CN114959771A - Nickel-based electrocatalyst and electrolytic cell for degrading formaldehyde wastewater by hydrogen production - Google Patents
Nickel-based electrocatalyst and electrolytic cell for degrading formaldehyde wastewater by hydrogen production Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
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Abstract
The invention discloses a nickel-based electrocatalyst and an electrolytic cell for producing hydrogen and degrading formaldehyde wastewater, which comprises the following specific steps: s11: mixing materials: adding a certain amount of nickel nitrate and potassium thiocyanate into a container, and uniformly mixing; s12: and (3) constant-temperature calcination: putting the mixture into a muffle furnace, and calcining at a constant temperature; s13: and (3) natural cooling: after constant-temperature calcination, naturally cooling the mixture to room temperature; s14: impurity removal: washing away the excess potassium thiocyanide by using deionized water; s15: and (3) drying: drying to obtain the nickel-based electrocatalyst; in the S12, the specific implementation of constant-temperature calcination is to control the muffle furnace to perform constant-temperature calcination at 450 ℃ for 2 hours, and the nickel-based electrocatalyst and the electrolytic cell for producing hydrogen and degrading formaldehyde wastewater disclosed by the invention have the effects of electrically oxidizing formaldehyde wastewater by the electrolytic cell and improving the hydrogen production efficiency.
Description
Technical Field
The invention relates to the technical field of wastewater degradation, in particular to a nickel-based electrocatalyst and an electrolytic cell for degrading formaldehyde wastewater by hydrogen production.
Background
Fossil fuels are consumed in large quantities as non-renewable resources, causing energy shortages and serious environmental pollution. Therefore, there is an urgent need to develop a renewable, environmentally friendly energy source, particularly a highly efficient clean energy source such as hydrogen. Hydrogen production by electrocatalytic decomposition of water is a clean and environmentally friendly method, but its slow anodic oxygen evolution reaction still limits its industrial applications.
Studies have shown that hydrogen production can be promoted by replacing the slow anodic oxygen evolution reaction with another oxidation reaction. Among them, formaldehyde is more easily oxidized than water molecules, thereby promoting the cathodic hydrogen evolution reaction. On the other hand, the harmfulness of formaldehyde is well known, and therefore, the present invention aims to improve the hydrogen production efficiency by directly using formaldehyde wastewater as an electrolyte while electrocatalytically oxidizing formaldehyde in the wastewater.
In the report, Korea Weiqing et al provided a device and method (CN202010339053.1) for treating formaldehyde-containing wastewater, which uses a titanium-based ruthenium dioxide electrode to treat formaldehyde in wastewater by electrocatalytic oxidation, but the cost is high. Li Yuejian et al provide the application of molybdenum phosphide in alkaline formaldehyde solution for catalytic hydrogen production (CN201710715999.1), the invention uses molybdenum phosphide in alkaline formaldehyde solution for catalytic hydrogen production, but the reaction needs strong alkali liquor and inert gas for protection, and the environment is not friendly.
Therefore, in order to obviously reduce the voltage of the electrolytic cell and improve the hydrogen production efficiency while degrading formaldehyde, the following scheme is provided.
Disclosure of Invention
The invention discloses a nickel-based electrocatalyst and an electrolytic cell for degrading formaldehyde wastewater by hydrogen production in a synergistic manner, and aims to solve the technical problems of low hydrogen production efficiency and unsatisfactory degradation effect of a formaldehyde solution in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a nickel-based electrocatalyst comprises the following specific steps:
s11: mixing materials: adding a certain amount of nickel nitrate and potassium thiocyanate into a container, and uniformly mixing;
s12: and (3) constant-temperature calcination: putting the mixture into a muffle furnace, and calcining at a constant temperature;
s13: and (3) natural cooling: after constant-temperature calcination, naturally cooling the mixture to room temperature;
s14: impurity removal: washing away the excess potassium thiocyanide by using deionized water;
s15: and (3) drying: drying to obtain the nickel-based electrocatalyst.
Fossil fuel is consumed in large quantity as non-renewable resource, which causes energy shortage and serious environmental pollution, therefore, the development of renewable and environment-friendly energy, especially high-efficiency clean energy such as hydrogen, is urgently needed, in the prior art, hydrogen production by electrocatalysis water is a clean and environment-friendly method, but the slow anodic oxygen evolution reaction still limits the industrial application, researches show that the hydrogen production can be promoted by replacing the slow anodic oxygen evolution reaction with other oxidation reactions, wherein, formaldehyde is easier to be oxidized compared with water molecules, and further promotes the cathodic hydrogen evolution reaction, on the other hand, the harmfulness of formaldehyde is well known, therefore, the invention aims to directly utilize formaldehyde wastewater as electrolyte to improve the hydrogen production efficiency, and electrocatalysis oxidation is to formaldehyde in the wastewater x As an electrocatalyst material, the voltage of the electrolytic cell is obviously reduced while the formaldehyde wastewater is electro-oxidized by the electrolytic cell, and the hydrogen production efficiency is improved, so that the method is an environment-friendly and energy-saving new hydrogen production strategy and has obvious practical application value.
In a preferred embodiment, in the S12, the constant temperature calcination is implemented by controlling a muffle furnace to perform constant temperature calcination at 450 ℃ for 2 hours;
the electrolytic cell for producing hydrogen and degrading formaldehyde wastewater in a synergic manner comprises the following specific steps:
s1: preparing an electrocatalyst: preparing a nickel-based electrocatalyst for later use;
s2: preparing an electrolyte: preparing electrolyte from PBS solution;
s3: preparing an electrode: using a nickel-based electrocatalyst to manufacture an electrode to form a two-electrode system;
s4: adding an electrocatalytic compound: adding a certain amount of electrocatalysis to carry out electrocatalysis;
s5: voltage application: applying a certain voltage to electrolyze the electrocatalytic product by using the electrode prepared in the electrode preparation;
in S2, the concentration of PBS in the electrolyte preparation is 0.01M;
in the step S4, the electro-catalytic substance added into the electro-catalytic substance is a certain amount of HCHO, wherein the concentration of HCHO is 2 mg/L;
in S3, the electrode preparation includes the following steps:
s31: preparing mixed slurry: mixing the prepared electrocatalyst with a certain amount of other materials to prepare the required mixed slurry;
s32: and (3) drying the slurry: the slurry was coated on a medium and dried at room temperature for 24 hours to give NiS x An electrode;
in the step S31, the specific implementation of the preparation of the mixed slurry is that the prepared nickel-based electrocatalyst, the prepared conductive carbon black and the polyvinylidene fluoride are mixed in a mass ratio of 8: 1: 1, mixing, dispersing in 1-methyl-2-pyrrolidone, and stirring to form uniform slurry;
in the step S32, the slurry is dried by coating the prepared slurry on a carbon fiber cloth with a coating area of 0.5cm by 0.5cm, and drying to obtain NiS x And an electrode.
The present invention will be further illustrated with reference to the following examples;
the first embodiment is as follows:
adding 1g of nickel nitrate and 10g of potassium thiocyanate into a container at room temperature, uniformly mixing, and then putting the mixture into the containerCalcining the mixture for 2 hours at the constant temperature of 450 ℃ in a muffle furnace, naturally cooling the calcined mixture to room temperature after 2 hours of calcination, washing off redundant potassium thiocyanate with deionized water, and drying the washed potassium thiocyanate to obtain the NiS x An electrocatalyst;
test example one:
as can be seen from FIG. 1, the characteristic peaks of the product prepared in the first example correspond to NiS and NiS 2 Example one preparation of products is NiS and NiS 2 The composite electrocatalyst of (a);
as can be seen from FIG. 2, NiS prepared in example one x The electrocatalyst consists of a mixture of large particles having a diameter of 2-10 μm and small particles having a diameter of 1 μm;
as can be seen from fig. 3, compared with the conventional PBS electrolytic cell, the cell voltage of the formaldehyde/PBS electrolytic cell is greatly reduced, and the current densities of the anode and the cathode are improved;
the test procedure was as follows:
NiS obtained in example one x The mass ratio of the electrocatalyst, the conductive carbon black and the polyvinylidene fluoride is 8: 1: 1, mixing, dispersing in 1-methyl-2-pyrrolidone, stirring to form uniform slurry, coating the slurry on carbon fiber cloth, and drying at room temperature for 24 hours to obtain NiS with a coating area of 0.5cm × 0.5cm x An electrode;
two sheets of NiS prepared by the above method x The electrodes are respectively used as a cathode and an anode, certain voltage is applied to the two electrode systems, electrocatalysis performance test is respectively carried out in 0.01MPBS and 0.01MPBS +2mg/LHCHO, as can be seen from figure 3, the addition of HCHO greatly reduces the overpotential of the electrolyzed water, and the cathode and the anode need to reach 10mA/cm 2 When the current density is high, the cell voltage of a PBS system is 3.55V, while the cell voltage of a PBS/HCHO system is only 3.10V, and the cell voltage is reduced by 0.45V, because the formaldehyde oxidation reaction replaces the slow four-electron water oxidation half reaction, the energy consumption of the electrolyzed water is reduced, and the hydrogen production is promoted.
The application steps of the nickel-based electrocatalyst and hydrogen production synergistic degradation formaldehyde wastewater electrolytic cell are as follows:
1. preparing an electrocatalyst, namely adding a certain amount of nickel nitrate and potassium thiocyanate into a container, uniformly mixing, putting the mixture into a muffle furnace, calcining at the constant temperature of 450 ℃ for 2 hours, naturally cooling to room temperature after calcining for 2 hours, washing off redundant potassium thiocyanate with deionized water, and drying to obtain the nickel-based electrocatalyst;
2. preparing electrolyte, and selecting proper electrolyte for later use;
3. preparation of electrode, NiS obtained x The mass ratio of the electrocatalyst, the conductive carbon black and the polyvinylidene fluoride is 8: 1: 1, mixing, dispersing in 1-methyl-2-pyrrolidone, stirring to form uniform slurry, coating the slurry on carbon fiber cloth, and drying at room temperature for 24 hours to obtain NiS with a coating area of 0.5cm × 0.5cm x An electrode;
two sheets of NiS obtained as described above x The electrodes are respectively used as a cathode and an anode, certain voltage is applied to the two-electrode system, and a certain amount of PBS and HCHO are added for carrying out electrocatalysis performance test, wherein the addition of HCHO greatly reduces the overpotential of the electrolyzed water, and because the slow four-electron water oxidation half reaction is replaced by the formaldehyde oxidation reaction, the energy consumption of the electrolyzed water is reduced, and the hydrogen production is promoted.
By using a nickel-based electrocatalyst as an electrode material, forming a two-electrode electrolytic cell, adding a certain amount of PBS and HCHO and adopting an HCHO/PBS electrolytic system, compared with the traditional electrolytic water system, the electrolytic water system effectively reduces the cell voltage, efficiently electrolyzes water, and oxidatively degrades formaldehyde pollutants.
From the above, a nickel-based electrocatalyst comprises the following specific steps:
s11: mixing materials: adding a certain amount of nickel nitrate and potassium thiocyanate into a container, and uniformly mixing;
s12: and (3) constant-temperature calcination: putting the mixture into a muffle furnace, and calcining at a constant temperature;
s13: and (3) natural cooling: calcining at constant temperature, and naturally cooling the mixture to room temperature;
s14: impurity removal: washing away the excess potassium thiocyanide by using deionized water;
s15: and (3) drying: drying to obtain the nickel-based electrocatalyst. The nickel-based electrocatalyst and the electrolytic cell for degrading the formaldehyde wastewater by the hydrogen production cooperation provided by the invention have the technical effects of electrically oxidizing the formaldehyde wastewater by the electrolytic cell and simultaneously improving the hydrogen production efficiency.
Drawings
FIG. 1 is an overall flow chart of the nickel-based electrocatalyst and an electrolytic cell for producing hydrogen and degrading formaldehyde wastewater in a synergic manner, which is provided by the invention.
FIG. 2 is a flow chart of the preparation of the nickel-based electrocatalyst and the electrocatalyst of the electrolytic cell for producing hydrogen and degrading formaldehyde wastewater in a synergic manner.
FIG. 3 is a flow chart of the preparation of an electrode of an electrolytic cell for degrading formaldehyde wastewater by the cooperation of nickel-based electrocatalyst and hydrogen generation.
FIG. 4 shows a nickel-based electrocatalyst NiS prepared in an embodiment of an electrolytic cell for producing hydrogen and degrading formaldehyde wastewater in coordination with a nickel-based electrocatalyst x X-ray diffraction (XRD) pattern of (a).
FIG. 5 shows NiS prepared in the first embodiment of the invention, which is an electrolytic cell for producing hydrogen and degrading formaldehyde wastewater with nickel-based electrocatalyst x Scanning Electron Microscope (SEM) images of the electrocatalyst.
FIG. 6 shows NiS prepared in the first embodiment of the invention, which is an electrolytic cell for producing hydrogen and degrading formaldehyde wastewater with nickel-based electrocatalyst x Electrocatalysis performance test patterns of the electrocatalysis in 0.01MPBS and 0.01MPBS +2mg/LHCHO respectively.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
The invention discloses a nickel-based electrocatalyst and an electrolytic cell for producing hydrogen and degrading formaldehyde wastewater, which are mainly applied to the scene of wastewater electrolysis.
Referring to fig. 2, a nickel-based electrocatalyst includes the following specific steps:
s11: mixing materials: adding a certain amount of nickel nitrate and potassium thiocyanate into a container, and uniformly mixing;
s12: and (3) constant-temperature calcination: putting the mixture into a muffle furnace, and calcining at a constant temperature;
s13: and (3) natural cooling: after constant-temperature calcination, naturally cooling the mixture to room temperature;
s14: impurity removal: washing away the excess potassium thiocyanide by using deionized water;
s15: and (3) drying: drying to obtain the nickel-based electrocatalyst.
Referring to fig. 2, in a preferred embodiment, in S12, the constant temperature calcination is performed by controlling a muffle furnace to perform constant temperature calcination at 450 ℃ for 2 hours.
Referring to fig. 1, the electrolytic cell for producing hydrogen and degrading formaldehyde wastewater in coordination comprises the following specific steps:
s1: preparing an electrocatalyst: preparing a nickel-based electrocatalyst for later use;
s2: preparing an electrolyte: preparing electrolyte by using PBS as base solution;
s3: preparing an electrode: using a nickel-based electrocatalyst to manufacture an electrode to form a two-electrode system;
s4: adding an electrocatalytic compound: adding a certain amount of electrocatalysis to carry out electrocatalysis;
s5: voltage application: and applying a certain voltage to electrolyze the electrocatalytic product by the electrode prepared in the electrode preparation.
Referring to fig. 1, in a preferred embodiment, in S2, the concentration of PBS in the electrolyte solution during electrolyte solution preparation is 0.01M.
Referring to FIG. 1, in a preferred embodiment, in S4, the electrocatalytic compound is added to the electrocatalytic compound in an amount of HCHO, wherein the concentration of HCHO is 2 mg/L.
Referring to fig. 3, in a preferred embodiment, in S3, the electrode preparation includes the following specific steps:
s31: preparing mixed slurry: mixing the prepared electrocatalyst with a certain amount of other materials to prepare the required mixed slurry;
s32: and (3) drying the slurry: the slurry was coated on a medium and dried at room temperature for 24 hours to give NiS x And an electrode.
Referring to fig. 3, in a preferred embodiment, in S31, the slurry mixture is prepared by mixing the prepared nickel-based electrocatalyst and conductive carbon black with polyvinylidene fluoride in a mass ratio of 8: 1: 1, mixing, dispersing in 1-methyl-2-pyrrolidone, and stirring to form uniform slurry.
Referring to fig. 3, in a preferred embodiment, in S32, the slurry is dried by coating the prepared slurry on a carbon fiber cloth with a coating area of 0.5cm by 0.5cm, and drying to obtain NiS x And an electrode.
The present invention will be further described with reference to the following examples.
The first embodiment is as follows:
adding 1g of nickel nitrate and 10g of potassium thiocyanate into a container at room temperature, uniformly mixing, then putting the mixture into a muffle furnace, calcining at the constant temperature of 450 ℃ for 2 hours, naturally cooling to room temperature after calcining for 2 hours, washing off redundant potassium thiocyanate with deionized water, and drying to obtain the NiS x An electrocatalyst;
test example one:
as can be seen from FIG. 1, the characteristic peaks of the product prepared in the first example correspond to NiS and NiS 2 Example one preparation of products is NiS and NiS 2 The composite electrocatalyst of (a);
as can be seen from FIG. 2, NiS prepared in example one x The electrocatalyst consists of a mixture of large particles having a diameter of 2-10 μm and small particles having a diameter of 1 μm;
as can be seen in FIG. 3, NiS x Compared with the traditional PBS electrolytic cell, the electrocatalyst of the formaldehyde/PBS electrolytic cell greatly reduces the cell voltage and improves the current density of the anode and the cathode;
the test procedure was as follows:
NiS obtained in example one x The mass ratio of the electrocatalyst, the conductive carbon black and the polyvinylidene fluoride is 8: 1: 1 mixing, dispersing in 1-methyl-2-pyrrolidone, stirring to form uniform slurry, coating the slurry on carbon fiber cloth, and drying at room temperature for 24 hr to obtain a coating area of 0.5cm × 0.5cmNiS x An electrode;
two sheets of NiS prepared by the above method x The electrodes are respectively used as a cathode and an anode, certain voltage is applied to the two electrode systems, electrocatalysis performance test is respectively carried out in 0.01MPBS and 0.01MPBS +2mg/LHCHO, as can be seen from figure 3, the addition of HCHO greatly reduces the overpotential of the electrolyzed water, and the cathode and the anode need to reach 10mA/cm 2 When the current density is high, the cell voltage of a PBS system is 3.55V, while the cell voltage of a PBS/HCHO system is only 3.10V, and the cell voltage is reduced by 0.45V, because the formaldehyde oxidation reaction replaces slow four-electron water oxidation half reaction, the energy consumption of the electrolyzed water is further reduced, and the hydrogen production is promoted, therefore, the design is energy-saving, and pollutants are degraded while the water is electrolyzed at low pressure and high efficiency.
The working principle is as follows: the application steps of the nickel-based electrocatalyst and hydrogen production synergistic degradation formaldehyde wastewater electrolytic cell are as follows:
4. preparing an electrocatalyst, namely adding a certain amount of nickel nitrate and potassium thiocyanate into a container, uniformly mixing, putting the mixture into a muffle furnace, calcining at the constant temperature of 450 ℃ for 2 hours, naturally cooling to room temperature after calcining for 2 hours, washing off redundant potassium thiocyanate with deionized water, and drying to obtain the nickel-based electrocatalyst;
5. preparing electrolyte, and selecting proper electrolyte for later use;
6. preparation of electrode, NiS obtained x The mass ratio of the electrocatalyst, the conductive carbon black and the polyvinylidene fluoride is 8: 1: 1, mixing, dispersing in 1-methyl-2-pyrrolidone, stirring to form uniform slurry, coating the slurry on carbon fiber cloth, and drying at room temperature for 24 hours with a coating area of 0.5cm × 0.5cm to obtain NiS x An electrode;
7. two sheets of NiS obtained as described above x The electrodes are respectively used as a cathode and an anode, certain voltage is applied to the two-electrode system, and a certain amount of PBS and HCHO are added for carrying out electrocatalysis performance test, wherein the addition of HCHO greatly reduces the overpotential of the electrolyzed water, because the slow four-electron water oxidation half reaction is replaced by formaldehyde oxidation reaction, the energy consumption of the electrolyzed water is further reduced, and the hydrogen production is promoted, therefore, the design is energy-savingThe method improves the hydrogen production efficiency and degrades pollutants while electrolyzing water at low pressure and high efficiency.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A nickel-based electrocatalyst, characterized by comprising the following specific steps:
s11: mixing materials: adding a certain amount of nickel nitrate and potassium thiocyanate into a container, and uniformly mixing;
s12: and (3) constant-temperature calcination: putting the mixture into a muffle furnace, and calcining at a constant temperature;
s13: and (3) natural cooling: after constant-temperature calcination, naturally cooling the mixture to room temperature;
s14: impurity removal: washing away the excess potassium thiocyanide by using deionized water;
s15: and (3) drying: drying to obtain the nickel-based electrocatalyst.
2. The nickel-based electrocatalyst according to claim 1, wherein in S12, the isothermal calcination is performed by controlling a muffle furnace to perform isothermal calcination at 450 ℃ for 2 hours.
3. The electrolytic cell for producing hydrogen and degrading formaldehyde wastewater is characterized by comprising the following specific steps:
s1: preparing an electrocatalyst: preparing a nickel-based electrocatalyst for later use;
s2: preparing an electrolyte: preparing electrolyte by taking Phosphate Buffered Saline (PBS) as base solution;
s3: preparing an electrode: using a nickel-based electrocatalyst to manufacture an electrode to form a two-electrode system;
s4: adding an electrocatalytic compound: adding a certain amount of electrocatalysis to carry out electrocatalysis;
s5: voltage application: applying a certain voltage to electrolyze the electrocatalytic product by the electrode prepared in the electrode preparation;
4. the electrolytic cell for the hydrogen-producing synergistic degradation of the formaldehyde wastewater as claimed in claim 3, wherein in the S2, the concentration of PBS in the electrolyte during the preparation of the electrolyte is 0.01M.
5. The electrolytic cell for hydrogen production and synergistic degradation of formaldehyde wastewater as claimed in claim 3, wherein the electrocatalytic compound added to the electrocatalytic compound in S4 is an amount of formaldehyde, namely HCHO, wherein the concentration of HCHO is 2 mg/L.
6. The electrolytic cell for hydrogen production and formaldehyde wastewater synergistic degradation as claimed in claim 3, wherein in the step S3, the electrode preparation comprises the following specific steps:
s31: preparing mixed slurry: mixing the prepared electrocatalyst with a certain amount of other materials to prepare required mixed slurry;
s32: and (3) drying the slurry: the slurry was coated on a medium and dried at room temperature for 24 hours to give NiS x And an electrode.
7. The electrolytic cell for hydrogen production and synergistic degradation of formaldehyde wastewater as claimed in claim 6, wherein in the step S31, the specific implementation manner of the preparation of the mixed slurry is that the prepared nickel-based electrocatalyst, conductive carbon black and polyvinylidene fluoride are mixed in a mass ratio of 8: 1: 1, mixing, dispersing in 1-methyl-2-pyrrolidone, and stirring to form uniform slurry.
8. The electrolytic cell for hydrogen production and formaldehyde wastewater degradation as claimed in claim 7, wherein in the step S32, the slurry is dried by coating the prepared slurry on carbon fiber cloth with a coating area of 0.5cm by 0.5cm to obtain NiS x And an electrode.
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