CN109534456A - A kind of Co3O4/ graphite felt method for preparing composite electrode applied to anodic oxidation system - Google Patents
A kind of Co3O4/ graphite felt method for preparing composite electrode applied to anodic oxidation system Download PDFInfo
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- CN109534456A CN109534456A CN201811340146.5A CN201811340146A CN109534456A CN 109534456 A CN109534456 A CN 109534456A CN 201811340146 A CN201811340146 A CN 201811340146A CN 109534456 A CN109534456 A CN 109534456A
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- graphite felt
- cobalt acetate
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- combination electrode
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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
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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
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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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
- C02F2001/46133—Electrodes characterised by the material
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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
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- General Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Electrodes For Compound Or Non-Metal Manufacture (AREA)
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Abstract
A kind of Co applied to anodic oxidation system3O4/ graphite felt method for preparing composite electrode, belongs to technical field of electrochemical water treatment.The present invention is using graphite felt as matrix, after its area load cobalt acetate, calcines to obtain Co in air environment high temperature3O4Graphite felt is loaded, at a certain temperature high-temperature calcination Co3O4Graphite felt is loaded, Co is utilized3O4Etching graphite felt obtains Co3O4/ graphite felt combination electrode.With the Co without etching prepared under equal conditions3O4Load graphite felt electrode is compared, Co3O4/ graphite felt combination electrode has higher oxidation efficiency.
Description
Technical field
The invention belongs to technical field of electrochemical water treatment, are related to a kind of Co applied to anodic oxidation system3O4/ graphite
Felt method for preparing composite electrode is mainly used for the electrochemical oxidation degradation of classes of herbicides pollutant in water.
Background technique
Herbicide is widely used in farmland, orchard, floral nursery, grassland and bare place region weeds, miscellaneous filling, miscellaneous tree etc.
The prevention and control of noxious plant.However, most of herbicide has bio-toxicity and is considered to have potential " three cause " effect, it is water
Typical persistence organic pollutant in body.Therefore, it is very necessary for removing classes of herbicides pollutant in water removal.Anodizing
As a kind of environmentally-friendly technique, there is good answer in terms of persistence organic pollutant in environment prevention and treatment especially degradation water
Use prospect.
The key of anodizing processing classes of herbicides pollutant is the preparation of anode material, the electrochemistry of anode material
Performance directly affects the degradation effect of organic pollutant.Carbon materials have excellent chemical property, are widely used in electricity
Pole field of material preparation, when carbon materials are as electrode matrix, decorative material and method of modifying have the performance of electrode bright
Aobvious influence.Researchers' discovery, Co3O4Graphite felt fibres can be etched, its surface area, especially Co are increased3O4/ graphite felt
Composite material has excellent electron transmission performance, makes it uniquely suited for as anode material.Therefore, Co3O4/ graphite felt is compound
It is the more efficient method of persistence organic pollutant in degradation water that electrode, which carries out electrocatalytic oxidation,.
The present invention is using graphite felt as carrier, with Co3O4As decorative material, it is dedicated to preparing and is urged with efficient electricity
Change the anode material of oxidation susceptibility.
Summary of the invention
It is an object of the invention to solve the problems of the prior art, provide it is a kind of prepare it is easy, good degrading effect with
Graphite felt is the Co of matrix3O4The preparation method of/graphite felt combination electrode.
Above-mentioned Co3O4The preparation method and process of/graphite felt combination electrode, comprising the following steps:
(1) graphite felt is such as removed into dirt having a size of ultrasonic cleaning in 1cm × 7cm merging aqueous isopropanol, then with pure
Water rinses remaining isopropanol well, is dried with nitrogen to obtain unsupported graphite felt；
(2) it takes four hydrate of cobalt acetate to be added in ethanol solution to be sufficiently stirred after dissolution as soak, cobalt acetate
Four hydrate concentration are the preferred 4mmol/L of 1-8mmol/L；The graphite felt that step (1) is cleaned up immerses four water of cobalt acetate
Ultrasound 30 minutes in the ethanol solution of compound, are then dried at room temperature for overnight；
(3) graphite felt after drying is placed in atmosphere furnace, (preferably room temperature rises to 300 DEG C, rises within 60 minutes for 300 DEG C of calcinings
Warm 5 DEG C/min of rate), air is pressed into furnace (the preferably flow velocity 1L/min of air) during calcining, obtains Co3O4Load stone
Black felt is spare；
(4) Co for preparing step (3)3O4Load graphite felt 60 minutes (preferably rooms of 300-500 DEG C of calcining in atmosphere furnace
Air is pressed into furnace during calcining with the flow velocity of 1L/min, is obtained to set temperature, 5 DEG C/min of heating rate) by temperature rise
Co3O4/ graphite felt combination electrode；The calcination temperature of step (4) be higher than step (3) calcination temperature, preferably 400 DEG C.
Compared with prior art, the invention has the following advantages:
1, the present invention is special using its biggish specific surface area, good electric conductivity and high intensity etc. using graphite felt as matrix
Point is conducive to the oxidation efficiency for improving electrode, provides basis to the electrochemical oxidation degradation of classes of herbicides pollutant for its realization.
2, the present invention is in graphite felt area load Co3O4, it is subsequent Co3O4The preparation of/graphite felt combination electrode provides item
Part.
3, the present invention is with Co3O4Co is prepared using etching graphite felt surface as decorative material3O4/ graphite felt composite wood
Material improves tool electron transmission efficiency, is conducive to the oxidation efficiency for enhancing electrode.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of unsupported graphite felt.
Fig. 2 is Co3O4Load the scanning electron microscopic picture of graphite felt.
Fig. 3 is Co3O4The scanning electron microscopic picture of/graphite felt combination electrode.
Fig. 4 is the Co of embodiment 1, embodiment 23O4The Co of/graphite felt combination electrode and comparative example3O4Load graphite felt electricity
Pole anodic oxidation degradation diuron effect picture.
Specific embodiment
Following example and comparative example will the present invention is further illustrated in conjunction with attached drawing, but the present invention is not limited to
Lower embodiment.
Embodiment 1:
(1) dirt is removed into ultrasonic cleaning in the graphite felt merging aqueous isopropanol of 1cm × 7cm, is then rushed with ultrapure water
The remaining isopropanol of wash clean is dried with nitrogen to obtain unsupported graphite felt；
(2) it takes four hydrate of cobalt acetate to be added in ethanol solution to be sufficiently stirred after dissolution as soak, cobalt acetate
Four hydrate concentration are 4mmol/L.The ethyl alcohol that the graphite felt that step (1) is cleaned up immerses four hydrate of cobalt acetate is molten
Ultrasound 30 minutes, are then placed in culture dish at room temperature and are dried overnight in liquid.
(3) graphite felt after drying is placed in atmosphere furnace, (room temperature rises to 300 DEG C, heating speed within 60 minutes for 300 DEG C of calcinings
5 DEG C/min of rate), air is pressed into furnace with the flow velocity of 1L/min during calcining, obtains Co3O4It is spare to load graphite felt；
(4) Co for preparing step (3)3O4Loading graphite felt, (room temperature, which rises to, to be set within 60 minutes for 400 DEG C of calcinings in atmosphere furnace
Determine temperature, 5 DEG C/min of heating rate), air is pressed into furnace with the flow velocity of 1L/min during calcining, obtains Co3O4/ graphite felt
Combination electrode；
(5) Co obtained with step (4)3O4/ graphite felt combination electrode anode, Pt piece are cathode, and degradation 300mL concentration is
20mg L-1Diuron waste water, 0.05mol L-1For sodium sulphate as electrolyte, kinetic current density is 2mA cm-2, reaction solution
PH is 6.8.
Embodiment 2:
(1) dirt is removed into ultrasonic cleaning in the graphite felt merging aqueous isopropanol of 1cm × 7cm, is then rushed with ultrapure water
The remaining isopropanol of wash clean is dried with nitrogen to obtain unsupported graphite felt；
(2) it takes four hydrate of cobalt acetate to be added in ethanol solution to be sufficiently stirred after dissolution as soak, cobalt acetate
Four hydrate concentration are 4mmol/L.The ethyl alcohol that the graphite felt that step (1) is cleaned up immerses four hydrate of cobalt acetate is molten
Ultrasound 30 minutes, are then placed in culture dish at room temperature and are dried overnight in liquid.
(3) graphite felt after drying is placed in atmosphere furnace, (room temperature rises to 300 DEG C, heating speed within 60 minutes for 300 DEG C of calcinings
5 DEG C/min of rate), air is pressed into furnace with the flow velocity of 1L/min during calcining, obtains Co3O4It is spare to load graphite felt；
(4) Co for preparing step (3)3O4Loading graphite felt, (room temperature, which rises to, to be set within 60 minutes for 500 DEG C of calcinings in atmosphere furnace
Determine temperature, 5 DEG C/min of heating rate), air is pressed into furnace with the flow velocity of 1L/min during calcining, obtains Co3O4/ graphite felt
Combination electrode；
(5) Co obtained with step (4)3O4/ graphite felt combination electrode anode, Pt piece are cathode, and degradation 300mL concentration is
20mg L-1Diuron waste water, 0.05mol L-1For sodium sulphate as electrolyte, kinetic current density is 2mA cm-2, reaction solution
PH is 6.8
Comparative example:
(1) dirt is removed into ultrasonic cleaning in the graphite felt merging aqueous isopropanol of 1cm × 7cm, is then rushed with ultrapure water
The remaining isopropanol of wash clean is dried with nitrogen to obtain unsupported graphite felt；
(2) it takes four hydrate of cobalt acetate to be added in ethanol solution to be sufficiently stirred after dissolution as soak, cobalt acetate
Four hydrate concentration are 4mmol/L.The ethyl alcohol that the graphite felt that step (1) is cleaned up immerses four hydrate of cobalt acetate is molten
Ultrasound 30 minutes, are then placed in culture dish at room temperature and are dried overnight in liquid.
(3) graphite felt after drying is placed in atmosphere furnace, (room temperature rises to 300 DEG C, heating speed within 60 minutes for 300 DEG C of calcinings
5 DEG C/min of rate), air is pressed into furnace with the flow velocity of 1L/min during calcining, obtains Co3O4It is spare to load graphite felt；
(4) Co obtained with step (3)3O4Graphite felt anode is loaded, Pt piece is cathode, and degradation 300mL concentration is 20mg
L-1Diuron waste water, 0.05mol L-1For sodium sulphate as electrolyte, kinetic current density is 2mA cm-2, reaction solution pH is
6.8
From fig. 4, it can be seen that embodiment 1 and embodiment 2 are more preferable to diuron treatment effect compared with comparative example, anodizing
It can be higher.
Claims (6)
1. a kind of Co applied to anodic oxidation system3O4/ graphite felt method for preparing composite electrode, comprising the following steps:
(1) will graphite felt be placed in aqueous isopropanol in ultrasonic cleaning go dirt, then it is clean with pure water rinsing, be dried with nitrogen
To unsupported graphite felt；
(2) it takes four hydrate of cobalt acetate to be added in ethanol solution to be sufficiently stirred after dissolution as soak, four water of cobalt acetate
Compound concentration is 1-8mmol/L；The graphite felt that step (1) is cleaned up immerses the ethanol solution of four hydrate of cobalt acetate
It middle ultrasonic 30 minutes, is then dried at room temperature for overnight；
(3) graphite felt after drying is placed in atmosphere furnace, 300 DEG C are calcined 60 minutes, with the flow velocity of 1L/min during calcining
Air is pressed into furnace, Co is obtained3O4It is spare to load graphite felt；
(4) Co for preparing step (3)3O4It loads graphite felt to calcine 60 minutes for 300-500 DEG C in atmosphere furnace, during calcining
Air is pressed into furnace with the flow velocity of 1L/min, obtains Co3O4/ graphite felt combination electrode；The calcination temperature of step (4) is higher than step
(3) calcination temperature.
2. according to the method for claim 1, which is characterized in that four hydrate concentration of cobalt acetate is 4mmol/L.
3. according to the method for claim 1, which is characterized in that the calcination temperature in step (4) is 400 DEG C.
4. according to the method for claim 1, which is characterized in that step (4) and step (3) calcination process temperature ramp
5℃/min。
5. according to the Co of the described in any item method preparations of claim 1-43O4/ graphite felt combination electrode.
6. according to the Co of the described in any item method preparations of claim 1-43O4The application of/graphite felt combination electrode, as sun
Pole, the electrochemical oxidation degradation for classes of herbicides pollutant in water.
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Cited By (3)
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| CN110482660A (en) * | 2019-07-26 | 2019-11-22 | 北京工业大学 | A kind of preparation method and application of the etching graphite felt electrode applied to electric Fenton-like system |
| CN112678924A (en) * | 2020-12-30 | 2021-04-20 | 北京工业大学 | Preparation method and application of hydrothermal modified graphite felt electrode applied to electro-Fenton system |
| CN118515344A (en) * | 2024-07-18 | 2024-08-20 | 湖南工程学院 | Electrocatalytic anode material for treating organic wastewater and preparation method and application thereof |
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Cited By (4)
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| CN110482660A (en) * | 2019-07-26 | 2019-11-22 | 北京工业大学 | A kind of preparation method and application of the etching graphite felt electrode applied to electric Fenton-like system |
| CN110482660B (en) * | 2019-07-26 | 2022-02-08 | 北京工业大学 | Preparation method and application of etched graphite felt electrode applied to electro-Fenton system |
| CN112678924A (en) * | 2020-12-30 | 2021-04-20 | 北京工业大学 | Preparation method and application of hydrothermal modified graphite felt electrode applied to electro-Fenton system |
| CN118515344A (en) * | 2024-07-18 | 2024-08-20 | 湖南工程学院 | Electrocatalytic anode material for treating organic wastewater and preparation method and application thereof |
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