CN110482660A - A kind of preparation method and application of the etching graphite felt electrode applied to electric Fenton-like system - Google Patents
A kind of preparation method and application of the etching graphite felt electrode applied to electric Fenton-like system Download PDFInfo
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- CN110482660A CN110482660A CN201910684805.5A CN201910684805A CN110482660A CN 110482660 A CN110482660 A CN 110482660A CN 201910684805 A CN201910684805 A CN 201910684805A CN 110482660 A CN110482660 A CN 110482660A
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- graphite felt
- etching
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- electric fenton
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
A kind of preparation method and application of the etching graphite felt electrode applied to electric Fenton-like system, belongs to technical field of electrochemical water treatment.The present invention makes cobalt acetate be dispersed in graphite felt fibres surface using graphite felt as matrix, by ultrasonic immersing, high-temperature calcination under conditions of being continually fed into air by force, can get etching graphite felt.Compared with original graphite felt, when etching graphite felt as cathode material, yields of hydrogen peroxide can be effectively improved, is obviously improved the degradation capability of organic pollutant, and the cathode material is with good stability.The method of the present invention, production is simple, convenient controllable, is produced on a large scale, has a good application prospect.
Description
Technical field
The invention belongs to technical field of electrochemical water treatment, are related to a kind of etching graphite felt applied to electric Fenton-like system
The preparation method and application of electrode is mainly used for the electrochemical oxidation degradation of organic pollutants.
Background technique
Electric Fenton technology is a kind of processing method of organic pollutants of rapidly and efficiently degrading, and is to pass through cathodic oxygen reduction
The Fe in hydrogen peroxide and solution that reaction (ORR) generates in situ2+Reaction generates a kind of hydroxyl radical free radical with strong oxidizing property
(OH), hydroxyl radical free radical being capable of efficient non-selectivity ground organic pollutants of degrading.Electric Fenton technology is as a kind of environment
The electrochemical techniques of friendly have wide prospect in terms of environmental improvement especially water process, have caused that people's is wide
General concern.
Currently, carbon material is the electric common electrode material of Fenton technology, wherein graphite felt is due to biggish specific surface
Long-pending and good chemical stability, is widely used in water treatment field, but that there are hydrophilies is poor, hydrogen peroxide produces for graphite felt
The disadvantages of low, active site is few is measured, currently, researcher has conducted extensive research the modification and modification of graphite felt both at home and abroad,
Wherein the method for graphite felt modification and modification mainly has: chemical treatment, modified metal oxide, nonmetallic modification etc., but these
Many problems such as that there are costs of manufacture is high for method, manufacture craft is cumbersome, is unsuitable for producing on a large scale.Therefore, one kind is developed
Electrode prepared by the method is used in electric Fenton-like system raising water have by the preparation method for the modified graphite felt electrode being simple and efficient
The degradation effect of machine pollutant, has great importance.
Summary of the invention
For graphite felt cathode is improved to the degradation capability of organic pollutants, the invention proposes a kind of novel height
The preparation method and application of the modified graphite felt electrode for being applied to electric Fenton-like system of effect, simple possible, can be improved degradation speed
Rate, degradation depth and improve cyclicity, efficiency etc..
A kind of preparation method of the etching graphite felt electrode applied to electric Fenton-like system, comprising the following steps:
(1) it degreases and high temperature pre-processes:
Graphite felt is soaked in acetone soln and is cleaned by ultrasonic 20-50min, is removed for several times with deionized water ultrasonic cleaning residual
The acetone stayed, it is dry, graphite felt is finally put into 500 DEG C of high-temperature process 2-4h in high-temperature atmosphere furnace；
(2) etching pretreatment:
Graphite felt after step (1) resulting high-temperature process is soaked in the ethanol solution of the cobalt acetate containing 0.5-1.5g/L
In, it is ultrasonically treated 10-30min, guarantees that cobalt acetate ethanol solution sufficiently infiltrates graphite felt；Then it is dried at room temperature for 12h, makes vinegar
Sour cobalt uniform crystal dispersion is in graphite felt fibres surface；
(3) high temperature etching processing:
The resulting graphite felt for being loaded with cobalt acetate crystal of step (2) is placed in high-temperature atmosphere furnace, is being continually fed into sky by force
Under conditions of gas, it is warming up to 200-300 DEG C, constant temperature 0.5-1.5h with 3 DEG C -6 DEG C/min, obtains load cobalt sesquioxide crystal
Graphite felt；Then the graphite felt for loading cobalt sesquioxide crystal is placed in high-temperature atmosphere furnace, in the item for being continually fed into air by force
Under part, it is warming up to 400-600 DEG C with 3 DEG C -6 DEG C/min, constant temperature 0.5-1.5h finally obtains etching graphite felt.
It is described that be continually fed into the cavity that air is every 4.5 liters of volumes to correspond to air velocity by force be 5-15L/min.
The etching graphite felt of the method preparation is as electric Fenton-like system cathode material, for going organic contamination in water removal
Object, especially organochlorine pollutant.
Compared with prior art, the present invention has following excellent effect:
1. manufacture craft of the invention is simple, it is produced on a large scale, application easy to spread.
2. the graphite felt being prepared using the method for the present invention has bigger specific surface area, more surface defect structures
And stronger hydrophily, to significantly improve electric Fenton-like system to the degradation effect of organic pollutants.
3. the graphite felt being prepared using the method for the present invention is had as electric Fenton-like system cathode degradable organic pollutant
Degradation rate is fast, and degradation depth is good, can very degrade, while with good stability and repeated.
4. electrode of the present invention can effectively improve yields of hydrogen peroxide, it is obviously improved the degradation capability of organic pollutant, and
The cathode material is with good stability.
Detailed description of the invention
Fig. 1 (A), Fig. 1 (B) are respectively the scanning electron microscope (SEM) photograph (figure (A) on the method for the present invention etching front and back graphite felt materials surface
Comparative example, Fig. 1 (B) embodiment 1).
Fig. 2 is the N that the method for the present invention etches front and back graphite felt2Adsorption-desorption curve (77K).(curve a: comparative example；It is bent
Line b: embodiment 1)
Fig. 3 is that the method for the present invention etches degradation effect of the front and back graphite felt as electric Fenton-like system cathode material to diuron
Fruit.(curve a: comparative example；Curve b: embodiment 1；Curve c: embodiment 2；Curve d: embodiment 3)
Fig. 4 is repeat performance of the present invention etching graphite felt as electric Fenton-like system cathode material.
Specific embodiment
The present invention is first by cobalt acetate crystal uniform load to graphite felt fibres surface, under conditions of being continually fed into air
High-temperature calcination obtains etching graphite felt.The present invention to graphite felt perform etching key step include: degrease, etch pretreatment,
High temperature etching processing.
Graphite felt materials purchase of the present invention is in the magnificent carbon high-tech Co., Ltd of Hunan nine, with a thickness of 5mm.
Invention is further described in detail for following example and comparative example combination attached drawing, but the present invention is not limited in
Embodiment below.
Embodiment 1
The present invention etches the preparation method of graphite felt electrode, as follows:
(1) it degreases and high temperature pre-processes:
Graphite felt is soaked in acetone soln and is cleaned by ultrasonic 30min, is removed and is remained for several times with deionized water ultrasonic cleaning
Acetone, it is dry, graphite felt is finally put into 500 DEG C of high-temperature process 3h in high-temperature atmosphere furnace；
(2) etching pretreatment:
Graphite felt after step (1) resulting high-temperature process is soaked in the ethanol solution of the cobalt acetate containing 1g/L, ultrasound
15min is handled, guarantees that cobalt acetate ethanol solution sufficiently infiltrates graphite felt；Then it is dried at room temperature for 12h, keeps cobalt acetate crystal equal
It is even to be scattered in graphite felt fibres surface；
(3) high temperature etching processing:
The resulting graphite felt for being loaded with cobalt acetate crystal of step (2) is placed in high-temperature atmosphere furnace, is being continually fed into sky by force
Under conditions of gas (wherein size of burner hearth 200mm × 150mm × 150mm, air velocity 10L/min), it is warming up to 4 DEG C/min
300 DEG C, constant temperature 1h, obtain the graphite felt of load cobalt sesquioxide crystal；Then the graphite felt of cobalt sesquioxide crystal will be loaded
It is placed in high-temperature atmosphere furnace, and under conditions of being continually fed into air by force (wherein size of burner hearth 200mm × 150mm × 150mm, it is empty
Gas velocity is 10L/min), 400 DEG C are warming up to 4 DEG C/min, constant temperature 1h finally obtains etching graphite felt.
Embodiment 2
The present invention etches the preparation method of graphite felt electrode, as follows:
The present embodiment and 1 preparation process of embodiment are the difference is that will load cobalt sesquioxide crystal in step (3)
Graphite felt is placed in high-temperature atmosphere furnace, by force be continually fed into air under conditions of (wherein size of burner hearth 200mm × 150mm ×
150mm, air velocity 10L/min), 400 DEG C are warming up to 4 DEG C/min, constant temperature 0.5h finally obtains etching graphite felt.
Embodiment 3
The present invention etches the preparation method of graphite felt electrode, as follows:
The present embodiment and 1 preparation process of embodiment are the difference is that will load cobalt sesquioxide crystal in step (3)
Graphite felt is placed in high-temperature atmosphere furnace, by force be continually fed into air under conditions of (wherein size of burner hearth 200mm × 150mm ×
150mm, air velocity 10L/min), 600 DEG C are warming up to 4 DEG C/min, constant temperature 1h finally obtains etching graphite felt.
Comparative example
Graphite felt is soaked in acetone soln and is cleaned by ultrasonic 30min, is removed and is remained for several times with deionized water ultrasonic cleaning
Acetone, it is dry.
Effect application test example
Etching graphite felt prepared by above-described embodiment 1, adopts test performance in the following method.
1. etching the surface characteristics and physical characteristic of graphite felt
As shown in attached drawing 1 (B), there are many microcellular structures by high temperature, keen draft etching in graphite felt fibres surface
With surface defect structure, this makes it have more active sites.
As shown in Fig. 2, the specific surface area for etching graphite felt significantly increases, and the specific surface area of etching front and back graphite felt is by original
The 0.557m come2/ g increases to 5.506m2/ g, specific surface area improve 10 times, this makes it have more reaction sites.
2. etching the performance that graphite felt is applied in electric Fenton-like system.
The etching graphite felt that the embodiment 1 is obtained is applied to electric Fenton-like system as cathode material.The system uses three
Electrode system, reference electrode are saturated calomel electrode, are platinized platinum to electrode, working electrode is graphite felt, additional Fe2+Concentration is
0.5mM, electrolyte are 0.05M Na2SO4, operating potential is -0.7V (vs SCE), and initial pH is 3, and degradation 300ml contains
The diuron of 20mg/L simulates agricultural chemicals waste water.
As shown in Fig. 3, for etching graphite felt in 20min, the removal rate of diuron is up to 74.9%, and does not etch graphite
Felt is only 25.6% to the removal rate of diuron；Graphite felt is etched in 50min, diuron removal rate reaches 100%, and does not carve
Losing graphite felt is only 67.8% to the removal rate of diuron.This illustrates that the lithographic method can significantly improve graphite felt to organic contamination
The degradation capability of object.
From attached drawing 4 it is found that from reusing the 1st time to the 25th time, etching graphite felt electrode degrades to diuron apparent
Rate is gradually increased, and illustrates that the electrode becomes better and better to the degradation effect of diuron；Reuse the etching of the 35th time with the 1st time
The apparent speed that graphite felt electrode degrades to diuron is respectively 0.085,0.088min-1, illustrate that etching graphite felt reuses
35 times, significantly declining does not occur in diuron degradation effect, this shows that the etching graphite felt is with good stability and again
Renaturation.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, therefore
Without departing from the technical solutions of the present invention, to the above embodiments according to the technical essence of the invention any simply to repair
Change, all of which are still within the scope of the technical scheme of the invention.
Claims (5)
1. a kind of preparation method of the etching graphite felt electrode applied to electric Fenton-like system, which comprises the following steps:
(1) it degreases and high temperature pre-processes:
Graphite felt is soaked in acetone soln and is cleaned by ultrasonic 20-50min, is removed for several times with deionized water ultrasonic cleaning remaining
Acetone, it is dry, graphite felt is finally put into 500 DEG C of high-temperature process 2-4h in high-temperature atmosphere furnace；
(2) etching pretreatment:
Graphite felt after step (1) resulting high-temperature process is soaked in the ethanol solution of the cobalt acetate containing 0.5-1.5g/L, is surpassed
Sonication 10-30min guarantees that cobalt acetate ethanol solution sufficiently infiltrates graphite felt；Then it is dried at room temperature for, makes cobalt acetate crystal
It is dispersed in graphite felt fibres surface；
(3) high temperature etching processing:
The resulting graphite felt for being loaded with cobalt acetate crystal of step (2) is placed in high-temperature atmosphere furnace, is being continually fed into air by force
Under the conditions of, it is warming up to 200-300 DEG C, constant temperature 0.5-1.5h with 3 DEG C -6 DEG C/min, obtains the graphite of load cobalt sesquioxide crystal
Felt；Then the graphite felt for loading cobalt sesquioxide crystal is placed in high-temperature atmosphere furnace, under conditions of being continually fed into air by force,
It is warming up to 400-600 DEG C with 3 DEG C -6 DEG C/min, constant temperature 0.5-1.5h finally obtains etching graphite felt.
2. a kind of preparation method of etching graphite felt electrode applied to electric Fenton-like system described in accordance with the claim 1, special
Sign is, described to be continually fed into the cavity that air is every 4.5 liters of volumes to correspond to air velocity by force be 5-15L/min.
3. the etching graphite felt electrode of method preparation according to claim 1 or 2.
4. the application of the etching graphite felt electrode of method preparation according to claim 1 or 2, as electric Fenton-like system cathode
Material.
5. according to the application of claim 4, for removing organic pollutants, especially organochlorine pollutant.
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Cited By (6)
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| CN109534456A (en) * | 2018-11-12 | 2019-03-29 | 北京工业大学 | A kind of Co3O4/ graphite felt method for preparing composite electrode applied to anodic oxidation system |
| CN111153470A (en) * | 2020-02-12 | 2020-05-15 | 浙江师范大学 | Preparation method of electro-Fenton cathode material based on carbon felt loaded cobalt particles and application of electro-Fenton cathode material in sewage treatment |
| CN111883781A (en) * | 2020-06-05 | 2020-11-03 | 辽宁科技大学 | Activation method for nickel salt etched graphite felt electrode |
| 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 |
| CN112897645A (en) * | 2021-01-13 | 2021-06-04 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Three-dimensional graphene-based electro-Fenton cathode and preparation method and application thereof |
| CN113149155A (en) * | 2021-05-20 | 2021-07-23 | 北京工业大学 | Cu-doped Fe2O3Preparation and application of nano-particle/porous graphite felt cathode |
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| 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 |
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| CN113149155A (en) * | 2021-05-20 | 2021-07-23 | 北京工业大学 | Cu-doped Fe2O3Preparation and application of nano-particle/porous graphite felt cathode |
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