CN113511710B - Electrode active material for adsorbing lead ions through capacitor, and preparation method and application thereof - Google Patents

Electrode active material for adsorbing lead ions through capacitor, and preparation method and application thereof Download PDF

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CN113511710B
CN113511710B CN202110583322.3A CN202110583322A CN113511710B CN 113511710 B CN113511710 B CN 113511710B CN 202110583322 A CN202110583322 A CN 202110583322A CN 113511710 B CN113511710 B CN 113511710B
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electrode active
carbon foam
iron
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CN113511710A (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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    • 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

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Abstract

The invention discloses an electrode active material for adsorbing lead ions by a capacitor, and a preparation method and application thereof, wherein the electrode active material comprises a carbon foam skeleton, carbon nanotubes and seven iron octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the seven iron octasulfide is encapsulated in the carbon nano tube. 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 using the capacitor can be used for adsorbing or removing the lead ions in a solution, and has great application potential in actually treating the lead ions in wastewater.

Description

Electrode active material for adsorbing lead ions through capacitor, and preparation method and application thereof
Technical Field
The invention belongs to the technical field of capacitor deionization, and particularly relates to an electrode active material for adsorbing lead ions by a capacitor, and a preparation method and application thereof.
Background
Heavy metals are one of the most recognized hazardous contaminants because of their inherent non-degradability and enrichment. Among them, heavy metal lead (Pb) is one of the most common public hazards in drinking water, which 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.
Currently, methods for removing heavy metals from wastewater include membrane filtration, ion exchange, chemical precipitation, adsorption, and electrochemical methods. However, these methods have respective limitations. For example, the disadvantages of high cost, complex operation, multiple side reactions, high energy consumption and the like prevent the application of the catalyst.
The Capacitive Deionization (CDI) technology is a novel water treatment technology, and the basic principle is that charged ions are adsorbed on an electrode by using a low electric field, so that the charged ions in an aqueous solution are removed. Compared with membrane filtration, chemical precipitation and other processes, 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 heavy metal recovery and recycling of the electrode material, and simultaneously minimizing the problems of dirt and scaling. In aqueous CDI treatment solutions, CDI performance tends to be largely dependent on the nature of the electrode active material, and therefore, the selection of an appropriate 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 adsorbing lead ions by using a capacitor, 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 electro-adsorption effect on heavy metal lead ions, and has great application potential in actually treating 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 skeleton, carbon nanotubes and iron octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the seven iron octasulfide is encapsulated in the carbon nano tube.
The invention also provides a preparation method of the electrode active material for adsorbing lead ions by using the capacitor, 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 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-to-volume ratio of the iron source to the melamine foam is in g/cm 3 Calculated as 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 12-24 hours in an oil bath at 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-to-volume ratio of the iron source to the melamine foam is in g/cm 3 Calculated as 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 or ferrous salt; more preferably, the iron source is selected from one or more of ferric nitrate, ferric sulfate, ferric chloride. These iron salts may be hydrated salts or non-hydrated salts.
Preferably, when carbonizing, the carbonizing temperature is 700-850 ℃ and the carbonizing time is 1-4h; more preferably, upon carbonization, the temperature is raised to the carbonization temperature at a temperature-raising rate of 1 to 8 ℃/min.
The carbonization is carried out in an anaerobic atmosphere, wherein the anaerobic atmosphere is an inert gas or nitrogen atmosphere; preferably, carbonization is performed under 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 hours; the adding amount of the vulcanizing agent is 5-7 times of the mass of the carbonized product; more preferably, at the time of vulcanization, the temperature is raised from room temperature to the vulcanization temperature at a temperature-raising rate of 1 to 8 ℃/min.
Preferably, the carbon foam precursor is subjected to a freeze-drying treatment prior to carbonization; the freezing temperature is between-20 ℃ and-80 ℃ and the freezing time is between 24 and 48 hours; the freeze-drying temperature is-60 ℃ to-80 ℃ and the freeze-drying time is 48-72h.
The invention also provides an application of the electrode active material for adsorbing lead ions by capacitance or the electrode active material for adsorbing lead ions by capacitance prepared by the preparation method, which is used for adsorbing or removing lead ions in a solution.
Preferably, when the electrode active material for adsorbing lead ions by the capacitor is used as a negative electrode active material, activated carbon is used as a positive electrode active material, an asymmetric capacitor deionization device is constructed, and the asymmetric capacitor deionization device is used for adsorbing or removing lead ions in a solution.
The beneficial effects are that:
the invention provides an electrode active material, which comprises a carbon foam skeleton, carbon nanotubes and iron octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the seven iron octasulfide is encapsulated in the carbon nano tube. The electrode active material is used as a negative electrode active material, and the active carbon is used as a positive electrode active material, so that an asymmetric capacitance deionization device is constructed, and high-efficiency adsorption of heavy metal lead ions in a 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. In addition, the method is simple to operate, low in energy consumption and environment-friendly, and does not need additional treatment during adsorption.
Drawings
FIG. 1 shows the carbonized product (CF/CNT/Fe) obtained in example 1 3 C) And final product (CF/CNT/Fe) 7 S 8 ) Is a XRD pattern of (C).
FIG. 2 shows the carbonized product (CF/CNT/Fe) obtained in example 1 3 C) SEM images of (a).
FIG. 3 shows the final product (CF/CNT/Fe) obtained in example 1 7 S 8 ) SEM images of (a).
FIG. 4 shows the final product (CF/CNT/Fe) obtained in example 1 7 S 8 ) Is a high resolution XPS map of (1), wherein: (a) Fe 2p, (b) S2 p, (C) C1S, (d) N1S.
FIG. 5, (a) is a sample of the final product (CF/CNT/Fe) obtained in example 1 7 S 8 ) Lead ion removal performance for a 100ppm lead ion concentration solution at different voltages; (b) For CF/CNT/Fe prepared in example 1 at 1.2V voltage 7 S 8 The lead ion removal capacities of the materials for lead ion solutions with different concentrations are compared.
FIG. 6 shows the result of example 1 (CF/CNT/Fe at a voltage of 1.2V 7 S 8 ) XRD patterns of electrode plates prepared as active materials before and after electro-adsorption of 100ppm lead ion solution.
FIG. 7 shows the results of example 1 (CF/CNT/Fe at a voltage of 1.2V 7 S 8 ) After 100ppm lead ion solution was subjected to electric adsorption by the electrode sheet prepared as an active material, XPS measured by the electrode sheet, (a) Pb 4f, (b) S2 p.
FIG. 8 is a graph showing CF/CNT/Fe characteristics obtained by carbonization in example 1 3 C and CF/CNT/Fe obtained by vulcanization of example 1 7 S 8 The adsorption capacity of the product to lead ions in a solution with a lead ion concentration of 100ppm is compared.
FIG. 9 shows the final product (CF/CNT/FeS) obtained in comparative example 2 2 ) An XRD pattern of (b);
FIG. 10 shows the final product (CF/CNT/FeS) obtained in comparative example 2 2 ) SEM images of (a);
FIG. 11 shows the final product (CF/CNT/Fe) obtained in example 1 in 200ppm lead ion solution at a voltage of 1.2V 7 S 8 ) And comparative example 2 to give the final product (CF/CNT/FeS 2 ) Comparison of lead adsorption capacity.
FIG. 12 shows the CF/CNT/Fe prepared in example 1 7 S 8 The material had an electroadsorption capacity for lead ions during 16 cycles at a lead ion concentration of 10 ppm.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, which should be explicitly set forth 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 skeleton, carbon nanotubes and iron octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the seven iron octasulfide is encapsulated in the carbon nano tube. CF/CNT/Fe for electrode active material for capacitance adsorption of lead ion according to the present invention 7 S 8 The representation, wherein "CF" represents carbon foam, "CNT" is carbon nanotube, "Fe 7 S 8 "is seven iron octasulfide,"/"indicates a load.
In the electrode active material for adsorbing lead ions by using the capacitor, the seven-iron octasulfide is encapsulated in the carbon nano tube growing on the surface of the carbon foam skeleton, so that the stability of the seven-iron octasulfide can be enhanced, and the improvement of the cycle stability of the electro-adsorption lead ions is facilitated.
The invention also provides a preparation method of the electrode active material for adsorbing lead ions by using the capacitor, which comprises the steps of preparing a carbon foam precursor, carbonizing and vulcanizing; wherein, the preparation of the carbon foam precursor is to prepare the carbon foam precursor by cyanuric acidThe preparation method comprises the steps of taking amine foam, an iron source and urea as raw materials, and preparing the material by a hydrothermal method or an oil bath method. The carbonized product is treated with CF/CNT/Fe 3 C represents "CF" represents carbon foam, "CNT" is carbon nanotube, "Fe 3 C "is denoted as iron carbide and"/"is denoted as load.
The electrode active material for adsorbing lead ions in 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 functions to provide a carbon foam skeletal structure; iron source action: on one hand, the catalyst is used as a catalyst after carbonization and reduction, and carbon in melamine bubbles and urea is catalyzed to generate carbon nano tubes; on the other hand, iron is provided for the sulfidation reaction to produce heptairon octasulfide; urea action: on one hand, as a carbon source, the growth of the carbon nano tube is facilitated; on the other hand, as a nitrogen source, sufficient nitrogen is provided for the preparation of the nitrogen-doped carbon substrate material, which is advantageous for the capacitance adsorption performance of the finally prepared electrode active material.
The electrode active material for capacitance adsorption of lead ions and the electrode active material for capacitance 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 treated lead ion-containing solution is 10-300mg/L.
When the electrode active material is used as a negative electrode active material, activated carbon is used as a positive electrode active material, a negative electrode plate and a positive electrode plate are respectively prepared, and then an asymmetric capacitance deionization device is constructed.
The raw materials of the negative electrode plate, except the active material, which adopts the electrode active material for adsorbing lead ions of the capacitor, can adopt conventional raw materials, and can adopt but is 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 active material of the positive plate adopts active carbon, and other raw materials can adopt conventional raw materials, such as 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 methods for preparing the negative plate and the positive plate adopt conventional methods, and can adopt but are not limited to the following methods: adding an anode/cathode electrode active material, a binder and a conductive agent into a solvent according to a 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 coated effective area is 2X 2cm 2 The method comprises the steps of carrying out a first treatment on the surface of the And (5) 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 skeleton, carbon nanotubes and seven iron octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the iron octasulfide is encapsulated in the carbon nano tube.
The preparation method is as follows
(1) Preparing a carbon foam precursor by a hydrothermal method: 0.25g of ferric nitrate nonahydrate and 0.5g of urea are dissolved in 60mL of deionized water, poured into a high-pressure reaction kettle for mixing, and then 25cm of urea is added 3 Continuously heating melamine foam in an oven at 110 ℃ for 12 hours, and taking out after naturally 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 sample to 800 ℃ at a heating rate of 5 ℃/min for 2 hours, carbonizing, and cooling to room temperature to obtain CF/CNT/Fe 3 C;
(4) Vulcanizing: CF/CNT/Fe 3 C and sulfur powder are mixed according to the mass ratio of 1:5, the temperature is raised from room temperature to 600 ℃ at the temperature raising rate of 5 ℃/min, the mixture is maintained for 2 hours, and the final product CF/CNT/Fe is obtained after natural cooling 7 S 8
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 1 3 C) And final product (CF/CNT/Fe) 7 S 8 ) Is a XRD pattern of (C).
FIGS. 2 and 3 show the carbonized product (CF/CNT/Fe) obtained in example 1, respectively 3 C) And final product (CF/CNT/Fe) 7 S 8 ) SEM images of (a); as can be seen from fig. 3, the final product, namely the electrode active material for adsorbing lead ions by capacitance according to the present invention, contains carbon nanotubes and seven iron octasulfide encapsulated in the carbon nanotubes.
FIG. 4 shows the final product (CF/CNT/Fe) obtained in example 1 7 S 8 ) Is a high resolution graph of (2); as can be seen from FIG. 4, the final product (CF/CNT/Fe 7 S 8 ) Is made of Fe 7 S 8 Component and N, S co-doped carbon structure.
Example 2
An electrode active material for adsorbing lead ions by a capacitor comprises a carbon foam skeleton, carbon nanotubes and seven iron octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the iron octasulfide is encapsulated in the carbon nano tube.
The preparation method is as follows
(1) Preparing a carbon foam precursor by an oil bath method: uniformly mixing 0.2g of ferric chloride tetrahydrate and 0.5g of urea, and then putting the mixture into a container of 45cm 3 The melamine foam reacts for 12 hours in an oil bath at 80 ℃, and after natural cooling, the melamine foam is taken out to obtain a carbon foam precursor;
(2) Freezing the carbon foam precursor in a refrigerator at-20deg.C for 48 hr, and then transferring to a freeze dryer for drying at-60deg.C for 60 hr;
(3) Carbonizing: heating the sample to 800 ℃ at a heating rate of 5 ℃/min for 2 hours, carbonizing, and cooling to room temperature to obtain CF/CNT/Fe 3 C;
(4) Vulcanizing: CF/CNT/Fe 3 C and sulfur powder are mixed according to the mass ratio of 1:5, and rise is carried out at 5 ℃/minThe temperature rate is raised from room temperature to 600 ℃ for 2 hours, and the final product CF/CNT/Fe is obtained after natural cooling 7 S 8
Example 3:
an electrode active material for adsorbing lead ions by a capacitor comprises a carbon foam skeleton, carbon nanotubes and seven iron octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the iron octasulfide is encapsulated in the carbon nano tube.
The preparation method is as follows
(1) Preparing a carbon foam precursor by a hydrothermal method: 0.25g of ferric chloride tetrahydrate and 0.5g of urea are dissolved in 70mL of deionized water, poured into a high-pressure reaction kettle for mixing, and then 58cm of urea is added 3 Continuously heating melamine foam in a baking oven at 100 ℃ for 24 hours, and taking out after naturally cooling to obtain a carbon foam precursor;
(2) Freezing the carbon foam precursor in a refrigerator at-80 ℃ for up to 24 hours, and then transferring the carbon foam precursor to a freeze dryer for drying at-80 ℃ for up to 60 hours;
(3) Carbonizing: heating the sample to 700 ℃ at the heating rate of 7 ℃/min for 4 hours, carbonizing, and cooling to room temperature to obtain CF/CNT/Fe 3 C;
(4) Vulcanizing: CF/CNT/Fe 3 C and sulfur powder are mixed according to the mass ratio of 1:7, the temperature is raised from room temperature to 700 ℃ for 3 hours at the heating rate of 2 ℃/min, and the final product CF/CNT/Fe is obtained after natural cooling 7 S 8
Example 4
The same as in example 1, except that the iron source was changed from "ferric nitrate nonahydrate" to "ferric sulfate".
Performance test:
preparing a negative plate: the final product (CF/CNT/Fe) obtained in example 1 7 S 8 ) The electrode active material, the conductive agent ketjen black and the adhesive polyvinylidene fluoride are poured into a dimethylformamide solution according to the mass ratio of 8:1:1, and uniformly stirred and mixed to obtain electrode slurry, and then a proper amount of electrode slurry is taken and uniformly coated on the surface of a current collector titanium sheet (the effective coating area is 2×)2cm 2 ) Finally, putting the electrode plate into an oven to be dried at 70 ℃ to obtain the required electrode plate; preparation of a positive plate: the active carbon is used as an anode active material and is prepared by adopting the same method as a cathode plate.
Capacitive deionization device: the negative electrode plate and the positive electrode plate are assembled into an asymmetric capacitance deionization device;
the capacitive deionization device is used for adsorbing/removing lead ions in a solution, and comprises the following specific operations: and (3) transmitting the solution containing lead ions to an asymmetric capacitance deionization device through a peristaltic pump, and then applying voltage to perform electric adsorption.
1. Adsorption Performance test
To verify the final product (CF/CNT/Fe) produced by the present invention 7 S 8 ) The adsorption performance of lead ions is tested, and the effect of removing the lead ions from the solution with the lead ion concentration of 100ppm under different voltages is tested.
FIG. 5 (a) shows the final product (CF/CNT/Fe) obtained in example 1 7 S 8 ) Lead ion removal performance for a 100ppm lead ion concentration solution at different voltages; it can be seen that as the voltage increases, the amount of lead ions removed increases.
FIG. 5 (b) shows the final product (CF/CNT/Fe) obtained in example 1 at a voltage of 1.2V 7 S 8 ) Lead ion removal capacity of lead ion solutions with different concentrations is compared; it can be seen that at a voltage of 1.2V, the electrosorption performance for lead ions is saturated when the lead ion concentration reaches 200 ppm.
FIG. 6 is an XRD pattern of the electrode sheet before and after adsorption of 100ppm of lead ion solution at a voltage of 1.2V; as can be seen, in CF/CNT/Fe 7 S 8 After the electrodes electrically adsorb lead ions, pbS phase appears.
FIG. 7 is an XPS spectrum of the electrode sheet before and after adsorption of 100ppm lead ion solution at a voltage of 1.2V; further demonstrating the presence of PbS.
To further illustrate the capacitive 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 1 3 C) The negative electrode plate and the positive electrode plate are made of a negative electrode active material and active carbon as a positive electrode active material according to the same method, and then the asymmetric capacitance deionization device is assembled; the lead ion-containing solution was transferred to the capacitive deionization apparatus described in comparative example 1 by peristaltic pump, and then subjected to electric adsorption by applying a voltage.
FIG. 8 is a graph showing the comparison of the adsorption capacities of the electrode active materials of example 1 and comparative example 1 with respect to lead ions in a solution having a lead ion concentration of 100 ppm; it can be seen that the catalyst is mixed with CF/CNT/Fe before vulcanization 3 C comparison, CF/CNT/Fe after vulcanization 7 S 8 The removal performance of lead ions is better.
Comparative example 2, an electrode active material comprising carbon foam backbone, carbon nanotubes, iron disulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the iron disulfide is encapsulated within the carbon nanotubes.
The preparation method is the same as in example 1, except that the vulcanization temperature of the step (4) is adjusted from 600 ℃ to 500 ℃ and the final product obtained after vulcanization is treated with CF/CNT/FeS 2 And (3) representing. The XRD pattern and SEM pattern 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, a lead ion solution of 200ppm 7 S 8 And CF/CNT/FeS 2 ) Comparing lead ion removal performance; it is evident that CF/CNT/Fe 7 S 8 The removal capacity of lead ions is far higher than that of CF/CNT/FeS 2
2. Cycle stability test
To investigate the final product (CF/CNT/Fe) produced in the present invention 7 S 8 ) Cycle stability during the electro-adsorption of lead ions, the final product (CF/CNT/Fe) obtained in example 1 7 S 8 ) And (3) carrying out cyclic electroadsorption on lead ions.
FIG. 12 is CF/CNT/Fe 7 S 8 The electrode carries out the cyclic desorption experiment result graph of lead ions for 16 times under the voltage of 1.2V and the lead ion solution of 10 ppm; it can be seen that in 1 stAfter 6 cycles, CF/CNT/Fe 7 S 8 The electric adsorption quantity of the electrode to lead ions is basically maintained above 90% of the initial value, and the electrode active material has excellent cycle stability.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (8)

1. An electrode active material for adsorbing lead ions by a capacitor is characterized by comprising a carbon foam skeleton, carbon nanotubes and seven iron octasulfide; wherein, the carbon nano tube grows on the surface of the carbon foam skeleton; the seven iron octasulfide is encapsulated in the carbon nano tube;
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; when the hydrothermal method is adopted to prepare the carbon foam precursor, melamine foam, an iron source and urea are mixed, deionized water is added and stirred until the solution is clear, and the mixture reacts at 100-120 ℃ for 12-24h, and is cooled to obtain the carbon foam precursor; the mass-to-volume ratio of the iron source to the melamine foam is in g/cm 3 Counting as 1:100-250; the preparation method of the carbon foam precursor by adopting the oil bath method specifically comprises the following steps: mixing melamine foam, an iron source and urea, reacting for 12-24 hours in an oil bath at 80-100 ℃, and cooling to obtain a carbon foam precursor; the mass ratio of the iron source to the urea is 1:1-3;
when carbonizing, the carbonizing temperature is 700-850 ℃ and the carbonizing time is 1-4h; during vulcanization, sulfur powder is used as a vulcanizing agent, the vulcanization temperature is 550-700 ℃, and the vulcanization time is 1-4 hours; the addition amount of the vulcanizing agent is 5-7 times of the mass of the carbonized product.
2. The method for producing an electrode active material for capacitive adsorption of lead ions according to claim 1The preparation method 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; when the hydrothermal method is adopted to prepare the carbon foam precursor, melamine foam, an iron source and urea are mixed, deionized water is added and stirred until the solution is clear, and the mixture reacts at 100-120 ℃ for 12-24h, and is cooled to obtain the carbon foam precursor; the mass-to-volume ratio of the iron source to the melamine foam is in g/cm 3 Counting as 1:100-250;
the preparation method of the carbon foam precursor by adopting the oil bath method specifically comprises the following steps: mixing melamine foam, an iron source and urea, reacting for 12-24 hours in an oil bath at 80-100 ℃, and cooling to obtain a carbon foam precursor; the mass ratio of the iron source to the urea is 1:1-3;
when carbonizing, the carbonizing temperature is 700-850 ℃ and the carbonizing time is 1-4h; during vulcanization, sulfur powder is used as a vulcanizing agent, the vulcanization temperature is 550-700 ℃, and the vulcanization time is 1-4 hours; the addition amount of the vulcanizing agent is 5-7 times of the mass of the carbonized product.
3. The method for preparing an electrode active material for adsorbing lead ions by capacitance according to claim 2, wherein the mass ratio of the iron source to urea is 1:1-3 when preparing the carbon foam precursor by the hydrothermal method.
4. The method for producing an electrode active material for capacitive adsorption of lead ions according to claim 2 or 3, wherein the iron source is a trivalent iron salt or a divalent iron salt.
5. The method for producing an electrode active material for capacitive adsorption of lead ions according to claim 4, wherein the iron source is selected from one or a combination of a plurality of iron nitrate, iron sulfate and iron chloride.
6. The method for producing an electrode active material for capacitive adsorption of lead ions according to claim 2 or 3, wherein the temperature is raised to the carbonization temperature at a temperature-raising rate of 1 to 8 ℃/min at the time of carbonization.
7. The method for producing an electrode active material for capacitive adsorption of lead ions according to claim 2 or 3, wherein, at the time of vulcanization, the temperature is raised from room temperature to vulcanization temperature at a temperature-raising rate of 1 to 8 ℃/min.
8. The method for producing an electrode active material for capacitive adsorption of lead ions according to claim 2 or 3, wherein the carbon foam precursor is subjected to freezing and freeze-drying treatment prior to carbonization; freezing temperature is-20 ℃ to-80 ℃ and freezing time is 24-48h; the freeze-drying temperature is-60 ℃ to-80 ℃ and the freeze-drying time is 48-72h.
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