CN113213588A - Electrode material based on hollow carbon nanofiber and preparation method and application thereof - Google Patents

Electrode material based on hollow carbon nanofiber and preparation method and application thereof Download PDF

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CN113213588A
CN113213588A CN202110391488.5A CN202110391488A CN113213588A CN 113213588 A CN113213588 A CN 113213588A CN 202110391488 A CN202110391488 A CN 202110391488A CN 113213588 A CN113213588 A CN 113213588A
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electrode material
hollow carbon
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carbon nanofiber
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CN113213588B (en
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黄洪
代益
司徒粤
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South China University of Technology SCUT
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • C02F2001/46138—Electrodes comprising a substrate and a coating
    • C02F2001/46142—Catalytic coating
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46152—Electrodes characterised by the shape or form
    • C02F2001/46157—Perforated or foraminous electrodes
    • C02F2001/46161—Porous electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention discloses an electrode material based on hollow carbon nanofibers and a preparation method and application thereof. The electrode material based on the hollow carbon nanofiber comprises a carbon fiber net, and carbon nanofibers, carbon nanotubes and carbon-coated iron-nickel nanoparticles, which are loaded on the carbon fiber net, wherein the carbon fiber net is made of the hollow carbon fibers. The preparation method of the electrode material based on the hollow carbon nanofiber comprises the following steps: polyacrylonitrile, polyvinylpyrrolidone, soluble iron salt and soluble nickel salt are dispersed in a solvent to prepare a spinning solution, then electrostatic spinning is carried out to form a net, and carbonization is carried out. The hollow carbon nanofiber-based electrode material has the advantages of large specific surface area, strong hydrophilicity, more active sites, good stability, simple preparation process, light and thin anode and good application prospect in the field of wastewater treatment by an electrochemical method.

Description

Electrode material based on hollow carbon nanofiber and preparation method and application thereof
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to an electrode material based on hollow carbon nanofibers and a preparation method and application thereof.
Background
With the development of science and technology and the increasing popularization of electronic products, the PCB (printed circuit board) industry is rapidly developed, and because the PCB is inevitably etched in the manufacturing process, a large amount of acidic waste etching solution containing high-concentration copper ions is generated in the etching process, and the regeneration and recovery of the acidic waste etching solution are important issues concerned by the PCB production industry.
At present, the regeneration and recovery of acidic etching waste liquid are mainly carried out by a chemical recovery method and an electrochemical regeneration method. The chemical recovery method is to recover part of Cu in the etching waste liquid+Is oxidized into Cu2+Then converted into acid etching regeneration liquid meeting the production requirements, and the other part of the etching waste liquid is sent to a designated factory for chemical recovery of CuSO4Or CuO, which is simple to operate but requires a large amount of chemical raw materials to be consumed, and generates a large amount of waste liquid in the whole recovery process, thus having a large influence on the environment. The electrochemical regeneration method can recover the redundant copper in the etching waste liquid, and the whole process flow needs less chemical agents, has little pollution to the environment, has high value of recovered products and has better application prospect.
The performance of the electrode material can directly influence the effect of the electrochemical regeneration method, and the development of the electrode material with more excellent performance is the key for further developing the regeneration of the electrochemical regeneration method and recovering the acidic etching waste liquid.
Disclosure of Invention
The invention aims to provide an electrode material based on hollow carbon nanofibers and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
an electrode material based on hollow carbon nano-fiber comprises a carbon fiber net, carbon nano-fiber loaded on the carbon fiber net and containing iron-nickel nano-particles, carbon nano-tubes and carbon-coated iron-nickel nano-particles; the carbon fiber net is composed of hollow carbon fibers.
Preferably, the diameter of the carbon nanofiber containing iron-nickel nanoparticles is 10nm to 25 nm.
Preferably, the diameter of the carbon nanotube is 10nm to 25 nm.
Preferably, the particle size of the carbon-coated iron-nickel nanoparticle is 10nm to 25 nm.
Preferably, the diameter of the hollow carbon fiber is 90nm to 170 nm.
The preparation method of the electrode material based on the hollow carbon nanofiber comprises the following steps: polyacrylonitrile, polyvinylpyrrolidone, soluble ferric salt and soluble nickel salt are dispersed in a solvent to prepare spinning solution, then electrostatic spinning is carried out to form a net, and carbonization is carried out to obtain the electrode material based on the hollow carbon nanofiber.
Preferably, the mass ratio of the polyacrylonitrile to the polyvinylpyrrolidone to the soluble ferric salt to the soluble nickel salt is 1: 0.5-1.5: 0.05-0.35.
Preferably, the solid content of the spinning solution is 10-15%.
Preferably, the polyacrylonitrile has a number average molecular weight of 150000 to 200000.
Preferably, the polyvinylpyrrolidone has a number average molecular weight of 1000000 to 2000000.
Preferably, the soluble iron salt is at least one of ferric nitrate, ferric acetate and ferric acetylacetonate.
Preferably, the soluble nickel salt is at least one of nickel acetate, nickel nitrate and nickel chloride.
Preferably, the solvent is at least one of N, N-Dimethylformamide (DMF) and N, N-Dimethylacetamide (DEF).
Preferably, the voltage difference between the positive electrode and the negative electrode of the electrostatic spinning is 10kV to 15kV, the distance between the positive electrode and the negative electrode is 10cm to 20cm, and the spinning speed is 0.5mL/h to 2 mL/h.
Preferably, the carbonization is performed by the following specific steps: firstly heating to 250-290 ℃ at the speed of 0.5-2 ℃/min, pre-oxidizing for 1-5 h, then heating to 900-1200 ℃ at the speed of 5-20 ℃/min, and carbonizing for 2-3 h.
The invention has the beneficial effects that: the hollow carbon nanofiber-based electrode material has the advantages of large specific surface area, strong hydrophilicity, more active sites, good stability, simple preparation process, light and thin anode and good application prospect in the field of wastewater treatment by an electrochemical method.
Specifically, the method comprises the following steps:
1) the electrode material based on the hollow carbon nanofiber is composed of a carbon fiber net, carbon nanofibers containing iron-nickel nanoparticles, carbon nanotubes and carbon-coated iron-nickel nanoparticles, wherein the carbon nanofibers are loaded on the carbon fiber net;
2) the electrode material based on the hollow carbon nanofiber has the characteristic of being light and thin, and is beneficial to reducing the size of a reactor and improving the engineering efficiency in practical application.
Drawings
Fig. 1 is an SEM image of the hollow carbon nanofiber-based electrode material of example 2.
Fig. 2 is an XRD pattern of the hollow carbon nanofiber-based electrode material of example 2.
FIG. 3 is a cyclic voltammogram of the hollow carbon nanofiber-based electrode materials of examples 1 to 3.
Fig. 4 is an anodic potential diagram of an anode made of the hollow carbon nanofiber-based electrode material of example 2 and a carbon felt anode during operation.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a preparation method of the electrode material based on the hollow carbon nanofiber comprises the following steps:
0.5g of polyacrylonitrile with the number average molecular weight of 150000, 0.5g of polyvinylpyrrolidone with the number average molecular weight of 1300000, 0.5g of ferric acetylacetonate and 0.1g of nickel acetate are dispersed in 10mL of DMF, stirred at room temperature for 12h to prepare spinning solution (with the solid content of 12 percent), then transferred to an electrostatic spinning instrument for electrostatic spinning and weaving into a net, the electrostatic spinning electrode voltage difference is 15kV, the distance between a positive electrode and a negative electrode is 15cm, the spinning speed is 0.5mL/h, then transferred to an oven, baked at 80 ℃ for 24h, transferred to a muffle furnace, filled with argon, the argon flow rate is 40mL/min, then heated to 290 ℃ at the speed of 0.5 ℃/min, pre-oxidized for 3h, heated to 1000 ℃ at the speed of 10 ℃/min, and carbonized for 3h to obtain the electrode material (marked as CNF-1000) based on the hollow carbon nanofiber.
Example 2:
a preparation method of the electrode material based on the hollow carbon nanofiber comprises the following steps:
0.5g of polyacrylonitrile with the number average molecular weight of 150000, 0.5g of polyvinylpyrrolidone with the number average molecular weight of 1300000, 0.5g of ferric acetylacetonate and 0.1g of nickel acetate are dispersed in 10mL of DMF, stirred at room temperature for 12h to prepare spinning solution (solid content of 12 percent), then transferred to an electrostatic spinning instrument for electrostatic spinning and weaving into a net, the voltage difference of an electrode of the electrostatic spinning is 15kV, the distance between a positive electrode and a negative electrode is 15cm, the spinning speed is 0.5mL/h, then transferred to an oven, baked at 80 ℃ for 24h, transferred to a muffle furnace, filled with argon, the flow rate of the argon is 40mL/min, then heated to 290 ℃ at the speed of 0.5 ℃/min, pre-oxidized for 3h, heated to 1100 ℃ at the speed of 10 ℃/min, and carbonized for 3h to obtain the electrode material (CNF-1100) based on the hollow carbon nanofiber.
A Scanning Electron Microscope (SEM) pattern and an X-ray diffraction (XRD) pattern of the hollow carbon nanofiber-based electrode material prepared in this example are shown in fig. 1 and 2, respectively.
As can be seen from fig. 1: the carbon fiber net substrate is composed of hollow carbon fibers with the diameter of 90 nm-170 nm, the carbon fibers, carbon nano tubes and carbon-coated iron-nickel nano particles are loaded on the carbon fiber net, the carbon fibers and the carbon nano tubes containing the iron-nickel nano particles have the diameter of 10 nm-25 nm, and the carbon-coated iron-nickel nano particles have the particle size of 10 nm-25 nm.
As can be seen from fig. 2: as can be seen from fig. 1, most of the particles existing on the hollow carbon fiber are carbon-coated iron-nickel nanoparticles, and the hollow carbon fiber is also loaded with a carbon nanotube and a carbon nanofiber coated with iron-nickel nanoparticles, and the metal particles exist as a catalyst for carbon graphitization.
Example 3:
a preparation method of the electrode material based on the hollow carbon nanofiber comprises the following steps:
0.5g of polyacrylonitrile with the number average molecular weight of 150000, 0.5g of polyvinylpyrrolidone with the number average molecular weight of 1300000, 0.5g of ferric acetylacetonate and 0.1g of nickel acetate are dispersed in 10mL of DMF, stirred at room temperature for 12h to prepare spinning solution (with the solid content of 12 percent), then transferred to an electrostatic spinning instrument for electrostatic spinning and weaving into a net, the electrostatic spinning electrode voltage difference is 15kV, the distance between a positive electrode and a negative electrode is 15cm, the spinning speed is 0.5mL/h, then transferred to an oven, baked at 80 ℃ for 24h, transferred to a muffle furnace, filled with argon, the argon flow rate is 40mL/min, then heated to 290 ℃ at the speed of 0.5 ℃/min, pre-oxidized for 3h, heated to 1200 ℃ at the speed of 10 ℃/min, and carbonized for 3h to obtain the electrode material (marked as CNF-1200) based on the hollow carbon nanofiber.
And (3) performance testing:
1) CNF-1000, CNF-1100 and CNF-1200 were fabricated into anodes with a size of 2cm × 2cm × 0.5mm, respectively, and placed in an acidic etching waste solution (composition: 1.7mol/L of CuCl20.055mol/L CuCl, 2mol/L NaCl and 2mol/L HCl) to remove residual metal on the electrode, wherein the control group is a carbon felt electrode with the same volume, the copper sheet is used as a cathode, and the electrolyte comprises the following components: 0.5mol/L of CuCl20.03mol/L CuCl, 2mol/L NaCl and 2mol/L HCl, and performing cyclic voltammetry tests at a scanning rate of 5mv/s and a scanning voltage interval of 0-0.8V to obtain a cyclic voltammetry curve as shown in FIG. 3.
As can be seen from fig. 3: the electrocatalytic activity of the electrode material based on hollow carbon nanofibers prepared at a carbonization temperature of 1100 ℃ is highest.
2) Regeneration of acid etching waste liquid:
adopt two rooms electrolytic cell as reaction vessel, solution volume all is 70mL in two electrolytic cells, uses electrochemical workstation as power and test instrument, and the acid etching waste liquid in the waste liquid collecting vat constitutes: 1.7mol/L of CuCl20.055mol/L CuCl, 2mol/L NaCl and 2mol/L HCl, wherein the composition of the catholyte is as follows: 0.17mol/L CuCl20.0055mol/L CuCl, 0.2mol/L NaCl and 0.2mol/L HCl, the cathode region is not stirred, the acid etching waste liquid is placed in the anode region, and the stirring speed of the anode region isThe rate was 200 r/min.
Respectively making CNF-1000, CNF-1100 and CNF-1200 into anodes with size of 2cm × 2cm × 0.5mm, soaking in acidic etching solution for 24h, using copper sheet as cathode, and keeping the current density at 35A/m2The test was carried out under conditions of 28.91C capacity and electrochemical tests were carried out on the whole electrolysis system (in view of Cu)+Too high ion concentration can affect the etching performance of the etching solution, and when Cu is in the acidic etching waste solution+If the ion concentration is lower than 0.05mol/L, the regeneration of the acid etching solution is successful; cu+The ion concentration test method comprises the following steps: transferring 2mL of anode solution to be tested into a conical flask, and adding 5mL of FeCl with the concentration of 0.2mol/L3The solution was added with 1 drop of 1, 10-phenanthroline indicator and then with 0.05mol/L Ce (SO)4)2Titration of the standard solution until the solution changes color from red to green, depending on the Ce (SO) used4)2Amount of standard solution to determine Cu+The amount of ions oxidized), the control group is carbon felt electrodes with the same volume, the anode potential diagram of the anode made of CNF-1100 and the carbon felt anode in the running process is shown in fig. 4, and the obtained test results of the regeneration effect are shown in the following table:
TABLE 1 results of the test of the regeneration effect of the acidic etching waste liquid
Figure BDA0003016915100000051
As can be seen from Table 1: compared with a carbon felt anode, the CNF-1000, CNF-1100 and CNF-1200 used as the anode reduce the energy consumption of copper recovery unit mass by 12%, 19% and 17% respectively.
As can be seen from fig. 4: as the reaction proceeded, the anode potential became higher and the cell voltage of the whole reaction became higher, and the anode potential rising rate was faster for the carbon felt anode compared to the anode made of CNF-1100, so the energy consumption increased, indicating that the electrocatalytic activity of the carbon felt was lower than that of CNF-1100 (same current density, voltage on the cathode remained the same, and anode potential trend reflected the whole cell voltage potential under the same apparatus, same test conditions).
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. An electrode material based on hollow carbon nanofibers, characterized in that: the composition of the hollow carbon nanofiber-based electrode material comprises a carbon fiber net, and carbon nanofibers, carbon nanotubes and carbon-coated iron-nickel nanoparticles, which contain iron-nickel nanoparticles, loaded on the carbon fiber net; the carbon fiber net is composed of hollow carbon fibers.
2. The hollow carbon nanofiber-based electrode material as claimed in claim 1, wherein: the diameter of the carbon nanofiber containing the iron-nickel nanoparticles is 10 nm-25 nm.
3. The hollow carbon nanofiber-based electrode material according to claim 1 or 2, characterized in that: the diameter of the carbon nano tube is 10 nm-25 nm.
4. The hollow carbon nanofiber-based electrode material as claimed in claim 3, wherein: the particle size of the carbon-coated iron-nickel nano particles is 10 nm-25 nm.
5. The hollow carbon nanofiber-based electrode material as claimed in claim 4, wherein: the diameter of the hollow carbon fiber is 90 nm-170 nm.
6. The method for preparing the hollow carbon nanofiber-based electrode material as claimed in any one of claims 1 to 5, comprising the steps of: polyacrylonitrile, polyvinylpyrrolidone, soluble ferric salt and soluble nickel salt are dispersed in a solvent to prepare spinning solution, then electrostatic spinning is carried out to form a net, and carbonization is carried out to obtain the electrode material based on the hollow carbon nanofiber.
7. The method for preparing a hollow carbon nanofiber-based electrode material as claimed in claim 6, wherein: the mass ratio of the polyacrylonitrile to the polyvinylpyrrolidone to the soluble ferric salt to the soluble nickel salt is 1: 0.5-1.5: 0.05-0.35.
8. The method for preparing a hollow carbon nanofiber-based electrode material as claimed in claim 6 or 7, wherein: the voltage difference between the positive electrode and the negative electrode of the electrostatic spinning is 10 kV-15 kV, the distance between the positive electrode and the negative electrode is 10 cm-20 cm, and the spinning speed is 0.5 mL/h-2 mL/h.
9. The method for preparing a hollow carbon nanofiber-based electrode material as claimed in claim 6 or 7, wherein: the concrete operation of carbonization is as follows: firstly heating to 250-290 ℃ at the speed of 0.5-2 ℃/min, pre-oxidizing for 1-5 h, then heating to 900-1200 ℃ at the speed of 5-20 ℃/min, and carbonizing for 2-3 h.
10. Use of the hollow carbon nanofiber-based electrode material as claimed in any one of claims 1 to 5 as an anode material in the electrochemical treatment of wastewater.
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