CN113511710A - Electrode active material for capacitance adsorption of lead ions and preparation method and application thereof - Google Patents

Electrode active material for capacitance adsorption of lead ions and preparation method and application thereof Download PDF

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CN113511710A
CN113511710A CN202110583322.3A CN202110583322A CN113511710A CN 113511710 A CN113511710 A CN 113511710A CN 202110583322 A CN202110583322 A CN 202110583322A CN 113511710 A CN113511710 A CN 113511710A
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active material
electrode active
lead ions
carbon
temperature
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CN113511710B (en
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龚成云
周宏建
汪国忠
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Anhui Zhongkesona New Material Technology Co ltd
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Anhui Zhongkesona New Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/469Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
    • C02F1/4691Capacitive deionisation

Abstract

The invention discloses an electrode active material for capacitance adsorption of lead ions, a preparation method and application thereof, wherein the electrode active material comprises a carbon foam framework, a carbon nano tube and heptaferric octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; and the heptaferric octasulfide is encapsulated in the carbon nanotube. The preparation method comprises the steps of preparing a carbon foam precursor, carbonizing and vulcanizing; the carbon foam precursor is prepared from melamine foam, an iron source and urea serving as raw materials by a hydrothermal method or an oil bath method. The electrode active material for adsorbing lead ions by the capacitor can be used for adsorbing or removing lead ions in a solution, and has great application potential in the practical treatment of lead ions in wastewater.

Description

Electrode active material for capacitance adsorption of lead ions and preparation method and application thereof
Technical Field
The invention belongs to the technical field of capacitive deionization, and particularly relates to an electrode active material for capacitive adsorption of lead ions, and a preparation method and application thereof.
Background
Heavy metals are recognized as one of the most hazardous contaminants due to their own undegradability and enrichment. Among them, heavy metal lead (Pb) is one of the most common public hazards in drinking water, and is widely derived from battery manufacturing, metal plating, mining, and the like. If a person is exposed to lead-related contaminants or drinking water for a long period of time, the immune system, nervous system, liver, etc. of the person may be damaged.
At present, methods for removing heavy metals from wastewater include membrane filtration, ion exchange, chemical precipitation, adsorption, and electrochemical methods. However, these methods have their own limitations. For example, the application is hindered by the disadvantages of high cost, complex operation, more side reactions, high energy consumption and the like.
The Capacitive Deionization (CDI) technology is a new water treatment technology, and its basic principle is to use a low electric field to adsorb charged ions onto electrodes, so as to remove the charged ions from aqueous solution. Compared with the processes such as membrane filtration, chemical precipitation and the like, the capacitive deionization technology has the advantages of high energy efficiency, simplicity in operation, low cost and the like. Moreover, the electrode can regenerate the electrode material in situ through short circuit or reverse connection of a power supply, thereby realizing the recovery of heavy metal and the recycling of the electrode material, and simultaneously reducing the problems of dirt and scaling to the minimum. In aqueous CDI treatment solutions, the performance of CDI tends to depend largely on the properties of the electrode active material, and therefore, the selection of a suitable electrode active material is a key step in its development.
Disclosure of Invention
Based on the technical problems, the invention provides an electrode active material for capacitance adsorption of lead ions, and a preparation method and application thereof. The electrode active material can be used as an electrode material in a capacitive deionization device, has a good electric adsorption effect on heavy metal lead ions, and has a great application potential in the practical treatment of the lead ions in wastewater.
The technical scheme of the invention is as follows:
the invention provides an electrode active material for adsorbing lead ions by a capacitor, which comprises a carbon foam framework, carbon nano tubes and heptaferric octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; and the heptaferric octasulfide is encapsulated in the carbon nanotube.
The invention also provides a preparation method of the electrode active material for capacitive adsorption of lead ions, which comprises the steps of preparing a carbon foam precursor, carbonizing and vulcanizing; the carbon foam precursor is prepared from melamine foam, an iron source and urea serving as raw materials by a hydrothermal method or an oil bath method.
Preferably, the hydrothermal method for preparing the carbon foam precursor specifically comprises the following steps: mixing melamine foam, an iron source and urea, adding deionized water, stirring until the solution is clear, reacting at the temperature of 100-120 ℃ for 12-24h, and cooling to obtain a carbon foam precursor; the mass ratio of the iron source to the urea is 1: 1-3; the mass volume ratio of the iron source to the melamine foam is g/cm3The value is 1: 100-250.
Preferably, the oil bath method for preparing the carbon foam precursor specifically comprises the following steps: mixing melamine foam, an iron source and urea, reacting for 12-24h under an oil bath at the temperature of 80-100 ℃, and cooling to obtain a carbon foam precursor; the mass ratio of the iron source to the urea is 1: 1-3; the mass volume ratio of the iron source to the melamine foam is g/cm3The value is 1: 100-250.
The melamine foam used in the present invention is a commercial foam, and is commercially available from conventional sources.
Preferably, the iron source is a ferric salt or a ferrous salt; more preferably, the iron source is selected from the group consisting of ferric nitrate, ferric sulfate, ferric chloride, or a combination of one or more thereof. These iron salts may be hydrated or non-hydrated salts.
Preferably, the carbonization temperature is 700-850 ℃ and the carbonization time is 1-4 h; more preferably, the temperature is raised to the carbonization temperature at a temperature raising rate of 1 to 8 ℃/min at the time of carbonization.
The carbonization is carried out in an oxygen-free atmosphere, wherein the oxygen-free atmosphere is inert gas or nitrogen atmosphere; preferably, the carbonization is performed under a nitrogen atmosphere. After carbonization, the mixture was cooled to room temperature.
Preferably, during vulcanization, sulfur powder is used as a vulcanizing agent, the vulcanization temperature is 550-700 ℃, and the vulcanization time is 1-4 h; the adding amount of the vulcanizing agent is 5-7 times of the mass of the carbonized product; more preferably, the temperature is raised from room temperature to the vulcanization temperature at a temperature raising rate of 1 to 8 ℃/min at the time of vulcanization.
Preferably, the carbon foam precursor is subjected to a freezing, freeze-drying process prior to carbonization; the freezing temperature is-20 ℃ to-80 ℃, and the freezing time is 24-48 h; the freeze drying temperature is-60 deg.C to-80 deg.C, and the freeze drying time is 48-72 h.
The invention also provides application of the electrode active material for lead ion adsorption by capacitance or the electrode active material for lead ion adsorption by capacitance prepared by the preparation method, which is used for adsorbing or removing lead ions in a solution.
Preferably, when the capacitive deionization device is applied, the capacitive electrode active material for adsorbing lead ions is used as a negative electrode active material, activated carbon is used as a positive electrode active material, the asymmetric capacitive deionization device is constructed, and the asymmetric capacitive deionization device is used for adsorbing or removing lead ions in a solution.
Has the advantages that:
the invention provides an electrode active material, which comprises a carbon foam framework, carbon nano tubes and heptaferric octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; and the heptaferric octasulfide is encapsulated in the carbon nanotube. The electrode active material is used as a negative electrode active material, the active carbon is used as a positive electrode active material, and the asymmetric capacitive deionization device is constructed, so that the high-efficiency adsorption of heavy metal lead ions in the solution can be realized.
Compared with the existing carbon material, the electrode active material provided by the invention has higher adsorption capacity, and can effectively solve the problem of limited adsorption capacity of the carbon material. And in addition, when the method is applied, the operation is simple, the energy consumption is low, extra treatment is not needed during adsorption, and the method is environment-friendly.
Drawings
FIG. 1 shows the carbonized product (CF/CNT/Fe) obtained in example 13C) And final product (CF/CNT/Fe)7S8) XRD pattern of (a).
FIG. 2 shows the carbonized product (CF/CNT/Fe) obtained in example 13C) SEM image of (d).
FIG. 3 shows the final product (CF/CNT/Fe) obtained in example 17S8) SEM image of (d).
FIG. 4 shows the final product (CF/CNT/Fe) obtained in example 17S8) Wherein: (a) fe 2p, (b) S2p,(c)C 1s,(d)N 1s。
FIG. 5(a) shows the final product (CF/CNT/Fe) obtained in example 17S8) The lead ion removal performance of the solution with lead ion concentration of 100ppm under different voltages; (b) is CF/CNT/Fe obtained in example 1 at a voltage of 1.2V7S8The material is compared with lead ion removal capacity of lead ion solutions with different concentrations.
FIG. 6 shows the result of the formation of (CF/CNT/Fe) film of example 1 at 1.2V7S8) The XRD pattern of the electrode slice prepared as the active material before and after the electrode slice carries out electro-adsorption on 100ppm lead ion solution.
FIG. 7 shows the result of example 1 (CF/CNT/Fe) at 1.2V7S8) XPS measured on an electrode sheet obtained as an active material after the electrode sheet electrically adsorbs 100ppm of a lead ion solution, (a) Pb 4f, and (b) S2 p.
FIG. 8 CF/CNT/Fe obtained by carbonization in example 13C and example 1 sulfurization of the obtained CF/CNT/Fe7S8The adsorption capacity of the product to lead ions in a solution with lead ion concentration of 100ppm is compared.
FIG. 9, final product (CF/CNT/FeS) for comparative example 22) XRD pattern of (a);
FIG. 10, final product (CF/CNT/FeS) for comparative example 22) SEM picture of (1);
FIG. 11 shows the final product (CF/CNT/Fe) obtained in example 1 in a lead ion solution of 200ppm at a voltage of 1.2V7S8) And comparative example 2 to obtain the final product (CF/CNT/FeS)2) Comparison of lead adsorption capacity.
FIG. 12 shows CF/CNT/Fe obtained in example 17S8The material has the capacity of electric adsorption to lead ions in the process of circulating 16 times under the lead ion concentration of 10ppm solution.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
The invention provides an electrode active material for adsorbing lead ions by a capacitor, which comprises a carbon foam framework, carbon nano tubes and heptaferric octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; and the heptaferric octasulfide is encapsulated in the carbon nanotube. CF/CNT/Fe for electrode active material for capacitive adsorption of lead ions according to the present invention7S8Wherein "CF" represents carbon foam, "CNT" is carbon nanotube, "Fe7S8"is heptairon octasulfide and"/"indicates the load.
In the electrode active material for lead ion adsorption by capacitance, the heptaferric octasulfide is packaged in the carbon nano tube growing on the surface of the carbon foam framework, so that the stability of the heptaferric octasulfide can be enhanced, and the improvement of the cycling stability of the lead ion adsorption by electricity is facilitated.
The invention also provides a preparation method of the electrode active material for capacitive adsorption of lead ions, which comprises the steps of preparing a carbon foam precursor, carbonizing and vulcanizing; the carbon foam precursor is prepared by using melamine foam, an iron source and urea as raw materials and performing a hydrothermal method or an oil bath method. The carbonized product is CF/CNT/Fe3C denotes "CF" denotes carbon foam, "CNT" denotes carbon nanotube, "Fe3C "represents iron carbide and"/"represents a load.
The electrode active material for adsorbing lead ions by the capacitor is prepared by taking melamine foam, an iron source and urea as raw materials, preparing a carbon foam precursor by a hydrothermal method or an oil bath method, and then carbonizing and vulcanizing. Wherein, the melamine foam is used for providing a carbon foam framework structure; the function of the iron source: on one hand, the catalyst is used as a catalyst after the catalyst is subjected to carbonization and reduction, and carbon in melamine bubbles and urea is catalyzed to generate carbon nano tubes; in another aspect, iron is provided for the sulfidation reaction to produce heptaferric octasulfide; the function of urea: on one hand, the carbon source is favorable for the growth of the carbon nano tube; on the other hand, as a nitrogen source, sufficient nitrogen is provided for preparation of the nitrogen-doped carbon base material, which is beneficial to the capacity adsorption performance of the finally prepared electrode active material.
The electrode active material for capacitive adsorption of lead ions and the electrode active material for capacitive adsorption of lead ions prepared by the method can be used for adsorption or removal of lead ions in a solution. Preferably, the lead ion concentration in the lead ion-containing solution is treated to be 10-300 mg/L.
When the electrode active material is applied, the electrode active material is used as a negative electrode active material, the active carbon is used as a positive electrode active material, a negative electrode plate and a positive electrode plate are respectively prepared, and then the asymmetric capacitance deionization device is constructed.
The raw materials of the negative electrode plate, except for the active material which adopts the electrode active material for capacitance adsorption of lead ions, can adopt conventional raw materials, and can adopt but not limited to the following raw materials: the conductive agent in the electrode slurry is selected from one of acetylene black, carbon black and Ketjen black; the adhesive is selected from one of polyvinylidene fluoride, polytetrafluoroethylene and naphthol; the current collector is selected from one of carbon paper, carbon felt and titanium sheet.
The raw material of the positive plate, the active material is activated carbon, and the other raw materials can adopt conventional raw materials, and can adopt but not limited to the following raw materials: the conductive agent in the electrode slurry is selected from one of acetylene black, carbon black and Ketjen black; the adhesive is selected from one of polyvinylidene fluoride, polytetrafluoroethylene and naphthol; the current collector is selected from one of carbon paper, carbon felt and titanium sheet.
The method for preparing the negative plate and the positive plate adopts a conventional method, and can adopt but not limited to the following methods: adding the positive electrode/negative electrode active material, the adhesive and the conductive agent into the solvent according to the ratio of 80-95:10:10, and uniformly stirring to obtain electrode slurry; uniformly coating the stirred electrode slurry on the surface of a current collector, wherein the coating effective area is 2 multiplied by 2cm2(ii) a And (4) drying in an oven at 70 ℃ to obtain the positive/negative plate.
Example 1
An electrode active material for adsorbing lead ions by a capacitor comprises a carbon foam framework, carbon nano tubes and heptaferric octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; the heptairon octasulfide is encapsulated in the carbon nanotube.
The preparation method comprises
(1) Preparing a carbon foam precursor by a hydrothermal method: dissolving 0.25g of ferric nitrate nonahydrate and 0.5g of urea in 60mL of deionized water, pouring into a high-pressure reaction kettle, mixing, and adding 25cm of solution3Continuously heating the melamine foam in an oven at 110 ℃ for 12 hours, and taking out the melamine foam after natural cooling to obtain a carbon foam precursor;
(2) freezing the carbon foam precursor in a refrigerator at-40 ℃ for up to 24 hours, and then transferring the carbon foam precursor to a freeze dryer for drying at-70 ℃ for up to 48 hours;
(3) carbonizing: heating the treated carbon foam precursor to 800 ℃ at the heating rate of 5 ℃/min and maintaining for 2 hours, cooling to room temperature after carbonization to obtain CF/CNT/Fe3C;
(4) And (3) vulcanization: mixing CF/CNT/Fe3Mixing C and sulfur powder at a mass ratio of 1:5, heating from room temperature to 600 ℃ at a heating rate of 5 ℃/min, maintaining for 2 hours, and naturally cooling to obtain the final product CF/CNT/Fe7S8
The intermediate and final products prepared in example 1 were verified and characterized:
FIG. 1 shows the carbonized product (CF/CNT/Fe) obtained in example 13C) And final product (CF/CNT/Fe)7S8) XRD pattern of (a).
FIGS. 2 and 3 are graphs showing the carbonized product (CF/CNT/Fe) obtained in example 13C) And final product (CF/CNT/Fe)7S8) SEM picture of (1); as can be seen from fig. 3, the final product, that is, the electrode active material for capacitive adsorption of lead ions according to the present invention, contains carbon nanotubes and heptaferric octasulfide encapsulated in the carbon nanotubes.
FIG. 4 shows the final product obtained in example 1 (CF/CNT/Fe)7S8) High resolution of (2); as can be seen from FIG. 4, the final product (CF/CNT/Fe)7S8) Is made of Fe7S8Component and N, S co-doped carbon structures.
Example 2
An electrode active material for adsorbing lead ions by a capacitor comprises a carbon foam framework, carbon nano tubes and heptaferric octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; the heptairon octasulfide is encapsulated in the carbon nanotube.
The preparation method comprises
(1) Preparing a carbon foam precursor by an oil bath method: 0.2g of ferric chloride tetrahydrate and 0.5g of urea were uniformly mixed, followed by charging into a 45cm container3Reacting melamine foam for 12 hours in an oil bath at the temperature of 80 ℃, and taking out after natural cooling to obtain a carbon foam precursor;
(2) freezing the carbon foam precursor in a refrigerator at-20 ℃ for 48 hours, and then transferring the carbon foam precursor to a freeze dryer for drying at-60 ℃ for 60 hours;
(3) carbonizing: heating the treated carbon foam precursor to 800 ℃ at the heating rate of 5 ℃/min and maintaining for 2 hours, cooling to room temperature after carbonization to obtain CF/CNT/Fe3C;
(4) And (3) vulcanization: mixing CF/CNT/Fe3Mixing C and sulfur powder at a mass ratio of 1:5, heating from room temperature to 600 ℃ at a heating rate of 5 ℃/min for 2 hours, and naturally cooling to obtain the final product CF/CNT/Fe7S8
Example 3:
an electrode active material for adsorbing lead ions by a capacitor comprises a carbon foam framework, carbon nano tubes and heptaferric octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; the heptairon octasulfide is encapsulated in the carbon nanotube.
The preparation method comprises
(1) Preparing a carbon foam precursor by a hydrothermal method: dissolving 0.25g of ferric chloride tetrahydrate and 0.5g of urea in 70mL of deionized water, pouring into a high-pressure reaction kettle, mixing, and adding 58cm3Continuously heating the melamine foam in an oven at 100 ℃ for 24 hours, and taking out the melamine foam after natural cooling to obtain a carbon foam precursor;
(2) freezing the carbon foam precursor in a refrigerator at-80 ℃ for 24 hours, and then transferring the carbon foam precursor to a freeze dryer for drying at-80 ℃ for 60 hours;
(3) carbonizing: will be provided withHeating the sample to 700 ℃ at the heating rate of 7 ℃/min for 4 hours by using the treated carbon foam precursor, cooling to room temperature after carbonization, and obtaining CF/CNT/Fe3C;
(4) And (3) vulcanization: mixing CF/CNT/Fe3Mixing C and sulfur powder at a mass ratio of 1:7, heating from room temperature to 700 ℃ at a heating rate of 2 ℃/min for 3 hours, and naturally cooling to obtain the final product CF/CNT/Fe7S8
Example 4
Same as example 1 except that the iron source was changed from "iron nitrate nonahydrate" to "iron sulfate".
And (3) performance testing:
preparing a negative plate: the final product obtained in example 1 (CF/CNT/Fe)7S8) Pouring the electrode active material, the conductive agent Keqin black and the adhesive polyvinylidene fluoride into a dimethyl formamide solution according to the mass ratio of 8:1:1, uniformly stirring and mixing to obtain electrode slurry, and uniformly coating a proper amount of the electrode slurry on the surface of a current collector titanium sheet (coating effective area is 2 multiplied by 2 cm)2) Finally, drying the electrode slices in an oven at 70 ℃ to obtain the required electrode slices; preparing a positive plate: the active carbon is used as an anode active material and is prepared by the same method as the cathode sheet.
Capacitive deionization device: assembling the negative plate and the positive plate into an asymmetric capacitance deionization device;
the capacitive deionization device is used for adsorbing/removing lead ions in a solution, and the capacitive deionization device is specifically operated as follows: and (3) conveying the solution containing lead ions into an asymmetric capacitance deionization device through a peristaltic pump, and then applying voltage to carry out electro-adsorption.
1. Adsorption Performance test
To verify the final product (CF/CNT/Fe) produced by the present invention7S8) The adsorption performance of the adsorbent on lead ions is tested, and the removal effect of the adsorbent on lead ions in a solution with the lead ion concentration of 100ppm is tested under different voltages.
FIG. 5(a) is the final product (CF/CNT/Fe) obtained in example 17S8) Lead ion concentration of 100ppm solution under different voltagesRemoving the performance; it can be seen that as the voltage increases, the amount of lead ions removed increases.
FIG. 5(b), the final product (CF/CNT/Fe) obtained in example 1 at 1.2V7S8) Comparing the lead ion removal capacity of lead ion solutions with different concentrations; it can be seen that at a voltage of 1.2V, the electric adsorption performance for lead ions was saturated when the lead ion concentration reached 200 ppm.
FIG. 6 is an XRD spectrum before and after adsorption of 100ppm lead ion solution by the electrode sheet at 1.2V; it can be seen that in CF/CNT/Fe7S8After the electrode electrically adsorbs lead ions, a PbS phase appears.
FIG. 7 is an XPS spectrum of the electrode sheet before and after adsorption of 100ppm lead ion solution at 1.2V; the presence of PbS is further demonstrated.
To further illustrate the capacity adsorption performance of the electrode active material of the present invention to lead ions, the following comparative examples are provided.
Comparative example 1 carbonized product (CF/CNT/Fe) obtained in example 13C) Preparing a negative plate and a positive plate by the same method for a negative active material and active carbon as a positive active material, and assembling the negative plate and the positive plate into an asymmetric capacitance deionization device; the solution containing lead ions was transferred to the capacitive deionization apparatus described in comparative example 1 by a peristaltic pump, and voltage was applied thereto for electro-adsorption.
FIG. 8 is a graph showing a comparison of adsorption capacities of the electrode active materials described in example 1 and comparative example 1 for lead ions in a solution having a lead ion concentration of 100 ppm; it can be seen that the same as CF/CNT/Fe before sulfurization3C phase ratio, CF/CNT/Fe after sulfurization7S8The removal performance of lead ions is better.
Comparative example 2, an electrode active material comprising a carbon foam skeleton, carbon nanotubes, iron disulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; the iron disulfide is packaged in the carbon nanotube.
The preparation method is the same as that of the example 1, except that the vulcanization temperature of the step (4) is adjusted from 600 ℃ to 500 ℃, and the vulcanization is carried outThe final product obtained is CF/CNT/FeS2And (4) showing. The XRD and SEM images are shown in figures 9 and 10.
FIG. 11 shows the final products (CF/CNT/Fe) obtained in example 1 and comparative example 2 at a voltage of 1.2V and 200ppm lead ion solution7S8And CF/CNT/FeS2) Comparing the removal performance of lead ions; it is clearly seen that CF/CNT/Fe7S8The removal capability to lead ions is far higher than that of CF/CNT/FeS2
2. Test for cycling stability
To investigate the final product (CF/CNT/Fe) produced in the present invention7S8) Cycling stability during the electro-adsorption of lead ions the final product obtained in example 1 (CF/CNT/Fe)7S8) And carrying out cyclic electric adsorption on the lead ions.
FIG. 12 shows CF/CNT/Fe7S8The electrode is subjected to 16 times of cyclic absorption and desorption experiment results of lead ions under the voltage of 1.2V and the lead ion solution of 10 ppm; it can be seen that after the 16 th cycle, CF/CNT/Fe7S8The electric adsorption quantity of the electrode to lead ions is basically kept above 90% of the initial value, and the excellent cycle stability of the electrode active material is proved.
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 (10)

1. The electrode active material for adsorbing lead ions by a capacitor is characterized by comprising a carbon foam framework, carbon nano tubes and heptaferric octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam framework; and the heptaferric octasulfide is encapsulated in the carbon nanotube.
2. A preparation method of an electrode active material for capacitance adsorption of lead ions is characterized by comprising the steps of preparing a carbon foam precursor, carbonizing and vulcanizing; the carbon foam precursor is prepared from melamine foam, an iron source and urea serving as raw materials by a hydrothermal method or an oil bath method.
3. The method for preparing the electrode active material for capacitive adsorption of lead ions according to claim 2, wherein the hydrothermal method for preparing the carbon foam precursor specifically comprises the following steps: mixing melamine foam, an iron source and urea, adding deionized water, stirring until the solution is clear, reacting at the temperature of 100-120 ℃ for 12-24h, and cooling to obtain a carbon foam precursor; the mass ratio of the iron source to the urea is 1: 1-3; the mass volume ratio of the iron source to the melamine foam is g/cm3The value is 1: 100-250.
4. The method for preparing the electrode active material for capacitive adsorption of lead ions according to claim 2, wherein the step of preparing the carbon foam precursor by an oil bath method specifically comprises the following steps: mixing melamine foam, an iron source and urea, reacting for 12-24h under an oil bath at the temperature of 80-100 ℃, and cooling to obtain a carbon foam precursor; the mass ratio of the iron source to the urea is 1: 1-3; the mass volume ratio of the iron source to the melamine foam is g/cm3The value is 1: 100-250.
5. The method for producing an electrode active material for capacitive adsorption of lead ions according to any one of claims 2 to 4, wherein the iron source is a ferric salt or a ferrous salt; preferably, the iron source is selected from one or more of ferric nitrate, ferric sulfate and ferric chloride.
6. The method for preparing an electrode active material for capacitive adsorption of lead ions as claimed in any one of claims 2 to 5, wherein the carbonization temperature is 700 ℃ and 850 ℃ and the carbonization time is 1 to 4 hours; preferably, the temperature is raised to the carbonization temperature at a temperature raising rate of 1-8 ℃/min during carbonization.
7. The method for preparing an electrode active material for capacitive adsorption of lead ions as claimed in any one of claims 2 to 6, wherein during the vulcanization, sulfur powder is used as a vulcanizing agent, the vulcanization temperature is 550 ℃ and 700 ℃, and the vulcanization time is 1-4 h; the adding amount of the vulcanizing agent is 5-7 times of the mass of the carbonized product; preferably, the temperature is increased from room temperature to the vulcanization temperature at a temperature increase rate of 1-8 ℃/min during vulcanization.
8. The method for producing an electrode active material for capacitive adsorption of lead ions according to any one of claims 2 to 7, wherein the carbon foam precursor is subjected to freezing and freeze-drying treatment before carbonization; the freezing temperature is-20 ℃ to-80 ℃, and the freezing time is 24-48 h; the freeze drying temperature is-60 deg.C to-80 deg.C, and the freeze drying time is 48-72 h.
9. Use of the electrode active material for capacitive adsorption of lead ions according to claim 1 for adsorption or removal of lead ions in a solution.
10. The application of claim 9, wherein the electrode active material for lead ion capacitive adsorption is used as a negative electrode active material, and activated carbon is used as a positive electrode active material to construct an asymmetric capacitive deionization device, and the asymmetric capacitive deionization device is used for adsorbing or removing lead ions in a solution.
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CN114843112A (en) * 2022-05-18 2022-08-02 广州大学 Preparation method of compressible pseudocapacitance electrode material with autocatalytic induced growth

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