937 Sn—Ni Inorganic materials 0.000 title claims abstract description 24
- 230000003647 oxidation Effects 0.000 title claims abstract description 21
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 238000004070 electrodeposition Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 14
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910018100 Ni-Sn Inorganic materials 0.000 claims abstract description 10
- 229910018532 Ni—Sn Inorganic materials 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004020 conductor Substances 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 238000007605 air drying Methods 0.000 claims abstract description 5
- 230000015556 catabolic process Effects 0.000 claims abstract description 5
- 238000006731 degradation reaction Methods 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 17
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 17
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 16
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 16
- 235000011150 stannous chloride Nutrition 0.000 claims description 16
- 239000001119 stannous chloride Substances 0.000 claims description 16
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- ZZPAXHDZFDUTLY-UHFFFAOYSA-L ammonium nickel sulfate hexahydrate Chemical compound N.N.O.O.O.O.O.O.[Ni+2].OS([O-])(=O)=O.OS([O-])(=O)=O ZZPAXHDZFDUTLY-UHFFFAOYSA-L 0.000 claims description 8
- 239000001509 sodium citrate Substances 0.000 claims description 8
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 2
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical compound Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract 1
- 238000007781 pre-processing Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000012851 eutrophication Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001546 nitrifying effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/835—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
-
- 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
- C02F1/461—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
-
- 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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses a preparation method of a treelike Sn-Ni electrocatalytic oxidation electrode, which comprises the steps of preprocessing a substrate made of conductive materials, and then putting the preprocessed substrate into RECl 3 Mixing PVP solution uniformly, placing the mixture in an autoclave for sealing reaction, and then separating solid from liquid, and cleaning the solid to obtain the self-cleaning luminous electrode substrate; the self-cleaning luminous electrode substrate is used as a cathode, the graphite electrode is used as an anode, the cathode and the anode are placed in Ni-Sn/SD electrodeposition liquid, electrodeposition is carried out at room temperature, the voltage is 5-15V, and the current density is 4-8mA/cm 2 Air-drying after reaction to obtain the product;the leaf-like Sn-Ni electrocatalytic oxidation electrode is applied to ammonia nitrogen degradation, the nitrate nitrogen removal rate is above 75%, the electrode catalytic efficiency is high, and the electrode has a great application prospect.
Description
Technical Field
The invention belongs to the technical field of electrocatalytic water treatment, and particularly relates to a preparation method and application of a treelike Sn-Ni ammonia nitrogen selective electrocatalytic nitrifying electrode.
Background
In recent years, with the development of industrialization, the pollution problem caused by ammonia nitrogen wastewater is increasingly serious, and ammonia nitrogen is one of important factors for destroying the balance of water and causing eutrophication of water; the excessive discharge of the water can cause great harm to the ecological environment and human body, and the water can promote the eutrophication of the water body, generate malodor and cause barriers to water supply. The ammonia nitrogen in the water is mainly discharged from waste water and garbage percolate in industries such as chemical fertilizers, tanning, cultivation, petrochemical industry, meat processing and the like, and urban sewage and agricultural irrigation drainage. The world health organization and the U.S. environmental protection agency limit the maximum pollutant content in drinking water to 50mg/L (NO) 3 - ) And 10mg/L (NO) 3 -N). Therefore, how to economically and efficiently remove ammonia nitrogen in wastewater has become a research hot spot in recent years, and is considered as the most promising industrial popularization technology due to environmental adaptability, stability and operability of electrochemical technology.
The electrode material affects dynamics and product selectivity in the electrochemical nitrate reduction process, so the key of the electrocatalytic reduction technology is the selection of the electrode material and the catalyst, and the material with good performance has the characteristics of electrocatalytic performance and higher conductivity and stability. The noble metals such as Pt, pd, ru and the like have good electrocatalytic activity, but have high cost, and Ni-Sn has high reaction kinetics speed, but the pure nickel plate is used as a cathode to have poor reaction activity, so that the introduction of Sn is used for modifying the electrode performance and apparent morphology, so that the search of an electrode with excellent performance is of great significance for researching water treatment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a treelike Sn-Ni electrocatalytic oxidation electrode, solves the problem of low treatment efficiency of the conventional wastewater, and can be used for electrocatalytically reducing nitrate nitrogen in water.
The preparation method of the leaf-like Sn-Ni electrocatalytic oxidation electrode comprises the following steps:
(1) After the substrate made of the conductive material is pretreated, the pretreated substrate is put into RECl 3 Mixing PVP solution uniformly, sealing in an autoclave, reacting at 160-200 ℃ for 1-3h, separating solid from liquid, and cleaning the solid to obtain the self-cleaning luminous electrode substrate;
RECl 3 the PVP solution is prepared by mixing RECl 3 Respectively dissolving polyvinylpyrrolidone (PVP) in glycol, stirring, mixing, and adding RECl 3 Dripping the solution into polyvinylpyrrolidone solution, and mixing, wherein RECl is prepared 3 Is yttrium chloride, lanthanum chloride, cerium chloride, europium chloride or terbium chloride, RECl 3 The mass ratio of the polyvinyl pyrrolidone to the polyvinyl pyrrolidone is 1:1-2;
the conductive material is one of titanium, ruthenium, ITO and carbon cloth, and the substrate pretreatment is that the conductive material is cleaned by sand paper polishing water and then is cleaned by acetone, absolute ethyl alcohol and water in sequence, and is dried for standby;
(2) Placing nickel ammonium sulfate hexahydrate and stannous chloride in water, uniformly mixing, adding sodium dodecyl sulfate, then adding sodium citrate, and uniformly mixing to obtain Ni-Sn/SD electrodeposition liquid;
the molar ratio of nickel ammonium sulfate hexahydrate to stannous chloride is 1-4:1, the molar ratio of stannous chloride to sodium dodecyl sulfate is 40-60:1, and the molar ratio of stannous chloride to sodium citrate is 20-40:1;
(3) Taking the self-cleaning luminous electrode substrate in the step (1) as a cathode, taking a graphite electrode as an anode, placing a cathode and an anode in Ni-Sn/SD electrodeposition liquid, and performing electrodeposition at room temperature, wherein the voltage is 5-15V, and the current density is 4-8mA/cm 2 And (3) air-drying after the reaction to obtain the leaf-like Sn-Ni electrocatalytic oxidation electrode.
The invention also aims to apply the leaf-shaped Sn-Ni-like electrocatalytic oxidation electrode prepared by the method to ammonia nitrogen degradation.
The invention has the advantages and technical effects that:
1. the electrochemical performance and apparent morphology of the electrode are modified after the electrode substrate is doped with Sn-Ni, so that the electrode has good stability, and meanwhile, the leaf-shaped tip has the advantages of multiple reaction points, good corrosion resistance, high specific surface area and the like, and the efficiency of electrocatalytic reduction of ammonia nitrogen and degradation of organic pollutants is effectively improved;
2. according to the invention, two non-noble metals (Sn and Ni) are selected as catalysts, the Ni metal has good promotion effect on the speed limiting step of the nitrate reduction process, the Sn-Ni electrode electrolysis product is mainly nitrogen, the selectivity is between 50% and 70%, and simultaneously, the dendritic tip can generate larger voltage, so that more active substances such as free radicals and the like are generated, and the degradation of pollutants in water is enhanced;
3. the invention adopts electrodeposition preparation, and has simple method, good stability and long preservation time; compared with the conventional electrode, the Sn-Ni nano electrode prepared by the method has more excellent ammonia nitrogen and organic matter removal efficiency.
Drawings
FIG. 1 is an SEM image of a treelike Sn-Ni electrocatalytic oxidation electrode made by the method of the present invention;
FIG. 2 shows the effect of the electrode of example 1 on purifying ammonia nitrogen;
FIG. 3 shows the effect of the electrode of example 2 on purifying ammonia nitrogen.
Detailed Description
The present invention will be further described in detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more comprehensible. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the invention;
example 1: the preparation and application of the leaf-like Sn-Ni electrocatalytic oxidation electrode are as follows:
1. polishing a titanium mesh with the purity of 99.9% and the thickness of 0.2mm by using 300-mesh and 600-mesh sand paper respectively until the surface is free from scratches, flushing the surface by using deionized water, sequentially putting the titanium mesh into acetone, absolute ethyl alcohol and deionized water, respectively carrying out ultrasonic treatment for 10min, taking out and drying for later use;
2. the pretreated titanium mesh was placed in a reaction vessel, and 0.435g of YCl was added 3 And 0.676g PVP were dissolved in 15mL and 30mL ethylene glycol, respectively, and YCl was then stirred vigorously 3 Solution is slowSlowly dripping the self-cleaning luminescent electrode substrate into PVP solution to form uniform solution, then placing the solution into an autoclave for sealing, reacting for 2 hours at 180 ℃, separating solid from liquid, and respectively cleaning the solid with absolute ethyl alcohol and water for 3 times to obtain the self-cleaning luminescent electrode substrate;
3. placing nickel ammonium sulfate hexahydrate and stannous chloride in water, uniformly mixing, adding sodium dodecyl sulfate, then adding sodium citrate, and uniformly mixing to obtain Ni-Sn/SD electrodeposition liquid, wherein the molar ratio of the nickel ammonium sulfate hexahydrate to the stannous chloride is 2:1, the molar ratio of the stannous chloride to the sodium dodecyl sulfate is 50:1, and the molar ratio of the stannous chloride to the sodium citrate is 30:1;
4. taking a graphite electrode as an anode, taking a self-cleaning luminous electrode substrate as a cathode, placing a cathode and an anode in Ni-Sn/SD electrodeposition liquid, and performing electrodeposition at room temperature, wherein the voltage is 10V, and the current density is 5mA/cm 2 And after 30min of reaction, naturally air-drying to obtain the leaf-like Sn-Ni electrocatalytic oxidation electrode, wherein an SEM image of the electrode is shown in figure 1, and the fact that a load on the electrode grows on a substrate is seen from the image, and an ordered fern leaf-shaped structure is formed through a certain crystal arrangement, so that the contact area of the electrode and pollutants can be effectively increased, and the electrode has good catalytic activity. .
5. The tree leaf-like Sn-Ni electrocatalytic oxidation electrode is adopted to simulate wastewater through electrocatalytic reduction
490mL of wastewater containing 100mg/L of nitrate nitrogen is simulated, 0.5g/L of sodium sulfate is used as electrolyte, the prepared leaf-like catalytic electrode is used as a cathode, the graphite electrode is used as an anode, the distance between the anode and the cathode is 3cm, and the current density is 20mA/cm at the moment 2 The electrocatalytic reduction reaction is carried out for 2 hours, the relation between the removal effect of nitrate nitrogen and time is shown in figure 2, the removal rate of nitrate nitrogen is 75% after 2 hours of electrocatalytic treatment, and the electrode has higher catalytic efficiency.
Example 2: the preparation and application of the leaf-like Sn-Ni electrocatalytic oxidation electrode are as follows:
1. polishing an ITO plate with the purity of 99.9% and the thickness of 0.2mm by using 300-mesh sand paper and 600-mesh sand paper respectively until the surface is free from scratches, flushing the surface by using deionized water, sequentially putting the ITO plate into acetone, absolute ethyl alcohol and deionized water, respectively carrying out ultrasonic treatment for 10min, taking out and drying for later use;
2. placing the pretreated ITO substrate into a reaction vessel, and adding 0.435g of EuCl 3 And 0.676g PVP were dissolved in 15mL and 30mL ethylene glycol, respectively, and then EuCl was dissolved with vigorous stirring 3 Slowly dripping the solution into PVP solution to form uniform solution, sealing in an autoclave, reacting at 180 ℃ for 2 hours, separating solid from liquid, and cleaning the solid with absolute ethyl alcohol and water for 3 times to obtain a self-cleaning luminous electrode substrate;
3. placing nickel ammonium sulfate hexahydrate and stannous chloride in water, uniformly mixing, adding sodium dodecyl sulfate, then adding sodium citrate, and uniformly mixing to obtain Ni-Sn/SD electrodeposition liquid, wherein the molar ratio of the nickel ammonium sulfate hexahydrate to the stannous chloride is 1:1, the molar ratio of the stannous chloride to the sodium dodecyl sulfate is 45:1, and the molar ratio of the stannous chloride to the sodium citrate is 35:1;
4. taking a graphite electrode as an anode, taking a self-cleaning luminous electrode substrate as a cathode, placing a cathode and an anode in Ni-Sn/SD electrodeposition liquid, and performing electrodeposition at room temperature, wherein the voltage is 8V, and the current density is 7mA/cm 2 Naturally air-drying after reacting for 25min to obtain the leaf-like Sn-Ni electrocatalytic oxidation electrode;
5. 490mL of wastewater containing 100mg/L of nitrate nitrogen is simulated, 0.5g/L of sodium sulfate is used as electrolyte, the prepared leaf-like catalytic electrode is used as a cathode, the graphite electrode is used as an anode, the distance between the anode and the cathode is 3cm, and the current density is 20mA/cm at the moment 2 The electrocatalytic reduction reaction is carried out for 2 hours, the relation between the removal effect of nitrate nitrogen and time is shown in figure 3, the removal rate of nitrate nitrogen is 82% after 2 hours of electrocatalytic treatment, and the electrode has higher catalytic efficiency.
Claims (5)
1. The preparation method of the leaf-like Sn-Ni electrocatalytic oxidation electrode is characterized by comprising the following steps of:
(1) After the substrate made of the conductive material is pretreated, the pretreated substrate is put into RECl 3 Mixing PVP solution uniformly, sealing in an autoclave, reacting at 160-200 ℃ for 1-3h, separating solid from liquid, and cleaning the solid to obtain the self-cleaning luminous electrode substrate;
(2) Placing nickel ammonium sulfate hexahydrate and stannous chloride in water, uniformly mixing, adding sodium dodecyl sulfate, then adding sodium citrate, and uniformly mixing to obtain Ni-Sn/SD electrodeposition liquid;
(3) Taking the self-cleaning luminous electrode substrate in the step (1) as a cathode, taking a graphite electrode as an anode, placing a cathode and an anode in Ni-Sn/SD electrodeposition liquid, and performing electrodeposition at room temperature, wherein the voltage is 5-15V, and the current density is 4-8mA/cm 2 And (3) air-drying after the reaction to obtain the leaf-like Sn-Ni ammonia nitrogen selective electrocatalytic oxidation electrode.
2. The method for preparing the leaf-shaped Sn-Ni electrocatalytic oxidation electrode according to claim 1, wherein the method comprises the following steps: RECl 3 The PVP solution is prepared by mixing RECl 3 Respectively dissolving polyvinylpyrrolidone in glycol, stirring, mixing, and adding RECl 3 Dripping the solution into polyvinylpyrrolidone solution, and mixing, wherein RECl is prepared 3 Is yttrium chloride, lanthanum chloride, cerium chloride, europium chloride or terbium chloride, RECl 3 The mass ratio of the polyvinyl pyrrolidone to the polyvinyl pyrrolidone is 1:1-2.
3. The method for preparing the leaf-shaped Sn-Ni electrocatalytic oxidation electrode according to claim 1, wherein the method comprises the following steps: the conductive material is one of titanium, ruthenium, ITO and carbon cloth, and the substrate pretreatment is that the conductive material is cleaned by sand paper polishing water and then is cleaned by acetone, absolute ethyl alcohol and water in sequence, and is dried for standby.
4. The method for preparing the leaf-shaped Sn-Ni electrocatalytic oxidation electrode according to claim 1, wherein the method comprises the following steps: the molar ratio of nickel ammonium sulfate hexahydrate to stannous chloride is 1-4:1, the molar ratio of stannous chloride to sodium dodecyl sulfate is 40-60:1, and the molar ratio of stannous chloride to sodium citrate is 20-40:1.
5. Use of the treelike Sn-Ni electrocatalytic oxidation electrode made by the method for making a treelike Sn-Ni electrocatalytic oxidation electrode of any one of claims 1-4 for ammonia nitrogen degradation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311159699.1A CN117303511A (en) | 2023-09-11 | 2023-09-11 | Preparation method and application of leaf-like Sn-Ni electrocatalytic oxidation electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311159699.1A CN117303511A (en) | 2023-09-11 | 2023-09-11 | Preparation method and application of leaf-like Sn-Ni electrocatalytic oxidation electrode |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117303511A true CN117303511A (en) | 2023-12-29 |
Family
ID=89249009
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311159699.1A Pending CN117303511A (en) | 2023-09-11 | 2023-09-11 | Preparation method and application of leaf-like Sn-Ni electrocatalytic oxidation electrode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117303511A (en) |
-
2023
- 2023-09-11 CN CN202311159699.1A patent/CN117303511A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108191075B (en) | MoS in microbial electrolysis cell2Preparation method and application of/transition metal/graphene composite hydrogen evolution electrode | |
| CN113637989B (en) | Method for synthesizing ammonia by electrocatalytic nitrate or nitrite | |
| CN113828300B (en) | Preparation method of metal doped bismuth layered oxide and electrocatalytic reduction of CO 2 Application in (a) | |
| CN109594100B (en) | C3N4Cu/Sn loaded alloy material and preparation and application thereof | |
| CN107364934B (en) | Electrocatalytic reduction composite electrode, preparation method and application thereof | |
| CN111792705B (en) | Graphene oxide loaded carbon-based copper-nickel electrode, preparation method and application | |
| CN112626552B (en) | Method for electrodepositing Ni-Fe-Sn-P alloy on surface of foam nickel | |
| CN111501060B (en) | Copper-doped bismuth bimetallic material and preparation and application thereof | |
| CN114438545A (en) | Bimetal doped Ni3S2Preparation method of oxygen evolution electrocatalyst | |
| CN101728541A (en) | Method for preparing carbon nano tube loaded cobalt-platinum alloy catalyst | |
| CN113957456A (en) | Nickel-based alkaline electrolytic water catalyst with co-doped combination heterostructure and preparation method thereof | |
| CN114686917A (en) | Electro-catalytic catalyst for synthesizing ammonia by reducing nitrate, preparation method and application thereof | |
| CN115010217A (en) | Preparation method and application of three-dimensional composite electrode for efficiently removing nitrate in water through electro-catalysis | |
| CN113968602A (en) | Method for removing nitrified nitrogen in water through electro-catalysis | |
| CN113896299A (en) | electro-Fenton reaction cathode material of ferromanganese layered double hydroxide loaded biochar and preparation method and application thereof | |
| CN110975907B (en) | Preparation method of foam nickel electrode loaded with iron and basic cobalt carbonate for catalyzing oxidation of water or organic matters | |
| CN117303511A (en) | Preparation method and application of leaf-like Sn-Ni electrocatalytic oxidation electrode | |
| CN114920333B (en) | Treatment method of high-concentration ammonia nitrogen wastewater | |
| CN116282393A (en) | Palladium-nickel phosphide-foam nickel composite electrode and preparation method and application thereof | |
| CN102061483B (en) | Method for preparing palladium-nickel duplex metal catalytic electrode by using sodium dodecyl benzene sulfonate as aid | |
| CN115646214A (en) | Conductive catalytic hydrophobic membrane and preparation method and application thereof | |
| CN110453256B (en) | Polyhedral cobalt-iridium nanoparticle hydrogen evolution electrocatalyst, plating solution and preparation method thereof | |
| CN115504544B (en) | Cu-Bi/TiO2Preparation method and application of nano electrocatalytic denitrification electrode | |
| CN114887639B (en) | CO (carbon monoxide) 2 Reduction catalyst, application and preparation method thereof | |
| CN116426957A (en) | Preparation method and application of stainless steel carrier immobilized metal catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |