CN109896598A - The preparation method of electric Fenton cathode material based on carbon felt load iron nano-particle and its application in degradation organic pollutants - Google Patents
The preparation method of electric Fenton cathode material based on carbon felt load iron nano-particle and its application in degradation organic pollutants Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of electric Fenton cathode material based on carbon felt load iron nano-particle and its applications in degradation organic pollutants, belong to preparation and the electricity Fenton water-treatment technology field of electric Fenton cathode material.Technical solution of the present invention main points are as follows: load to polyaniline in pure carbon felt by electrochemical deposition, iron particle is loaded again obtains the porous compound carbon fibre material of iron carbon doping, this carbon felt is applied in electric Fenton water treatment facilities as cathode material and is exposed into air, it can be catalyzed at cathode and generate hydroxyl radical free radical, and then the organic pollutant in water of degrading.The present invention has given full play to the characteristics of carbon fiber large specific surface area, has many advantages, such as that treatment effeciency is high, environmentally protective, can generate economic benefit and social benefit in dyeing wastewater and groundwater treatment field.
Description
Technical field
The invention belongs to the preparation of electric Fenton cathode material and electric Fenton water-treatment technology fields, and in particular to one kind is based on
The preparation method and its application in degradation organic pollutants that carbon felt loads the electric Fenton cathode material of iron nano-particle.
Background technique
In recent years, to some extent by the pollution of organic matter, main contaminated area is the main rivers and lakes in China
In Middle And Lower Reaches of Changjiang River, Yellow River basin, the Delta of the Pearl River and Songhua River Basin.The water proposed according to China's many years monitoring result
Middle priority pollutants are up to 68 kinds, and wherein toxic organic pollutant just has 58 kinds, and China's water pollution is mainly with organic pollution
Based on.Wherein persistence organic pollutant is very big to the harmfulness of environmental ecology, it is difficult to degrade, pollution sources are wide.Wherein, printing and dyeing mill
Discharge largely contains dye wastewater with high concentration, complicated component, it is difficult to carry out degradation treatment using traditional physico-chemical process.Together
When soil pollution based on organic contamination also gradually attract extensive attention.Organic pollutant category is more, to environmental ecology with
And there are larger impacts for human health, have certain inhibition to sustainable development.Currently, China's processing industrial wastewater,
The mode in sanitary sewage and soil pollution waters is more single, alternative not strong, it is difficult to utilize extensively, higher cost, consumption
When effort, clean-up effect is bad.With the development of science and technology, advanced oxidation (AOP) technology water pollution processing in increasingly by
Favor in the industry has the characteristics that high energy efficiency, high degree of automation and operating environment are mildly safe, it is considered to be used for
One of the optimal selection of organic wastewater of processes composition complexity.
Electric Fenton technology depends on metal ion catalysis and generates hydrogen peroxide and then generate hydroxyl radical free radical to reach
Aoxidize the purpose of organic pollutant.Electric Fenton technology is particularly splendid in terms of degradation of organic substances, in degradation rate and soil removal efficiency side
Face all shows good performance, and a large amount of settled sludges can be generated and need to be continuously added to peroxidating by overcoming in traditional Fenton
The shortcomings that hydrogen.Electro-Fenton reaction system is different from that the water treatment technology based on other Fenton's reactions is more most important to be,
Electro-Fenton reaction can be electrolysed generation hydrogen peroxide, avoid the cost and risk of production hydrogen peroxide, in addition ferrous ion
The cyclic regeneration in cathode reduction process, it is ensured that the duration of degradation.During electro-Fenton reaction, a small amount of ferrous ion
The activity of hydrogen peroxide can be enhanced, to more effectively generate ferric ion and hydroxyl radical free radical.From the point of view of from many aspects, electricity
Fenton technology has a extensive future in Environmental electrochemistry field.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of simple process and the low-cost carbon felt load iron that is based on is received
The preparation method of the electric Fenton cathode material of rice grain, this method electric Fenton yin obtained based on carbon felt load iron nano-particle
Pole material is as electrode, and under conditions of pH is suitable for, being passed through air makes oxygen in activated carbon-fiber felt surface reduction at hydrogen peroxide, institute
It obtains hydrogen peroxide and is further catalyzed generation great amount of hydroxy group free radical, and then the organic pollutant in oxidative degradation water.
The present invention adopts the following technical scheme that the electricity based on carbon felt load iron nano-particle is fragrant to solve above-mentioned technical problem
The preparation method of cathode material, it is characterised in that specific steps are as follows:
Step S1: carbon fibre material being used respectively deionized water and EtOH Sonicate impregnate 20~40min, using cleaning,
It is spare after drying；
Step S2: by aniline, concentrated hydrochloric acid and deionized water mixed preparing aniline hydrochloride solution for standby, by seven hydrated sulfuric acids Asia
It is spare that iron and deionized water prepare ferrous sulfate solution；
Step S3: setting electric deposition device, the electrode in the electric deposition device include anode, cathode and reference electrode,
Anodic connects the anode of electrochemical workstation, and cathode connects the cathode of electrochemical workstation, and reference electrode is AgCl electrode, matches
For the aniline hydrochloride solution of system as deposition liquid, the voltage that electrochemical workstation is arranged is 0.8V, is carried out by the method for constant voltage
Electro-deposition obtains the depositing electrode of load polyaniline after 1~2h of electrodeposit reaction, then depositing electrode is immersed in the sulfuric acid of preparation
12 in ferrous iron solution~obtain for 24 hours load polyaniline and iron nano-particle electric Fenton cathode material；
Step S4: the electric Fenton cathode material for loading polyaniline and iron nano-particle is placed in tube furnace, in nitrogen atmosphere
600~900 DEG C of 1~2h of calcining are warming up to the heating rate of 5 DEG C/min under enclosing, target product carbon felt load iron nanometer is made
The electric Fenton cathode material of grain.
Preferably, the specification of carbon fibre material described in step S1 is 3cm*9cm*0.5cm~5cm*12cm*1cm.
Preferably, the mass ratio of aniline, concentrated hydrochloric acid and deionized water is 9:16 in aniline hydrochloride solution described in step S2:
75, the molar concentration of ferrous sulfate solution is 0.08~0.12mol/L.
Preferably, calcination temperature is 700 DEG C in step S4.
The electric Fenton cathode material organic contamination in degradation water of the present invention based on carbon felt load iron nano-particle
Application in object, it is characterised in that detailed process are as follows: in electric Fenton-like system, be based on carbon felt load iron nanometer for obtained above
Working electrode of the electric Fenton cathode material of particle as cathode connection electrochemical workstation, common carbon felt electrode connect electrochemistry
Work station to electrode, and green vitriol particle is added in the electrolytic solution, wherein electrolyte is 4~400mmol/L
Metabisulfite solution, the concentration of green vitriol in the electrolytic solution are 0.1mmol/L, and the electric current that electrochemical workstation is arranged is
50~130mA is electrolysed by way of constant current, and electrolysis time is 60~150min, opens magnetic agitation, adjusts solution
10~50 DEG C of pH=1~10 of system, temperature, oxygen generate hydrogen peroxide, gained peroxidating in activated carbon fiber surface reduction
Hydrogen, which is further catalyzed, generates great amount of hydroxy group free radical, and then the organic pollutant in oxidative degradation water, it is reacted after electrode warp
Deionized water flushing, drying can repetitive cycling uses.
Preferably, electrolyte is the metabisulfite solution of 40mmol/L, and the electric current that electrochemical workstation is arranged is 110mA, is adjusted
Save pH=2~3 of solution system.
Preferably, the organic pollutant is methyl orange, Congo red or rhodamine B.
Compared with the prior art, the invention has the following beneficial effects:
1, the present invention has given full play to the characteristics of carbon felt large specific surface area, has many advantages, such as that treatment effeciency is high, environmentally protective,
Economic benefit and social benefit can be generated in dyeing wastewater and groundwater treatment field；
2, reagent and electrode material used in the present invention are cheap and are easy to get, consumed in electrolytic process
Hydrogen peroxide automatic regeneration under conditions of being passed through air ensure that the sustaining degradation of pollutant, be not necessarily to compared with traditional Fenton process
Any oxidant is added in external source；
3, the electric Fenton cathode material produced by the present invention based on carbon felt load iron nano-particle used once purged energy
Enough repetitive cyclings use, and still maintain higher degradation efficiency.
Detailed description of the invention
Fig. 1 is the preparation method and its water treatment applications of the electric Fenton cathode material based on carbon felt load iron nano-particle
Technology Roadmap；
Fig. 2 is the scanning electron microscope (SEM) photograph that the electric Fenton cathode material based on carbon felt load iron nano-particle is made in embodiment 1；
Fig. 3 is the transmission electron microscope picture that the electric Fenton cathode material based on carbon felt load iron nano-particle is made in embodiment 1；
Fig. 4 is that the electric Fenton cathode material based on carbon felt load iron nano-particle is made as cathode in difference in embodiment 1
Under the conditions of to the degradation effect figure of methyl orange；
Fig. 5 is that circulation of the electric Fenton cathode material based on carbon felt load iron nano-particle as cathode is made in embodiment 1
Using renderings.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
The preparation of electric Fenton cathode material based on carbon felt load iron nano-particle:
(1) it pre-processes: choosing the carbon fibre material that specification is 3cm*9cm*0.5cm, it is super with deionized water and ethyl alcohol respectively
Sound impregnates 30min, using spare after cleaning, drying；
(2) prepare aniline hydrochloride solution and ferrous sulfate solution: aniline hydrochloride solution is by aniline, concentrated hydrochloric acid and deionization
Water mixed preparing forms, mass ratio 9:16:75, then carries out magnetic agitation 30min；Ferrous sulfate solution be by seven water and
What ferrous sulfate and deionized water were formulated, molar concentration 0.1mol/L；
(3) electric deposition device is set, and the electrode in the electric deposition device includes anode, cathode and reference electrode, middle-jiao yang, function of the spleen and stomach
Pole connects the anode of electrochemical workstation, and cathode connects the cathode of electrochemical workstation, and reference electrode is AgCl electrode, preparation
For aniline hydrochloride solution as deposition liquid, the voltage that electrochemical workstation is arranged is 0.8V, and it is heavy to carry out electricity by the method for constant voltage
Product, obtains the depositing electrode of load polyaniline after electrodeposit reaction 2h, then the ferrous sulfate that depositing electrode is immersed in preparation is molten
18h obtains the electric Fenton cathode material of load polyaniline and iron nano-particle in liquid；
(4) the electric Fenton cathode material for loading polyaniline and iron nano-particle the firing of depositing electrode: is placed in tube furnace
It is interior, 600~900 DEG C of calcining 1h are warming up to the heating rate of 5 DEG C/min under nitrogen atmosphere, carbon felt load iron nanometer is made
The electric Fenton cathode material of grain.
Fig. 2 and Fig. 3 is the scanning electron microscope (SEM) photograph of the electric Fenton cathode material of above-mentioned obtained carbon felt load iron nano-particle respectively
Piece and transmission electron microscope picture are dispersed with iron nano-particle on smooth activated carbon fiber surface as seen from the figure.
As shown in Figure 4 and Figure 5, use the electric Fenton cathode material of the resulting activity of the present invention as yin in electric Fenton-like system
Pole, be passed through air and magnetic agitation effect under, oxygen activated carbon fiber surface reduction generate hydrogen peroxide, gained peroxidating
Hydrogen, which is further catalyzed, generates great amount of hydroxy group free radical, and then the organic pollutant in oxidative degradation water.
Fig. 4 give the electric Fenton cathode material of the activity different firing temperatures (a), different current strength (b), solution not
Under conditions of same pH (c) and various concentration electrolyte (d), to the contrast schematic diagram of the removal effect of methyl orange.It can by scheming (a)
To find out, the electrode degrading effect under 700 DEG C of firing temperatures is best；Known by scheming (b), influence of the size of current to removal rate compared with
Small, degradation efficiency is relatively high under the electric current of 110mA.Degradation effect is higher in the case where pH=2~3 in figure (c)；By
Degradation efficiency highest when figure (d) can be seen that the sodium sulphate that 40mM is added.
Fig. 5 gives the effect picture that the electric Fenton cathode material of the activity degrade as cathode circulation, by scheme to can be found that with
The increase of access times, the removal rate of methyl orange can still reach 90% or more, it is seen that carbon felt load iron nanometer should be based on
The stability of the electric Fenton cathode material of grain is preferable.
Embodiment 2
Embodiment 1 is made the electric Fenton cathode material based on carbon felt load iron nano-particle and imitates to the removal of different dye liquors
Fruit:
Reaction solution volume: 100mL；
Reaction solution temperature: 25 ± 10 DEG C；
Reaction solution initial pH value: 3；
Electrode area: 27cm2；
Electrolyte concentration: 40mM Na2SO4Solution；
Oxygen gas flow rate: 100mL/min；
Current strength: 100mA；
Reaction time: 60min；
Different dye liquors: methyl orange, Congo red, rhodamine B；
Dye liquor concentration: 100mg/L.
The electric Fenton cathode material of table 1 is as cathode to the removal rate of different dye liquors
From embodiment 2 as can be seen that the electric Fenton cathode material work based on carbon felt load iron nano-particle is made in embodiment 1
For cathode to concentration be 100mg/L different dye liquors degradation efficiency it is especially significant.
Embodiment 3
Embodiment 1 is made under the electric Fenton cathode material condition of different pH based on carbon felt load iron nano-particle to methyl orange
The influence of removal effect:
Reaction solution volume: 100mL；
Reaction solution temperature: 25 ± 10 DEG C；
Electrode area: 27cm2；
Electrolyte concentration: 40mM Na2SO4Solution；
Oxygen gas flow rate: 100mL/min；
Current strength: 100mA；
Reaction time: 120min；
Dye liquor concentration: 100mg/L methyl orange solution；
Reaction solution initial pH value: 2,3,4,5.
The electric Fenton cathode material of table 2 influences the removal rate of methyl orange under condition of different pH
| pH | 2 | 3 | 4 | 5 |
| Removal rate | 97.8% | 96.7% | 91.3% | 92.1% |
From embodiment 3 as can be seen that the electricity sweet smell based on carbon felt load iron nano-particle is made in embodiment 1 in acid condition
Cathode material as cathode to the removal rate of methyl orange up to 90% or more, and it is the most significant in the removal rate of pH=2,3.
To sum up, the present invention utilizes the electric Fenton cathode material based on carbon felt load iron nano-particle, and polyaniline is passed through electricity
Deposition load in pure carbon felt, then load iron ion obtain iron carbon doping porous compound carbon fibre material, using this carbon felt as
Cathode in electro-Fenton reaction device is passed through air and magnetic agitation under conditions of pH is suitable for, makes oxygen in activated carbon fiber
Surface reduction generates hydrogen peroxide, and gained hydrogen peroxide, which is further catalyzed, generates great amount of hydroxy group free radical, and then oxidative degradation water
In organic pollutant.This support type electricity Fenton cathode material preparation method is simple, mild condition, used reagent and electrode
Material price is cheap and is easy to get, consumed hydrogen peroxide automatic regeneration under conditions of being passed through air in electrolytic process,
Any oxidant is added without external source compared with traditional Fenton process in the sustaining degradation that ensure that pollutant.And carbon is given full play to
The characteristics of felt large specific surface area, and active electrode use is Ke Xunhuanliyong later, stability is high, has treatment effeciency height, green
It the advantages that environmentally friendly, can be in dyeing wastewater and groundwater treatment field prosperity economic benefit and social benefit.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (7)
1. the preparation method of the electric Fenton cathode material based on carbon felt load iron nano-particle, it is characterised in that specific steps are as follows:
Step S1: carbon fibre material being used respectively deionized water and EtOH Sonicate impregnate 20~40min, using cleaning, drying
It is spare afterwards；
Step S2: by aniline, concentrated hydrochloric acid and deionized water mixed preparing aniline hydrochloride solution for standby, by green vitriol and
It is spare that deionized water prepares ferrous sulfate solution；
Step S3: electric deposition device is set, and the electrode in the electric deposition device includes anode, cathode and reference electrode, middle-jiao yang, function of the spleen and stomach
Pole connects the anode of electrochemical workstation, and cathode connects the cathode of electrochemical workstation, and reference electrode is AgCl electrode, preparation
For aniline hydrochloride solution as deposition liquid, the voltage that electrochemical workstation is arranged is 0.8V, and it is heavy to carry out electricity by the method for constant voltage
It is long-pending, the depositing electrode of load polyaniline is obtained after 1~2h of electrodeposit reaction, then depositing electrode is immersed in the ferrous sulfate of preparation
12 in solution~obtain for 24 hours load polyaniline and iron nano-particle electric Fenton cathode material；
Step S4: the electric Fenton cathode material for loading polyaniline and iron nano-particle is placed in tube furnace, under nitrogen atmosphere
600~900 DEG C of 1~2h of calcining are warming up to the heating rate of 5 DEG C/min, and target product carbon felt load iron nano-particle is made
Electric Fenton cathode material.
2. the preparation method of the electric Fenton cathode material according to claim 1 based on carbon felt load iron nano-particle,
Be characterized in that: the specification of carbon fibre material described in step S1 is 3cm*9cm*0.5cm~5cm*12cm*1cm.
3. the preparation method of the electric Fenton cathode material according to claim 1 based on carbon felt load iron nano-particle,
Be characterized in that: the mass ratio of aniline, concentrated hydrochloric acid and deionized water is 9:16:75, sulphur in aniline hydrochloride solution described in step S2
The molar concentration of sour ferrous iron solution is 0.08~0.12mol/L.
4. the preparation method of the electric Fenton cathode material according to claim 1 based on carbon felt load iron nano-particle,
Be characterized in that: calcination temperature is 700 DEG C in step S4.
5. the electric Fenton cathode material obtained based on carbon felt load iron nano-particle is dropping according to the method for claim 1
Solve the application in organic pollutants, it is characterised in that detailed process are as follows: in electric Fenton-like system, obtained will be based on carbon felt
Load working electrode of the electric Fenton cathode material of iron nano-particle as cathode connection electrochemical workstation, common carbon felt electrode
Connect electrochemical workstation to electrode, and in the electrolytic solution be added green vitriol particle, wherein electrolyte be 4~
The metabisulfite solution of 400mmol/L, the concentration of green vitriol in the electrolytic solution are 0.1mmol/L, and electrochemistry work is arranged
Making the electric current stood is 50~130mA, is electrolysed by way of constant current, and electrolysis time is 60~150min, opens magnetic force
Stirring, adjust solution system pH=1~10,10~50 DEG C of temperature, oxygen activated carbon fiber surface reduction generate peroxidating
Hydrogen, gained hydrogen peroxide, which is further catalyzed, generates great amount of hydroxy group free radical, and then the organic pollutant in oxidative degradation water, through anti-
Electrode after answering can repetitive cycling use through deionized water flushing, drying.
6. application according to claim 5, it is characterised in that: the electrolyte is the metabisulfite solution of 40mmol/L, if
The electric current for setting electrochemical workstation is 110mA, adjusts pH=2~3 of solution system.
7. application according to claim 5, it is characterised in that: the organic pollutant is methyl orange, Congo red or Luo Dan
Bright B.
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| CN114481187A (en) * | 2022-02-15 | 2022-05-13 | 中国科学院赣江创新研究院 | electro-Fenton cathode material and preparation method and application thereof |
| CN114481187B (en) * | 2022-02-15 | 2024-01-19 | 中国科学院赣江创新研究院 | electro-Fenton cathode material and preparation method and application thereof |
| CN115072839B (en) * | 2022-03-14 | 2023-08-08 | 南京理工大学 | Iron-containing composite magnetic material, preparation method and catalytic application thereof |
| CN115072839A (en) * | 2022-03-14 | 2022-09-20 | 南京理工大学 | Iron-containing composite magnetic material and preparation method and catalytic application thereof |
| CN115321646A (en) * | 2022-07-20 | 2022-11-11 | 湖北大学 | Method for degrading organic pollutants by electrocatalysis of external magnetic field |
| CN115321646B (en) * | 2022-07-20 | 2023-08-15 | 湖北大学 | Method for electrocatalytic degradation of organic pollutants by externally applied magnetic field |
| CN115382551A (en) * | 2022-07-26 | 2022-11-25 | 湖南大学 | Three-dimensional carbon functional cathode material based on potassium ferrate modification and preparation method and application thereof |
| CN115382551B (en) * | 2022-07-26 | 2023-10-13 | 湖南大学 | Three-dimensional carbonaceous functional cathode material based on potassium ferrate modification, and preparation method and application thereof |
| CN115893592A (en) * | 2022-11-03 | 2023-04-04 | 北京林业大学 | Rapid purification technology for electric flocculation in-situ coupling electro-Fenton overflow pollution |
| CN115893592B (en) * | 2022-11-03 | 2024-05-24 | 北京林业大学 | Rapid purification technology for electro-flocculation in-situ coupling electro-Fenton overflow pollution |
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