CN107324453A - A kind of Fe FeOx/ charcoal-aero gel self-supporting cathode preparation method and the electric Fenton degraded methyl orange system of out-phase - Google Patents
A kind of Fe FeOx/ charcoal-aero gel self-supporting cathode preparation method and the electric Fenton degraded methyl orange system of out-phase Download PDFInfo
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- CN107324453A CN107324453A CN201710540768.1A CN201710540768A CN107324453A CN 107324453 A CN107324453 A CN 107324453A CN 201710540768 A CN201710540768 A CN 201710540768A CN 107324453 A CN107324453 A CN 107324453A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
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- 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
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- C02F2101/00—Nature of the contaminant
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Abstract
The invention provides a kind of Fe FeOx/ charcoal-aero gel self-supporting cathode preparation method and the electric Fenton degraded methyl orange system of out-phase, belong to Environmental electrochemistry material and prepare and high-level oxidation technology processing waste water technology field.Fe FeO are prepared by the method for one-step synthesis collosol and gelx/ carbon aerogel electrodes, make negative electrode；With Ti/RuO2‑IrO2Electrode makees anode；Under conditions of additional power source, methyl orange of degrading；The electric Fenton of the out-phase of the present invention has the extensive pH value range of comparison, is adapted to various actual waste waters；The electrode of preparation is certainly into block, it is not necessary to the complicated post-processing such as tabletting；In situ it can produce H2O2, it is to avoid the danger of shipping storage, reduce cost；Iron precipitation is limited, catalyst can be recycled；Reactant is cooked with electronics, process cleans are environment-friendly；Electrode material is except with catalysed oxidn, being also accompanied by the synergy such as absorption.
Description
Technical field
Prepared the invention belongs to Environmental electrochemistry material and high-level oxidation technology processing waste water technology field, be related to negative electrode
The preparation of material, using charcoal-aero gel as substrate, by Fe-FeOxLoad in substrate, then with Fe-FeOx/ charcoal-aero gel (FCAs)
Make negative electrode to degrade methyl orange by electric Fenton mode.
Background technology
Electric Fenton by using cleaning, efficient electronics as reactant generate strong oxidizing property hydroxyl radical free radical (
OH), each pollutant of degraded that can be without selection, simple to operate, reaction condition is easily-controllable, environment-friendly, is closed extensively in recent years
Note.Its reaction mechanism is to be based on H2O2And Fe2+Simultaneously a series of chain reaction degradation of contaminant occur for reaction generation OH.H2O2It is
Dissolved oxygen in reaction system generates H under the catalytic action of appropriate cathode material by occurring two electronic reduction reactions2O2,
Then by Fe2+Catalytic decomposition produces strong oxidizing property OH.According to Fe2+Existence difference electric Fenton can be divided into homogeneous electricity
Fe in Fenton and the electric Fenton of out-phase, homogeneous electricity Fenton2+With Fe of the form dissolving of ion in the solution and in the electric Fenton of out-phase2+
It is present in the form of solid in catalyst.Compared to homogeneous electric Fenton, out-phase electricity Fenton has its unique advantage, such as compares
Extensive pH value range, limitation iron precipitation and catalyst be may be reused, therefore the electric Fenton of out-phase was studied in recent years
The extensive concern of person.Cathode material is the emphasis that researchers study all the time in electro-fenton process, finds suitable negative electrode
Material has important practical significance for the development in electrochemical environment field.
Charcoal-aero gel (carbon aerogels, CAs) is a kind of lightweight, porous, amorphous state, block nanometer Carbon Materials, and
And be unique conductive aeroge.Therefore charcoal-aero gel can be used as the carrier, cell negative electrode material, double electricity of catalyst
Layer capacitor etc..Resorcinol and formaldehyde based charcoal aerogel be research earliest and most charcoal-aero gel, it earliest by
What professor R.W.Pekala synthesized first, using resorcinol and formaldehyde as presoma, dried and obtained by supercritical carbon dioxide.
The present invention prepares FCAs cathode materials by the method for one-step synthesis.Using resorcinol and formaldehyde as presoma, with
Ferrous sulfate heptahydrate (FeSO4·7H2O it is) source of iron, is obtained by normal temperature and pressure drying and high temperature carbonization.Whole electrochemical system
It is simultaneously with Ti/RuO using FCAs negative electrode2-IrO2As anode, under conditions of additional power source, optimize the degraded of methyl orange
Condition, makes methyl orange reach the purpose of degraded.
The content of the invention
It is difficult to present invention is generally directed to homogeneous electro-Fenton reaction condition harshness, base material in current electrochemical oxidation process
The problems such as shaping and azo dyes are difficult to degraded, a kind of FCAs cathode materials of self-supporting are prepared, pass through the electric Fenton of out-phase
Method degraded methyl orange.This method is easy to operate, convenient and easy, and reactant is simple, can realize electro-Fenton reaction mild condition
Control is simultaneously certainly into electrode and methyl orange degradation etc..
Technical scheme：
A kind of Fe-FeOx/ charcoal-aero gel self-supporting cathode preparation method, step is as follows：
(1) it is in molar ratio 1 using resorcinol and formaldehyde as reactant:2 mixing, using deionized water as solvent, are adjusted
The mass percent of reactant is saved, by the experiment experience of early stage, optimization obtains what the total concentration of reactant was prepared for 40%
Preferably, adding appropriate sodium carbonate as catalyst, (mass ratio of resorcinol and sodium carbonate is 1000 to charcoal-aero gel effect:
1), while adding appropriate FeSO4·7H2O is used as source of iron (FeSO4·7H2O quality and total matter of resorcinol and formaldehyde
Than no more than 5%), 2h is sufficiently stirred at room temperature is sufficiently mixed solution to amount, mixed liquor is transferred in closed container, i.e. shape
Into the organosol of iron content.
(2) closed container for filling mixed solution is placed in electric heating air blast thermostatic drying chamber (or thermostat water bath)
Sol gel reaction is carried out, 25 DEG C are reacted one day, and 50 DEG C are reacted one day, and 90 DEG C are reacted three days.The RF for forming iron content is organic solidifying
Glue.
(3) RF organogels are placed on the trifluoroacetic acid that volume fraction is 3% (volume ratio of trifluoroacetic acid and acetone is 3:
100) it is aged for one day in, then places it in that surface tension coefficient is smaller again and place three in volatile organic solvent-acetone
My god, purpose changes once fresh acetone per 24h to replace the moisture in RF organogels.Then by after exchange of solvent
RF organogels put at normal temperatures and pressures dry 3 days, that is, obtain organic xerogel of iron content.
(4) organic xerogel is positioned in high temperature process furnances, under atmosphere of the nitrogen as protective gas, heating rate
5 DEG C/min, 300 DEG C of holdings 1h, 600 DEG C of holdings 1h, 900 DEG C of holding 5h are set to, FCAs is finally obtained.The Fe loads prepared
Amount is respectively 0%, 0.5%, 5% FCAs, and its density is respectively 0.3309g/cm3、0.4606g/cm3、0.4642g/cm3；
Electrical conductivity is respectively 26.67S/cm, 30.07S/cm, 43.48S/cm；Specific surface area is respectively 495.225m2/g、
406.369m2/g、377.063m2/g；Micro pore volume is respectively 0.2864cm3/g、0.2571cm3/g、0.2404cm3/g.Prepare
The FCAs physical properties gone out are good, can be used as cathode material.
One kind Fe-FeOxThe electric Fenton degraded methyl orange system of the out-phase of/charcoal-aero gel self-supporting negative electrode, its feature exists
In Fe-FeOx/ charcoal-aero gel self-supporting electrode is as negative electrode, with Ti/RuO2-IrO2For anode, under conditions of additional power source,
PEM exposes air as the barrier film between cathode chamber and anode chamber, cathodic region, methyl orange of degrading.
The preparation of cathode material：The FCAs electrodes of self-supporting are prepared by above-mentioned one-step method for synthesizing, high (H) is
3cm, diameter (D) is 2cm.
Anode material：Anode is purchased from the occasion Ti electrode Manufacturing Co., Ltd of Baoji one, 3cm × 4cm.
Reactor：Be sticked with and formed by lucite, PEM as barrier film, the purpose for placing barrier film be in order to avoid
The mixing of the two poles of the earth product, prevents side reaction and secondary reaction, so that purity and current efficiency of influence product etc..Prepare first
Base orange simulated wastewater, adds appropriate anhydrous sodium sulfate (Na2SO4) electrical conductivity of simulated wastewater is adjusted as electrolyte
Section, the anode chamber and the cathode chamber is separately added into appropriate above-mentioned methyl orange simulated wastewater, using the decolouring of methyl orange as evaluation index, in 464nm
Wavelength under, using visible spectrophotometer (VIS) carry out spectrum analysis, determine water sample absorbance.It is different by changing because
Element (the orange concentration of Fe load capacity, electric current, aeration quantity, initial pH, initial) investigates the degradation effect of methyl orange, optimal to determine
Methyl orange degradation condition, be the later stage realize industrialization target do early-stage preparations.Considering to meet actual waste water and reducing into
On the premise of this, the degradation effect condition of optimal methyl orange is drawn, is 50mA in electric current, aeration quantity is 1.4L/min, initial pH
=7, initial orange concentration is 150mg/L, and the FCAs electrodes using Fe load capacity as 5% are as negative electrode, by 180min electricity
Chemical treatment, percent of decolourization has reached 100%.
The invention has the advantages that 1) the out-phase electro-Fenton reaction formed using FCAs negative electrode has extensive pH
(between 3-9) value scope；2) electrode prepared is directly available to do electrode from into block, it is not necessary to other complexity such as tabletting
Post-processing；3) charcoal-aero gel substrate inherently has adsorptivity, therefore cathode material not only there is electrochemical catalytic oxidation to make
With, it is also accompanied by Electro Sorb etc. and acts synergistically, the degradation effect of reinforcement methyl orange.In addition the method for electrochemical regeneration can make the moon
Pole material activity recovery, reaches the purpose of recycling.
Brief description of the drawings
Fig. 1 is electrochemical reaction appts figure.
Fig. 2 (2.1,2.2,2.3) is that three negative electrode absorption properties of contrast and electrochemistry oxidation performance are imitated to methyl orange
The influence figure and influence figure of the Fe load capacity to methyl orange effect of fruit.
Fig. 2 .1 are CAs electrodes；Fig. 2 .2 are the FCAs electrodes that Fe load capacity is 0.5%；Fig. 2 .3 are that Fe load capacity is 5%
FCAs electrodes.
Fig. 3 is influence figure of the electric current to methyl orange effect.
Fig. 4 is influence figure of the aeration quantity to methyl orange effect.
Fig. 5 is influence figures of the initial pH to methyl orange effect.
Fig. 6 is influence figure of the orange concentration of initial to methyl orange effect.
In figure：1 dc source；2 anode regions；3 barrier films；4 cathodic regions；5 aeration heads；6 spinner flowmeters；7 air bottles.
Embodiment
The outstanding feature of the present invention and marked improvement are further elucidated with reference to embodiment, this hair of explanation is only that
It is bright and be in no way limited to following instance.The present invention uses homemade self-supporting Fe-FeOx/ carbon aerogel electrodes are used as negative electrode and right
Its electrochemical oxidation effect is tested.
Embodiment 1：The absorption property and electrochemistry oxygen of Different electrodes material (Fe load capacity is respectively 0%, 0.5%, 5%)
Change influence of the performance to the test of methyl orange Contrast on effect and difference Fe load capacity to methyl orange effect to test.
Reaction condition：Methyl orange simulated wastewater 150mg/L is prepared, appropriate Na is added2SO4The electrical conductivity of solution is adjusted, it is cloudy
Anode chamber is separately added into the above-mentioned solution of 60mL, and the FCAs electrodes using Fe load capacity as 0%, 0.5% and 5% are as negative electrode, in pH
=7, aeration quantity is 1.4L/min, under conditions of electric current is 0mA and 50mA, reacts 180min, determines the concentration of methyl orange simultaneously
Calculate its percent of decolourization.
As a result it is as shown in Figure 2：Fig. 2 .1 are that Fe load capacity is 0% cathode material, as a result show its absorption property and electrochemistry
Oxidation susceptibility is not very big to the decolorizing effect difference of methyl orange, and absorption property accounts for leading, and electrochemistry oxidation performance is due to the moon
Pole material produces H under conditions of aeration2O2Make methyl orange degradation.Fig. 2 .2 are that Fe load capacity is 0.5% cathode material, as a result
Show that absorption property is significantly reduced, being primarily due to the addition of iron makes the ratio surface of cathode material and micro pore volume reduce.This
Outside, electrochemistry oxidation performance increased but not notable, very few mainly due to iron load capacity, and the OH amounts of generation are few.Figure
2.3 be that Fe load capacity is 5% cathode material, as a result shows absorption property reduction, electrochemistry oxidation performance enhancing, by 180min
The percent of decolourization of methyl orange reaches 100%.Complex chart 2.1,2.2 and 2.3 is drawing a conclusion that Fe load capacity is 5% FCAs electrodes
With optimal electrochemical oxidation effect.
Embodiment 2：By 5%FCAs electrodes of Fe load capacity as negative electrode, shadow of the electric current to methyl orange effect is investigated
Ring.
Reaction condition：Methyl orange simulated wastewater 150mg/L is prepared, appropriate Na is added2SO4The electrical conductivity of solution is adjusted, it is cloudy
Anode chamber is separately added into the above-mentioned solution of 60mL, and the FCAs electrodes using Fe load capacity as 5%, as negative electrode, are 1.4L/ in aeration quantity
Min, pH=7, investigate electric current under conditions of 10mA, 30mA and 50mA, to react 180min, the percent of decolourization of methyl orange.
As a result it is as shown in Figure 3：With the increase of electric current, the percent of decolourization of methyl orange is remarkably reinforced, by 180min,
Under conditions of 10mA, 30mA and 50mA, percent of decolourization is respectively 52.59%, 77.05% and 100%.
Embodiment 3：By 5%FCAs electrodes of Fe load capacity as negative electrode, aeration quantity is investigated to methyl orange effect
Influence.
Reaction condition：Methyl orange simulated wastewater 150mg/L is prepared, appropriate Na is added2SO4The electrical conductivity of solution is adjusted, it is cloudy
Anode chamber is separately added into the above-mentioned solution of 60mL, and the FCAs electrodes using Fe load capacity as 5%, as negative electrode, are 50mA, pH in electric current
=7, aeration quantity is investigated under conditions of 0L/min, 0.7L/min and 1.4L/min, to react 180min, the percent of decolourization of methyl orange.
As a result it is as shown in Figure 4：With the increase of aeration quantity, the percent of decolourization of methyl orange is remarkably reinforced, by 180min,
Under conditions of 0L/min, 0.7L/min and 1.4L/min, percent of decolourization is respectively 48.79%, 95.10% and 100%.
Embodiment 4：By 5%FCAs electrodes of Fe load capacity as negative electrode, influences of the pH to methyl orange effect is investigated.
Reaction condition：Methyl orange simulated wastewater 150mg/L is prepared, appropriate Na is added2SO4The electrical conductivity of solution is adjusted, it is cloudy
Anode chamber is separately added into the above-mentioned solution of 60mL, and the FCAs electrodes using Fe load capacity as 5% are 50mA in electric current, exposed as negative electrode
Tolerance is 1.4L/min, investigates under conditions of pH=3, pH=7 and pH=11, reacts 180min, the percent of decolourization of methyl orange.
As a result it is as shown in Figure 5：With pH increase, different variation tendencies are presented in the percent of decolourization of methyl orange, by 180min,
Under conditions of pH=3, pH=7 and pH=11, percent of decolourization reaches 100%.Under conditions of pH=3, by 160min,
The percent of decolourization of methyl orange just reaches 100%.
Embodiment 5：By 5%FCAs electrodes of Fe load capacity as negative electrode, methyl orange initial concentration is investigated de- to methyl orange
The influence of color effect.
Reaction condition：Methyl orange simulated wastewater is prepared, concentration is respectively 100mg/L, 150mg/L and 200mg/L, is added suitable
The Na of amount2SO4The electrical conductivity of solution is adjusted, the anode chamber and the cathode chamber is separately added into the above-mentioned solution of 60mL, the FCAs using Fe load capacity as 5%
Electrode, as negative electrode, is 50mA in electric current, pH=7, aeration quantity tests methyl under conditions of 1.4L/min, to react 180min
The percent of decolourization of orange.
As a result it is as shown in Figure 6：With the increase of methyl orange initial concentration, the percent of decolourization of methyl orange is gradually reduced, and concentration is
100mg/L methyl orange, by 140min, the percent of decolourization of methyl orange just reaches 100%.Concentration is 150mg/L methyl orange, warp
180min is crossed, the percent of decolourization of methyl orange reaches 100%.And concentration is 200mg/L methyl orange, by 180min, methyl orange
Percent of decolourization only reaches 90.6%.
Claims (2)
1. a kind of Fe-FeOx/ charcoal-aero gel self-supporting cathode preparation method, it is characterised in that step is as follows：
(1) it is in molar ratio 1 using resorcinol and formaldehyde as reactant:2 mixing, using deionized water as solvent, regulation is anti-
The mass percent concentration for answering thing is 40%；Sodium carbonate is added as catalyst, the mass ratio of resorcinol and sodium carbonate is
1000:1, while adding FeSO4·7H2O is used as source of iron, FeSO4·7H2O quality and resorcinol and the total mass ratio of formaldehyde
No more than 5%；It is stirred well to and is thoroughly mixed at room temperature, mixed liquor is transferred in closed container, that is, form iron content has
Machine colloidal sol；
(2) organosol of iron content is placed under constant temperature and carries out sol gel reaction, 25 DEG C are reacted one day, 50 DEG C of reactions
One day, 90 DEG C were reacted three days, form the RF organogels of iron content；
(3) the RF organogels of iron content are positioned in the acetone soln for the trifluoroacetic acid that volume fraction is 3% and be aged for one day, so
Place it in acetone and place three days again afterwards, an acetone is changed per 24h；Then the RF organogels after exchange of solvent are placed on
Dried 3 days under normal temperature and pressure, that is, obtain organic xerogel of iron content；
(4) under atmosphere of the nitrogen as protective gas, heating rate is set to 5 DEG C/min, by organic xerogel in 300 DEG C of temperature
Keep keeping keeping 5h under 1h, 900 DEG C of temperature conditionss under 1h, 600 DEG C of temperature conditionss under the conditions of degree, obtain Fe-FeOxThe airsetting of/charcoal
Glue self-supporting negative electrode.
2. one kind Fe-FeOxThe electric Fenton degraded methyl orange system of the out-phase of/charcoal-aero gel self-supporting negative electrode, it is characterised in that
Fe-FeOx/ charcoal-aero gel self-supporting negative electrode is as negative electrode, with Ti/RuO2-IrO2For anode, under conditions of additional power source, matter
Proton exchange exposes air as the barrier film between cathode chamber and anode chamber, cathodic region, methyl orange of degrading.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108751382A (en) * | 2018-07-11 | 2018-11-06 | 常州大学 | A kind of preparation method of electricity Fenton packing material |
| CN109516641A (en) * | 2018-12-17 | 2019-03-26 | 南通寰宇博新化工环保科技有限公司 | Method for treating high-salt high-concentration organic wastewater by electrocatalytic oxidation-biochemical coupling |
| CN113479976A (en) * | 2021-07-27 | 2021-10-08 | 南京理工大学 | Integrated wastewater treatment device and application thereof |
| CN114368807A (en) * | 2022-01-14 | 2022-04-19 | 中国科学技术大学 | Preparation method and application of chitosan-coated electro-Fenton cathode |
| CN114538569A (en) * | 2022-02-25 | 2022-05-27 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell0/FeOxGranular electro-Fenton cathode and preparation and application thereof |
| CN114604943A (en) * | 2022-05-12 | 2022-06-10 | 清华大学深圳国际研究生院 | Wastewater treatment device and wastewater treatment method by cathode electro-Fenton coupling anodic oxidation |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108751382A (en) * | 2018-07-11 | 2018-11-06 | 常州大学 | A kind of preparation method of electricity Fenton packing material |
| CN109516641A (en) * | 2018-12-17 | 2019-03-26 | 南通寰宇博新化工环保科技有限公司 | Method for treating high-salt high-concentration organic wastewater by electrocatalytic oxidation-biochemical coupling |
| CN113479976A (en) * | 2021-07-27 | 2021-10-08 | 南京理工大学 | Integrated wastewater treatment device and application thereof |
| CN114368807A (en) * | 2022-01-14 | 2022-04-19 | 中国科学技术大学 | Preparation method and application of chitosan-coated electro-Fenton cathode |
| CN114368807B (en) * | 2022-01-14 | 2023-03-10 | 中国科学技术大学 | Preparation method and application of chitosan-coated electro-Fenton cathode |
| CN114538569A (en) * | 2022-02-25 | 2022-05-27 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell0/FeOxGranular electro-Fenton cathode and preparation and application thereof |
| CN114538569B (en) * | 2022-02-25 | 2023-03-10 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell 0 /FeO X Granular electro-Fenton cathode and preparation and application thereof |
| CN114604943A (en) * | 2022-05-12 | 2022-06-10 | 清华大学深圳国际研究生院 | Wastewater treatment device and wastewater treatment method by cathode electro-Fenton coupling anodic oxidation |
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