CN113526622A - Foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material and preparation method and application thereof - Google Patents
Foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material and preparation method and application thereof Download PDFInfo
- Publication number
- CN113526622A CN113526622A CN202110784849.2A CN202110784849A CN113526622A CN 113526622 A CN113526622 A CN 113526622A CN 202110784849 A CN202110784849 A CN 202110784849A CN 113526622 A CN113526622 A CN 113526622A
- Authority
- CN
- China
- Prior art keywords
- nickel
- iron
- tin
- porous carbon
- foamed
- 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.)
- Granted
Links
Images
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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- 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
- C02F2001/46142—Catalytic coating
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode and a preparation method and application thereof. The preparation method comprises the following steps: soaking the foamed nickel in a solution containing citric acid, ferric nitrate nonahydrate, stannous chloride, F127 and phenolic resin, and calcining the precursor polymer containing iron and tin loaded by the foamed nickel at high temperature in a tubular furnace to obtain the foamed nickel loaded porous carbon coated nickel-iron-nickel alloy electrode material. The electrode material has good electrocatalytic activity, is used for electrocatalytic reduction of nitrate radical reaction, can achieve good nitrate radical removal effect and realize good nitrogen selectivity. The method has the advantages of low cost, high catalytic activity and high nitrogen selectivity, and solves the problems of low nitrogen selectivity in the electrocatalytic reduction of nitrate, high use cost of a noble metal electrode and the like.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis, and particularly relates to a nickel foam loaded porous carbon coated nickel tin-iron nickel alloy electrode material, and a preparation method and application thereof.
Background
Due to the rapid development of industry and agricultural technology, a large amount of nitrate pollution is inevitably generated directly or indirectly, and the excessive nitrate causes eutrophication of water bodies. In view of nitrate pollution, many methods for removing nitrate have been developed, and conventional methods for removing nitrate include reverse osmosis, ion exchange, electrodialysis, catalytic denitrification, biological denitrification, etc., but are not suitable for large-scale application due to limitations such as high cost, many byproducts, and low reaction rate. There is a need to find a more suitable removal method, in contrast to the advantages of electrocatalytic reduction of nitrate, such as no chemical input, high catalytic efficiency, etc., which are gradually developing. Electrocatalytic reduction of nitrate is achieved by gradual reduction of nitrate to ammonium and nitrogen at the cathode surface. The selection of cathode materials becomes the core of the technology for electrocatalytic reduction of nitrate.
The current common nitrate-removing cathode materials are mainly noble metal-based electrodes, but are not suitable for large-scale application due to high price. The metal composite material is widely concerned due to good electrocatalytic activity, and in the metal composite material, NiSn and FeNi alloy are low in price and have good electrocatalytic activity, and in addition, the introduction of Sn can effectively improve the nitrogen selectivity. Therefore, the NiSn and FeNi alloy material has good application prospect in the process of electrocatalytic reduction of nitrate. The specific surface area and the porosity of the electrode play a vital role in dispersing active substances, improving mass transfer and enhancing the performance of the electrocatalyst, so that the introduction of the mesoporous carbon material as a catalyst carrier can improve the specific surface area of the electrode and well disperse the electrocatalytic active sites.
The invention provides a preparation method of a nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material, which is applied to electrocatalytic reduction of nitrate radicals in water. The method aims to improve the electrocatalytic efficiency of nitrate radicals, improve the selectivity of nitrogen and reduce the cost of an electrode.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a nickel foam loaded porous carbon coated nickel tin-iron nickel alloy electrode material.
Yet another object of the present invention is to: provides a preparation method of the foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material product.
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 foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material comprises a substrate and porous carbon coated nickel tin-iron nickel alloy nanoparticles (NiSn-FeNi/pC) growing on the surface of the substrate; the substrate is pretreated foamed nickel.
Further, in the foamed nickel-loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode material, the mass ratio of Sn: fe = (0-1): (2-4).
Furthermore, the pretreated foamed nickel is dried foamed nickel after being soaked in acetone and hydrochloric acid with the concentration of 2M-5M and washed by deionized water and ethanol.
The invention also provides a preparation method of the foamed nickel loaded porous carbon coated nickel-tin-iron-nickel alloy electrode material, which comprises the following steps of soaking foamed nickel in a precursor solution containing citric acid, ferric nitrate nonahydrate, stannous chloride, F127 and phenolic resin, and calcining the obtained precursor polymer containing iron and tin loaded by the foamed nickel in a tubular furnace at high temperature to obtain the foamed nickel loaded porous carbon coated nickel-tin-iron-nickel alloy electrode material:
1) preparing a precursor solution:
(1) dissolving a high-molecular nonionic surfactant F127 in absolute ethyl alcohol, wherein the mass ratio of the F127 to the absolute ethyl alcohol is 1: (2-5), stirring for 10-20 min to obtain an absolute ethyl alcohol solution of F127;
(2) adding 50% by mass of phenolic resin into the solution prepared in the step (1), and mixing and stirring for 20-40 min;
(3) adding 0-1 part by mass of stannous chloride and 2-5 parts by mass of absolute ethyl alcohol into the solution prepared in the step (2), stirring for 15-20 min, adding 2-8 parts by mass of ferric nitrate nonahydrate, stirring for 15-20 min, and enabling the dosage of the ferric nitrate nonahydrate to be 0.2 times of the mass of F127;
(4) dissolving anhydrous citric acid in an ethanol solution, adding the solution obtained in the step (3), wherein the ratio of the mass of the anhydrous citric acid to the total mass of stannous chloride and ferric nitrate nonahydrate is 3:1, the ethanol solution is 2-4 parts by mass, and stirring for 30-60 min to obtain a precursor solution;
2) soaking the pretreated foam nickel in a precursor solution for 3-6 min, taking out, standing at room temperature for 10-14 h, curing at 100-120 ℃ for 20-30 h, and calcining at 700-900 ℃ in a nitrogen atmosphere to obtain the foam nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material.
Wherein the temperature rise rate of the calcination is 1-5 ℃/min.
The foamed nickel is pretreated by the method comprising the following steps: the foamed nickel is soaked in acetone and hydrochloric acid with the concentration of 2M-5M in sequence, washed by deionized water and ethanol and dried.
The drying is carried out for 2 to 6 hours at the temperature of 70 to 80 ℃ in vacuum.
Further, the pretreatment specifically includes: soaking and washing the foamed nickel in acetone for 15 min, and ultrasonically washing for 5 min; washing with ultrapure water, etching with hydrochloric acid for 15 min, and performing ultrasonic treatment for 5 min; washing with ultrapure water, washing with ethanol, and vacuum drying at 70 deg.C for 4 hr.
In the step (1), when the mass part of F127 is 1, the mass ratio of F127 to absolute ethyl alcohol is preferably 1: 3.
as an embodiment of the invention, the curing temperature is 100 ℃ to 120 ℃. Preferably, the curing temperature is 100 ℃.
As an embodiment of the invention, the temperature rise rate of the calcination is 1-5 ℃/min, and the calcination temperature is 700-900 ℃. Preferably, the heating rate is 1 ℃/min, and the calcining temperature is 800 ℃.
The invention also provides application of the foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material in electrocatalytic reduction of nitrate.
The foam nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material is a novel electrode material which is low in price, high in electrocatalytic activity, stable in catalytic performance and high in nitrogen selectivity. The invention utilizes the carbothermic reduction and impregnation method to directly grow the porous carbon-coated nickel-tin-iron-nickel alloy on the surface of the foamed nickel, and can realize good conductivity without adding a binder and a conductive agent. The coating structure of the porous carbon enables the electrode to have a large specific surface area and well disperse alloy particles, and a large number of active sites are provided, so that high nitrogen selectivity is realized.
The invention relates to a foamed nickel loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode material, which is characterized in that pretreated foamed nickel is used as a substrate, a precursor solution of stannous chloride and ferric nitrate is adsorbed into pores of the foamed nickel by using an impregnation method, an oxide on the surface of the foamed nickel is used for providing a nickel source, and then an active substance porous carbon-coated nickel-tin-iron-nickel alloy directly grows on the surface of the foamed nickel through co-assembly and carbon thermal reduction, so that the high-stability and high-selectivity electrocatalytic electrode material is obtained.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention adopts an immersion method to ensure that the porous carbon-coated nickel-tin-iron-nickel alloy directly grows on the surface of the foamed nickel,
the porous carbon is coated with nickel-tin and iron-nickel alloy particles, so that active sites can be better dispersed, and the specific surface area of the catalyst can be improved, thereby improving the catalytic activity;
2) the invention takes the oxide on the surface of the foam nickel as a nickel source, successfully forms nickel-tin and iron-nickel alloy particles with a tin source and an iron source, and reduces chemical input;
3) the introduction of tin element can well improve the selectivity of the electrode to nitrogen;
4) the foamed nickel loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode disclosed by the invention is high in catalytic activity and good in nitrogen selectivity, and the problems of high cost, poor catalytic activity, low selectivity and the like of the traditional electrode material are solved.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting examples and comparative examples with reference to the following drawings:
FIG. 1 is an X-ray diffraction pattern of a porous carbon-coated nickel-tin-iron-nickel alloy active material on the surface of an electrode prepared in example 1;
FIG. 2 is a comparison graph of the performance of electrocatalytic reduction of nitrate by a foamed nickel-loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode at different iron-tin ratios;
FIG. 3 is a comparison graph of nitrogen selectivity for electrocatalytic reduction of nitrate with a foamed nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode at different iron-tin ratios.
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
A foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material comprises a substrate and porous carbon coated nickel tin-iron nickel alloy nanoparticles NiSn-FeNi/pC growing on the surface of the substrate, wherein the ratio of Fe to Sn is =2: 1; the substrate is pretreated foamed nickel and is prepared by the following steps:
1) preparing a base material: soaking and washing the foam nickel cut into 2 cm by 2.5 cm in acetone for 15 min, and ultrasonically washing for 5 min; washing with ultrapure water, etching with 3M HCl for 15 min, and performing ultrasonic treatment for 5 min; repeatedly washing with ultrapure water, washing with ethanol, standing at 70 deg.C, vacuum drying for 4 hr to obtain pretreated foamed nickel as substrate material;
2) preparing a precursor solution:
(1) dissolving 1 g of high-molecular nonionic surfactant F127 in 3 g of absolute ethyl alcohol, and stirring for 10 min to obtain an absolute ethyl alcohol solution of F127;
(2) adding 1 g of phenolic resin with the mass fraction of 50% into the solution prepared in the step (1), and then mixing and stirring for 20 min;
(3) adding 0.047 g of stannous chloride and 2 g of absolute ethyl alcohol into the solution prepared in the step (2), stirring for 15 min, adding 0.2 g of ferric nitrate nonahydrate, and stirring for 15 min to ensure that the ratio of Fe to Sn is =2:1, wherein the dosage of the ferric nitrate nonahydrate is 0.2 times of the mass of F127;
(4) dissolving 0.43 g of anhydrous citric acid in 2 g of ethanol, adding the solution into the solution obtained in the step (3), and stirring for 30 min to obtain a precursor solution;
3) and soaking the pretreated foamed nickel in a precursor solution, taking out after 5 min, standing at room temperature for 12 h, curing at 100 ℃ for 24 h, and calcining at the heating rate of 1-5 ℃/min for 3 h in the nitrogen atmosphere at 800 ℃ to obtain the foamed nickel-loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode material (Fe: Sn =2: 1).
FIG. 1 is an X-ray diffraction diagram of a scraped surface porous carbon-coated nickel-tin-iron-nickel alloy of a prepared foamed nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode (Fe: Sn =2: 1), and it can be seen from FIG. 1 that an electrocatalyst supported on the surface of foamed nickel is Ni1.5Sn and Fe0.64Ni0.36The alloy exists in the form of.
50 mg/L NO in 100 ml3 -0.05 mol/L sodium sulfate was added to the sodium nitrate solution of (E) -N. A three-electrode system is adopted, a working electrode is a prepared foamed nickel-loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode (Fe: Sn =2: 1), a counter electrode is a platinum mesh electrode, a reference electrode is a saturated calomel electrode, the removal rate of nitrate radicals after electrolysis for 24 hours under the voltage of-1.3V is 76%, as shown in figure 2, the selectivity of nitrogen is 42.7%, as shown in figure 3.
Example 2
This example is a variation on example 1, except that stannous chloride was added in an amount of 0.024 g, to yield a nickel foam supported porous carbon coated nickel-tin-iron-nickel alloy electrode (Fe: Sn = 4: 1), wherein the precursor solution was prepared as follows:
(1) dissolving 1 g of high-molecular nonionic surfactant F127 in 3 g of absolute ethyl alcohol, and stirring for 10 min to obtain an absolute ethyl alcohol solution of F127;
(2) adding 1 g of phenolic resin with the mass fraction of 50% into the solution prepared in the step (1), and then mixing and stirring for 20 min;
(3) adding 0.024 g of stannous chloride and 2 g of absolute ethyl alcohol into the solution prepared in the step (2), stirring for 15 min, adding 0.2 g of ferric nitrate nonahydrate, and stirring for 15 min to ensure that the ratio of Fe to Sn is = 4:1, wherein the dosage of the ferric nitrate nonahydrate is 0.2 times of the mass of F127;
(4) and (3) dissolving 0.43 g of anhydrous citric acid in 2 g of ethanol, adding the solution into the solution obtained in the step (3), and stirring for 30 min to obtain a precursor solution.
50 mg/L NO in 100 ml3 -0.05 mol/L sodium sulfate was added to the sodium nitrate solution of (E) -N. A three-electrode system is adopted, a working electrode is a prepared foamed nickel loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode (Fe: Sn = 4: 1), a counter electrode is a platinum mesh electrode, a reference electrode is a saturated calomel electrode, and the removal rate of nitrate radicals is 80.3% after electrolysis is carried out for 24 hours under the voltage of-1.3V, as shown in figure 2; the nitrogen selectivity was 26.4%, see FIG. 3.
Example 3
This example is a variation of example 1, and the technical scheme is the same as that of example 1, except that stannous chloride is not added to the precursor. And obtaining the foam nickel loaded porous carbon coated iron-nickel alloy electrode.
50 mg/L NO in 100 ml3 -0.05 mol/L sodium sulfate was added to the sodium nitrate solution of (E) -N. A three-electrode system is adopted, a working electrode is a prepared foamed nickel loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode, a counter electrode is a platinum mesh electrode, a reference electrode is a saturated calomel electrode, and the removal rate of nitrate radicals is 87.8 percent after electrolysis is carried out for 24 hours under the voltage of-1.3V, which is shown in figure 2; the nitrogen selectivity was 27.1%, see FIG. 3.
From the above, it can be seen that the performance of electrocatalytic reduction of nitrate is weakly limited as the Sn incorporation increases, but the nitrogen selectivity varies significantly, being highest when the mass ratio of iron to tin is 2: 1.
Example 4
This example is a modification of example 1, and the technical scheme is the same as that of example 1, except that 1 g/L sodium chloride is added to the electrolyte.
50 mg/L NO in 100 ml3 -0.05 mol/L sodium sulfate and 1 g/L sodium chloride are added into the sodium nitrate solution of the-N. A three-electrode system is adopted, a working electrode is a prepared foamed nickel loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode (Fe: Sn =2: 1), a counter electrode is a platinum mesh electrode, a reference electrode is a saturated calomel electrode, the removal rate of nitrate radicals is 80.2 percent, and the selectivity of nitrogen is 100 percent after electrolysis is carried out for 24 hours under the voltage of-1.3V.
This example illustrates that the introduction of sodium chloride can significantly improve nitrogen selectivity.
Claims (10)
1. A foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material is characterized by comprising a substrate and porous carbon coated nickel tin-iron nickel alloy nanoparticles (NiSn-FeNi/pC) growing on the surface of the substrate; the substrate is pretreated foamed nickel.
2. The foamed nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material as claimed in claim 1, wherein the mass ratio of the foamed nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material is Sn: fe = (0-1): (2-4).
3. The foamed nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material as claimed in claim 1, wherein the pretreated foamed nickel is foamed nickel dried after being sequentially soaked in acetone and hydrochloric acid with a concentration of 2M-5M, washed with deionized water and ethanol.
4. A method for preparing the foamed nickel-loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode material as claimed in any one of claims 1 to 3, wherein the foamed nickel is soaked in a precursor solution containing citric acid, ferric nitrate nonahydrate, stannous chloride, F127 and phenolic resin, and the obtained foamed nickel-loaded precursor polymer containing iron and tin is calcined at high temperature in a tubular furnace to obtain the foamed nickel-loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode material, which comprises the following steps:
1) preparing a precursor solution:
(1) dissolving a high-molecular nonionic surfactant F127 in absolute ethyl alcohol, wherein the mass ratio of the F127 to the absolute ethyl alcohol is 1: (2-5), stirring for 10-20 min to obtain an absolute ethyl alcohol solution of F127;
(2) adding 50% by mass of phenolic resin into the solution prepared in the step (1), and mixing and stirring for 20-40 min;
(3) adding 0-1 part by mass of stannous chloride and 2-5 parts by mass of absolute ethyl alcohol into the solution prepared in the step (2), stirring for 15-20 min, adding 2-8 parts by mass of ferric nitrate nonahydrate, stirring for 15-20 min, and enabling the dosage of the ferric nitrate nonahydrate to be 0.2 times of the mass of F127;
(4) dissolving anhydrous citric acid in an ethanol solution, adding the solution obtained in the step (3), wherein the ratio of the mass of the anhydrous citric acid to the total mass of stannous chloride and ferric nitrate nonahydrate is 3:1, the ethanol solution is 2-4 parts by mass, and stirring for 30-60 min to obtain a precursor solution;
2) soaking the pretreated foam nickel in a precursor solution for 3-6 min, taking out, standing at room temperature for 10-14 h, curing at 100-120 ℃ for 20-30 h, and calcining at 700-900 ℃ in a nitrogen atmosphere to obtain the foam nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material.
5. The method for preparing the foamed nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material according to claim 4, wherein the temperature rise rate of calcination is 1 ℃/min to 5 ℃/min.
6. The preparation method of the foamed nickel-supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material as claimed in claim 4 or 5, wherein the preparation method comprises the following steps: preparing a substrate and porous carbon coated nickel tin-iron nickel alloy nanoparticles NiSn-FeNi/pC growing on the surface of the substrate, wherein Fe: Sn =2: 1; the preparation method comprises the following steps:
1) preparing a base material: soaking and washing the foam nickel cut into 2 cm by 2.5 cm in acetone for 15 min, and ultrasonically washing for 5 min; washing with ultrapure water, etching with 3M HCl for 15 min, and performing ultrasonic treatment for 5 min; repeatedly washing with ultrapure water, washing with ethanol, and vacuum drying at 70-80 ℃ for 2-6 h to obtain pretreated foamed nickel serving as a substrate material for later use;
2) preparing a precursor solution:
(1) dissolving 1 g of high-molecular nonionic surfactant F127 in 3 g of absolute ethyl alcohol, and stirring for 10 min to obtain an absolute ethyl alcohol solution of F127;
(2) adding 1 g of phenolic resin with the mass fraction of 50% into the solution prepared in the step (1), and then mixing and stirring for 20 min;
(3) adding 0.047 g of stannous chloride and 2 g of absolute ethyl alcohol into the solution prepared in the step (2), stirring for 15 min, adding 0.2 g of ferric nitrate nonahydrate, and stirring for 15 min to ensure that the ratio of Fe to Sn is =2:1, wherein the dosage of the ferric nitrate nonahydrate is 0.2 times of the mass of F127;
(4) dissolving 0.43 g of anhydrous citric acid in 2 g of ethanol, adding the solution into the solution obtained in the step (3), and stirring for 30 min to obtain a precursor solution;
3) and soaking the pretreated foamed nickel in a precursor solution, taking out after 5 min, standing at room temperature for 12 h, curing at 100 ℃ for 24 h, and calcining at the heating rate of 1-5 ℃/min for 3 h in the nitrogen atmosphere at 800 ℃ to obtain the foamed nickel-loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode material (Fe: Sn =2: 1).
7. The preparation method of the foamed nickel supported porous carbon-coated nickel-tin-iron-nickel alloy electrode material as claimed in claim 6, wherein the addition amount of stannous chloride in the precursor solution is 0.024 g, so as to obtain the foamed nickel supported porous carbon-coated nickel-tin-iron-nickel alloy electrode (Fe: Sn = 4: 1), and the precursor solution is prepared by the following steps:
(1) dissolving 1 g of high-molecular nonionic surfactant F127 in 3 g of absolute ethyl alcohol, and stirring for 10 min to obtain an absolute ethyl alcohol solution of F127;
(2) adding 1 g of phenolic resin with the mass fraction of 50% into the solution prepared in the step (1), and then mixing and stirring for 20 min;
(3) adding 0.024 g of stannous chloride and 2-4 g of absolute ethyl alcohol into the solution prepared in the step (2), stirring for 15 min, adding 0.2 g of ferric nitrate nonahydrate, and stirring for 15 min to ensure that the ratio of Fe to Sn is = 4:1, wherein the dosage of the ferric nitrate nonahydrate is 0.2 times of the mass of F127;
(4) and (3) dissolving 0.43 g of anhydrous citric acid in 2 g of ethanol, adding the solution into the solution obtained in the step (3), and stirring for 30 min to obtain a precursor solution.
8. The preparation method of the foamed nickel supported porous carbon coated nickel-tin-iron-nickel alloy electrode material as claimed in claim 6, wherein stannous chloride is not added to the precursor solution to obtain the foamed nickel supported porous carbon coated iron-nickel alloy electrode.
9. Use of a foamed nickel supported porous carbon coated nickel tin-iron nickel alloy electrode material according to any one of claims 1 to 3 for electrocatalytic reduction of nitrate.
10. The use of the foamed nickel supported porous carbon coated nickel-tin-iron-nickel alloy electrode material of claim 9 for the electrocatalytic reduction of nitrate under the following conditions: 50 mg/L NO in 100 ml3 -Adding 0.05 mol/L sodium sulfate and 0-1 g/L sodium chloride into the sodium nitrate solution of the-N, adopting a three-electrode system, adopting a working electrode as a prepared foamed nickel-loaded porous carbon-coated nickel-tin-iron-nickel alloy electrode, adopting a platinum mesh electrode as a counter electrode and adopting a saturated calomel electrode as a reference electrode, and electrolyzing at the voltage of-1.3V.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110784849.2A CN113526622B (en) | 2021-07-12 | 2021-07-12 | Foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110784849.2A CN113526622B (en) | 2021-07-12 | 2021-07-12 | Foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113526622A true CN113526622A (en) | 2021-10-22 |
| CN113526622B CN113526622B (en) | 2022-12-27 |
Family
ID=78127493
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110784849.2A Active CN113526622B (en) | 2021-07-12 | 2021-07-12 | Foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113526622B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114210990A (en) * | 2021-12-02 | 2022-03-22 | 温州大学新材料与产业技术研究院 | Tin-iron alloy nanoparticle high-performance lithium and sodium storage material and application thereof |
| CN114346344A (en) * | 2021-12-02 | 2022-04-15 | 江苏大学 | Preparation method of carbon-coated high-melting-point foam metal network composite brazing interlayer |
| CN114560538A (en) * | 2022-01-25 | 2022-05-31 | 东北大学 | Foam nickel loaded carbon-embedded zero-valent iron cathode and method for preparing and degrading antibiotics |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61223189A (en) * | 1985-03-29 | 1986-10-03 | Tokuyama Soda Co Ltd | Production of cathode |
| CN109301249A (en) * | 2018-08-29 | 2019-02-01 | 济南大学 | A kind of nickel foam original position load SnO2Nanoparticle doped graphitic carbon composite material and preparation method thereof and application |
| CN110438528A (en) * | 2019-08-15 | 2019-11-12 | 上海工程技术大学 | A kind of modified nickel foam supported precious metal catalyst hydrogen-precipitating electrode and preparation method thereof |
| WO2020082443A1 (en) * | 2018-10-26 | 2020-04-30 | 苏州大学 | Fe-doped mos2 nanomaterial, preparation method therefor and use thereof |
| CN111498952A (en) * | 2020-04-09 | 2020-08-07 | 上海交通大学 | Porous carbon iron-nickel alloy foam nickel electrode and preparation method and application thereof |
| CN112354541A (en) * | 2019-07-24 | 2021-02-12 | 天津大学 | Co/CoO heterojunction electrocatalyst loaded on foamed nickel substrate and preparation method and application thereof |
| CN112473716A (en) * | 2020-11-30 | 2021-03-12 | 同济大学 | Nitrogen-doped mesoporous carbon-based nano material loaded with copper-nickel alloy particles and preparation method and application thereof |
| CN112626552A (en) * | 2021-01-07 | 2021-04-09 | 兰州大学 | Method for electrodepositing Ni-Fe-Sn-P alloy on surface of foamed nickel |
-
2021
- 2021-07-12 CN CN202110784849.2A patent/CN113526622B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61223189A (en) * | 1985-03-29 | 1986-10-03 | Tokuyama Soda Co Ltd | Production of cathode |
| CN109301249A (en) * | 2018-08-29 | 2019-02-01 | 济南大学 | A kind of nickel foam original position load SnO2Nanoparticle doped graphitic carbon composite material and preparation method thereof and application |
| WO2020082443A1 (en) * | 2018-10-26 | 2020-04-30 | 苏州大学 | Fe-doped mos2 nanomaterial, preparation method therefor and use thereof |
| CN112354541A (en) * | 2019-07-24 | 2021-02-12 | 天津大学 | Co/CoO heterojunction electrocatalyst loaded on foamed nickel substrate and preparation method and application thereof |
| CN110438528A (en) * | 2019-08-15 | 2019-11-12 | 上海工程技术大学 | A kind of modified nickel foam supported precious metal catalyst hydrogen-precipitating electrode and preparation method thereof |
| CN111498952A (en) * | 2020-04-09 | 2020-08-07 | 上海交通大学 | Porous carbon iron-nickel alloy foam nickel electrode and preparation method and application thereof |
| CN112473716A (en) * | 2020-11-30 | 2021-03-12 | 同济大学 | Nitrogen-doped mesoporous carbon-based nano material loaded with copper-nickel alloy particles and preparation method and application thereof |
| CN112626552A (en) * | 2021-01-07 | 2021-04-09 | 兰州大学 | Method for electrodepositing Ni-Fe-Sn-P alloy on surface of foamed nickel |
Non-Patent Citations (4)
| Title |
|---|
| CHEN, XIAOTONG: "Binderless and Oxygen Vacancies Rich FeNi/Graphitized Mesoporous Carbon/Ni Foam for Electrocatalytic Reduction of Nitrate", 《ENVIRONMENTAL SCIENCE & TECHNOLOGY》, vol. 54, no. 20, 29 September 2020 (2020-09-29), pages 13344 * |
| YIHUIWU: "Electrodeposition of self-supported Ni–Fe–Sn film on Ni foam: An efficient electrocatalyst for oxygen evolution reaction", 《ELECTROCHIMICA ACTA》, vol. 301, no. 1, 30 April 2019 (2019-04-30), pages 39 - 46 * |
| YIHUIWUA: "Potentiostatic electrodeposited of Ni–Fe–Sn on Ni foam served as an excellent electrocatalyst for hydrogen evolution reaction", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》, vol. 46, no. 53, 31 August 2021 (2021-08-31), pages 26930 - 26939, XP086699975, DOI: 10.1016/j.ijhydene.2021.05.189 * |
| 黄杨: "泡沫镍基复合材料的制备及电催化裂解水性能研究", 《中国优秀硕士学位论文库》, 31 December 2020 (2020-12-31) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114210990A (en) * | 2021-12-02 | 2022-03-22 | 温州大学新材料与产业技术研究院 | Tin-iron alloy nanoparticle high-performance lithium and sodium storage material and application thereof |
| CN114346344A (en) * | 2021-12-02 | 2022-04-15 | 江苏大学 | Preparation method of carbon-coated high-melting-point foam metal network composite brazing interlayer |
| CN114210990B (en) * | 2021-12-02 | 2024-05-17 | 温州大学新材料与产业技术研究院 | Tin-iron alloy nanoparticle high-performance lithium and sodium storage material and application thereof |
| CN114560538A (en) * | 2022-01-25 | 2022-05-31 | 东北大学 | Foam nickel loaded carbon-embedded zero-valent iron cathode and method for preparing and degrading antibiotics |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113526622B (en) | 2022-12-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113526622B (en) | Foamed nickel loaded porous carbon coated nickel tin-iron nickel alloy electrode material and preparation method and application thereof | |
| CN108840370B (en) | Transition metal oxide/nitrogen-doped ordered mesoporous carbon composite material and preparation method thereof | |
| CN110639525B (en) | Nickel oxide nanoflower/foamed nickel and electrodeposition preparation and application thereof | |
| CN110743566B (en) | Preparation method of monatomic catalyst | |
| CN111498952B (en) | Porous carbon iron-nickel alloy foam nickel electrode and preparation method and application thereof | |
| CN112626552B (en) | Method for electrodepositing Ni-Fe-Sn-P alloy on surface of foam nickel | |
| CN108315758B (en) | Catalyst for producing hydrogen by electrolyzing water and preparation method thereof | |
| CN111792705A (en) | Graphene oxide loaded carbon-based copper-nickel electrode, preparation method and application | |
| CN113279005A (en) | Cobalt doped MoS2/NiS2Preparation method of porous heterostructure material and application of material in electrocatalytic hydrogen evolution | |
| CN113716655A (en) | Ferronickel bimetal three-dimensional electrode particle filler and preparation method and application thereof | |
| CN114411175A (en) | Amorphous metal oxide modified p-BiVO4Preparation method and application of composite heterojunction | |
| CN112779586B (en) | Nickel phosphide with nanotube array structure and preparation method and application thereof | |
| CN113275027A (en) | Preparation and application of bimetallic phosphide derived from prussian blue analogue as template and growing on foamed nickel | |
| CN111807474A (en) | Preparation method of phosphorus-doped cobalt nanowire array for nitrate-nitrogen reduction in water | |
| CN112850860B (en) | Preparation method and application of nitrogen-doped ordered mesoporous carbon electrode | |
| CN113860438A (en) | Electrode for electro-chlorination assisted ammonia nitrogen oxidation and preparation method and application thereof | |
| CN113638005A (en) | Preparation method and application of efficient and bifunctional heterostructure full-electrolysis water-electricity catalyst | |
| CN112808289A (en) | Alginate-based metal monatomic catalyst and preparation method and application thereof | |
| CN113073354A (en) | Bismuth and ruthenium bimetal self-supporting electrocatalytic material, preparation method thereof and application thereof in nitrogen reduction | |
| CN104005075A (en) | Method for preparing carbon nano-tube modified palladium-loaded electrode through electrophoresis-chemical deposition | |
| CN114836770B (en) | Cobalt-based catalytic electrode for electrocatalytic reduction of nitrate radical into ammonia and preparation method thereof | |
| CN114774963B (en) | Nitrate radical reduction electrocatalyst and preparation method thereof | |
| CN114540862B (en) | Preparation method of electrode modified by combining efficient surface corrosion and graphitization | |
| CN114808005B (en) | Nickel-iron bimetallic phosphide electrode material with two-dimensional lamellar structure, preparation method thereof and application thereof in hydrogen production by water electrolysis | |
| CN113979518A (en) | Electrode for electrocatalytic oxidation of ammonia nitrogen and preparation method and application thereof |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |