CN107601624B - Preparation and application of electro-Fenton cathode material based on supported activated carbon fibers - Google Patents
Preparation and application of electro-Fenton cathode material based on supported activated carbon fibers Download PDFInfo
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- CN107601624B CN107601624B CN201711019400.7A CN201711019400A CN107601624B CN 107601624 B CN107601624 B CN 107601624B CN 201711019400 A CN201711019400 A CN 201711019400A CN 107601624 B CN107601624 B CN 107601624B
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Abstract
The invention discloses a preparation method and application of an electro-Fenton cathode material based on a supported activated carbon fiber. The preparation method of the activated carbon fiber electro-Fenton cathode is simple, the conditions are mild, and the danger possibly generated during transportation and storage is avoided by generating the hydrogen peroxide in situ; the treatment process is clean, and Fe (II) medicament does not need to be continuously added outside, so that the sludge yield is reduced, and secondary pollution is not generated. The invention has the advantages of cheap and easily obtained raw materials, simple preparation method, short treatment period, easy combination with other treatment methods and contribution to large-scale production and comprehensive treatment of organic pollutants.
Description
Technical Field
The invention belongs to the technical field of environmental functional materials and electrochemical water treatment, relates to a heterogeneous electro-Fenton activated carbon fiber cathode, and particularly relates to preparation and application of an electro-Fenton cathode material based on load-type activated carbon fibers.
Background
With economic development and social progress, a wide variety of drugs and personal care products (PPCPs), including prescription drugs and non-prescription drugs, veterinary drugs, cosmetics, artificially synthesized musk, hair dyes, bactericides and the like, are discharged into the water environment, and such novel pollutants are usually easy to be biologically enriched, affect aquatic organisms at low concentrations, and further affect human health. Most PPCPs are discharged into wastewater in raw or converted form into wastewater treatment plants. At present, for the sewage containing trace amount of pollutants difficult to degrade, the sewage is not available at home and abroadAn economical and effective method which can be widely popularized. The electro-Fenton process, as an environmentally friendly advanced oxidation technology for water treatment, draws increasing attention in the treatment of refractory organic pollutants. Since it can generate H in situ2O2Effectively avoiding the danger of transportation and storage. Traditional homogeneous phase electro-Fenton technique is more harsh to pH requirement, is only applicable to at present and handles acidic waste water (pH 2 ~ 4), to neutral and alkaline waste water, need throw with a large amount of acid, alkaline medicament before handling and discharging, greatly increased treatment cost, still can produce a large amount of iron-containing sludge after the reaction, cause secondary pollution.
Due to the above limitations of the homogeneous electro-Fenton system, the research and development of the non-homogeneous electro-Fenton catalyst has been the focus of domestic and foreign research. In patent CN 105905985 a, a decontaminated graphite felt material is used as a cathode, a platinum wire is used as an anode, a saturated calomel electrode is used as a reference electrode, a graphene oxide suspension, 3-4-ethylenedioxythiophene and sodium poly-p-styrenesulfonate mixed solution is used as an electrolyte, and a cyclic voltammetry electropolymerization method is adopted to prepare a modified graphite felt heterogeneous electro-fenton electrode; in patent CN 103496764A, a high oxygen evolution overpotential electrode is used as an anode, an air diffusion electrode is used as a cathode, and polytetrafluoroethylene modified iron-carbon is used as a heterogeneous catalyst to treat dichlorophenol, and the effect of the PTFE-bonded air diffusion electrode on pressure resistance and amplification experiments is yet to be examined.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method and application of an electro-Fenton cathode material based on a supported activated carbon fiber.
In order to achieve the purpose, the invention adopts the technical scheme that:
the preparation method of the electro-Fenton cathode material based on the supported activated carbon fiber comprises the following steps:
(1) pretreating an activated carbon fiber cathode substrate material;
(2) sequentially dipping the pretreated material in a complexing agent and a metal salt solution;
(3) and (5) washing and drying for later use.
The active carbon fiber cathode substrate material is viscose-based active carbon fiber, phenolic-based active carbon fiber, pitch-based active carbon fiber or polyacrylonitrile-based active carbon fiber.
The pretreatment is to ultrasonically soak the glass fiber for 10-30 minutes by using acetone or absolute ethyl alcohol, ultrasonically soak the glass fiber for 10-30 minutes by using 1-3 mol/L nitric acid solution after cleaning, finally clean the glass fiber by using deionized water, and dry the glass fiber for later use.
The complexing agent is one or more of ethylenediamine tetraacetic acid, succinic acid, oxalic acid, oxalate, citric acid and citrate; the metal salt is copper salt and/or iron salt.
And sequentially soaking the pretreated material in a complexing agent for 1-6 h and a metal salt solution for 1-6 h at normal temperature.
In an electro-Fenton system, the electro-Fenton cathode material is used as a cathode, dissolved oxygen in water is reduced on the surface of activated carbon fiber to generate hydrogen peroxide, and the obtained hydrogen peroxide reacts with a metal ion complex loaded on the surface of the activated carbon fiber to generate hydroxyl radicals, so that organic pollutants are degraded through oxidation.
The dissolved oxygen in the water is reduced on the surface of the cathode of the activated carbon fiber to generate hydrogen peroxide under the environmental conditions that: the pH is 2-10, and the temperature is 20-90 ℃.
In the electro-Fenton system, platinum, graphite, boron-doped diamond or metal oxide (RuO)2/Ti、IrO2/Ti、PbO2/Ti or SnO2and/Ti) is an anode.
The electro-Fenton cathode material and a counter electrode can also form an electrolytic cell, and the water flow state is static or flowing and is 0-20 mA/cm2And does not include 0mA/cm2The electrolytic reaction is carried out at a current density.
In the application system of the invention, air or oxygen is injected into the cathode region, or the oxygen generated by electrolyzing water at the anode is utilized to generate hydrogen peroxide in situ.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the conventional heterogeneous Fenton reagent, the method does not need to add hydrogen peroxide externally, effectively avoids the dangers of the reagent in the aspects of transportation and storage, and can control the yield of the hydrogen peroxide and the degradation rate of organic matters by controlling current and voltage.
2. The method adopts the activated carbon fiber as the cathode, has the characteristics of adsorption, conductivity, high specific surface area and the like, has the property of a quasi-three-dimensional electrode, increases the electrode surface of unit cell volume, and improves the current efficiency and the treatment effect.
3. According to the method, the iron ion or copper ion complex is loaded on the surface of the carbon material cathode, hydrogen peroxide can be effectively catalytically decomposed within the range of pH 2-10 to generate hydroxyl radicals, the defects of narrow pH application range and large iron sludge production amount in the traditional Fenton technology are overcome, and the method has good economic, environmental and social benefits.
Drawings
Fig. 1 is a schematic diagram of the application of the present invention.
Fig. 2 is a scanning electron microscope picture of the activated carbon fiber loaded with ferric citrate of the present invention.
Fig. 3 is a schematic diagram showing the comparison of the effects of activated carbon fiber adsorption, activated carbon fiber energization, activated carbon fiber loaded ferric citrate (heterogeneous), activated carbon fiber + ferric citrate (homogeneous), and activated carbon fiber + ferrous sulfate (homogeneous) on ibuprofen removal.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the drawings and examples.
The invention relates to a preparation method of an electro-Fenton cathode material based on load-type activated carbon fibers, which comprises the following steps:
(1) pretreatment: the method comprises the steps of taking viscose-based activated carbon fibers, phenolic-based activated carbon fibers, asphalt-based activated carbon fibers or polyacrylonitrile-based activated carbon fibers as an activated carbon fiber cathode substrate material, ultrasonically soaking the activated carbon fiber cathode substrate material for 10-30 minutes by using acetone or absolute ethyl alcohol, ultrasonically soaking the activated carbon fiber cathode substrate material for 10-30 minutes by using 1-3 mol/L nitric acid solution after cleaning, finally cleaning the activated carbon fiber cathode substrate material by using deionized water, and drying the cleaned activated carbon fiber cathode substrate material for later use.
(2) Sequentially dipping the pretreated material in a complexing agent and a metal salt solution; the complexing agent can be one or more of ethylenediamine tetraacetic acid, succinic acid, oxalic acid, oxalate, citric acid and citrate; the metal salt is copper salt and/or iron salt. The activated carbon fiber is sequentially soaked in the complexing agent for 1-6 h and the metal salt solution for 1-6 h, and the two steps of soaking are carried out at normal temperature.
(3) Washing with deionized water, and drying for use.
Fig. 1 is a schematic diagram of the application of the present invention. The dissolved oxygen in the water is electrochemically and rapidly reduced on the surface of the cathode to generate hydrogen peroxide in situ, the hydrogen peroxide and the iron ion complex loaded on the surface of the carbon cathode are excited to react to generate hydroxyl radicals, and the ibuprofen is oxidatively degraded.
Fig. 2 is a scanning electron microscope image of the activated carbon fiber loaded with the ferric citrate complex, and ferric citrate complex particles are distributed on the smooth surface of the activated carbon fiber.
As shown in FIG. 3, the electro-Fenton cathode material obtained by the invention is used in an electro-Fenton system, and platinum, graphite, boron-doped diamond or metal oxide (RuO)2/Ti、IrO2/Ti、PbO2/Ti or SnO2and/Ti) is used as an anode, the dissolved oxygen in the water is reduced on the surface of the activated carbon fiber to generate hydrogen peroxide, and the obtained hydrogen peroxide reacts with the metal ion complex loaded on the surface of the activated carbon fiber to generate hydroxyl radicals to oxidize and degrade organic pollutants.
Fig. 3 shows a schematic diagram comparing the effects of adsorption by activated carbon fiber, electrification of activated carbon fiber, loading of activated carbon fiber with ferric citrate (heterogeneous), activated carbon fiber + ferric citrate (homogeneous), and activated carbon fiber + ferrous sulfate (homogeneous) on ibuprofen removal. It can be seen that the removal of ibuprofen by activated carbon fiber adsorption and electrification (reduction of oxygen to produce hydrogen peroxide) is not high, while heterogeneous electro-fenton shows good ibuprofen removal rate under pH near-neutral condition, which is equivalent to the removal rate of ibuprofen by homogeneous electro-fenton at pH 3 of 120 min. The active carbon fiber is loaded with ferric citrate (heterogeneous), namely a ferric citrate complex is loaded on the surface of the active carbon fiber; activated carbon fiber + ferric citrate (homogeneous phase), which means that the ferric citrate is dissolved in a solution to be treated; activated carbon fiber + ferrous sulfate (homogeneous), which means that ferrous sulfate is dissolved in the solution to be treated.
Example 1 gives the formation of hydrogen peroxide and hydroxyl radicals during the electro-fenton reaction:
volume of reaction solution: 250mL of high purity water
Temperature of the reaction solution: 30 +/-2 DEG C
Initial pH of reaction solution: 6.8
Electrode area: 15cm2(2.5cm×6cm)
Electrolyte concentration: 0.05M Na2SO4
Oxygen flow rate: 100mL/min
Current intensity: 0.05A
Reaction time: 30min,60min,90min,120min
TABLE 1 concentration of generated oxides
| Concentration of generated oxide | 30min | 60min | 90min | 120min |
| Hydrogen peroxide concentration (μ M) | 104.7 | 141.8 | 163.2 | 182.7 |
| Hydroxyl radical concentration (μ M) | 8.6 | 13.7 | 20.6 | 26.1 |
As can be seen from example 1, the concentration of the generated hydrogen peroxide and hydroxyl radicals increases with increasing reaction time, indicating that this method is effective in exciting hydrogen peroxide to generate strong oxidant hydroxyl radicals under pH neutral conditions.
Example 2 illustrates the removal of ibuprofen of different initial concentrations according to the invention
Volume of reaction solution: 250mL of high purity water
Temperature of the reaction solution: 30 +/-2 DEG C
Initial pH of reaction solution: 6.8
Electrode area: 15cm2(2.5cm×6cm)
Electrolyte concentration: 0.05M Na2SO4
Oxygen flow rate: 100mL/min
Current intensity: 0.05A
Reaction time: 120min
Initial concentration: 1mg/L,5mg/L,10mg/L,20mg/L
Table 2 removal of ibuprofen for different initial concentrations
| Initial concentration (mg/L) | 1 | 5 | 10 | 20 |
| Removal Rate (%) | 98.0 | 97.5 | 96.8 | 94.7 |
As can be seen from example 2, the removal was relatively good for both the low and high concentrations of ibuprofen, 1mg/L to 20mg/L, and greater than 95% for the initial concentration of ibuprofen less than 10 mg/L.
Example 3 shows the effect of different current densities on the ibuprofen removal
Volume of reaction solution: 250mL of high purity water
Temperature of the reaction solution: 30 +/-2 DEG C
Initial pH of reaction solution: 6.8
Initial ibuprofen concentration: 10mg/L
Electrode area: 15cm2(2.5cm×6cm)
Electrolyte concentration: 0.05M Na2SO4
Oxygen flow rate: 100mL/min
Current intensity: 0.05A
Reaction time: 120min
Initial concentration: 1mA/cm2,3mA/cm2,5mA/cm2,7mA/cm2
Table 3 ibuprofen removal at different current densities
| Current Density (mA/cm)2) | 1 | 3 | 5 | 7 |
| Removal Rate (%) | 89.8 | 94.3 | 96.8 | 97.1 |
As can be seen from example 3, the removal of ibuprofen increases with increasing current density, which is higher than 5mA/cm2The removal rate of ibuprofen is not very different.
Example 4 shows the effect of different run cycles on the ibuprofen removal
Volume of reaction solution: 250mL of high purity water
Temperature of the reaction solution: 30 +/-2 DEG C
Initial pH of reaction solution: 6.8
Initial ibuprofen concentration: 10mg/L
Electrode area: 15cm2(2.5cm×6cm)
Electrolyte concentration: 0.05M Na2SO4
Oxygen flow rate: 100mL/min
Current intensity: 0.05A
One cycle is as follows: 120min
Table 4 different run cycles for ibuprofen removal
| Period of operation | 1 | 2 | 3 | 4 | 5 | 6 |
| Removal Rate (%) | 96.7 | 90.6 | 90.7 | 88.8 | 87.4 | 85.3 |
It can be seen from example 4 that, after 6 operating cycles (12 hours), ibuprofen is still well removed (more than 85%), the removal efficiency of the electrode on organic pollutants can be improved by re-loading ferric citrate subsequently, the loading process is mild in condition, short in time and good in application prospect.
In summary, the invention utilizes the electro-Fenton cathode material based on the supported activated carbon fiber, the dissolved oxygen generates hydrogen peroxide on the surface of the cathode of the activated carbon fiber through the oxygen reduction reaction of two electrons, the generated hydrogen peroxide reacts with the iron ion or copper ion complex catalyst loaded on the surface of the activated carbon fiber to generate strong oxidant hydroxyl radical, and the organic matters which are difficult to degrade can be removed by oxidation under the condition of neutral pH. The preparation method of the activated carbon fiber electro-Fenton cathode is simple, the conditions are mild, and the danger possibly generated during transportation and storage is avoided by generating the hydrogen peroxide in situ; the treatment process is clean, and Fe (II) medicament does not need to be continuously added outside, so that the sludge yield is reduced, and secondary pollution is not generated. The invention has the advantages of cheap and easily obtained raw materials, simple preparation method, short treatment period, easy combination with other treatment methods and contribution to large-scale production and comprehensive treatment of organic pollutants. The application of the method is a method for treating the electro-Fenton wastewater, which can continuously add the ferric salt, has wide pH application range, is particularly suitable for the electro-Fenton wastewater under the near-neutral condition, and has great application prospect.
Claims (7)
1. The preparation method of the electro-Fenton cathode material based on the supported activated carbon fiber is characterized by comprising the following steps of:
(1) taking an activated carbon fiber cathode substrate material for pretreatment, wherein the pretreatment comprises the steps of ultrasonically soaking the activated carbon fiber cathode substrate material by using acetone or absolute ethyl alcohol, ultrasonically soaking the activated carbon fiber cathode substrate material by using a nitric acid solution after cleaning, and finally cleaning and drying the activated carbon fiber cathode substrate material for later use;
(2) sequentially soaking the pretreated material in a complexing agent for 1-6 hours and a metal salt solution for 1-6 hours at normal temperature, wherein the complexing agent is one or more of ethylenediamine tetraacetic acid, succinic acid, oxalic acid, oxalate, citric acid and citrate; the metal salt is copper salt and/or iron salt;
(3) and (5) washing and drying for later use.
2. The preparation method of the electro-Fenton cathode material based on the supported activated carbon fiber according to claim 1, wherein the activated carbon fiber cathode base material is viscose-based activated carbon fiber, phenolic-based activated carbon fiber, pitch-based activated carbon fiber or polyacrylonitrile-based activated carbon fiber.
3. The use of the electro-Fenton cathode material based on supported activated carbon fibers as claimed in claim 1, wherein in the electro-Fenton system, the electro-Fenton cathode material is used as a cathode, dissolved oxygen in water is reduced on the surface of the activated carbon fibers to generate hydrogen peroxide, and the obtained hydrogen peroxide reacts with the metal ion complex loaded on the surface of the activated carbon fibers to generate hydroxyl radicals, so as to oxidatively degrade the organic pollutant which is ibuprofen.
4. The use of claim 3, wherein the dissolved oxygen in the water is reduced on the cathode surface of the activated carbon fiber to generate hydrogen peroxide under the following environmental conditions: the pH is 2-10, and the temperature is 20-90 ℃.
5. Use according to claim 3, wherein the electro-Fenton system is anodised by platinum, graphite, boron-doped diamond or a metal oxide.
6. The use of claim 3, wherein the electro-Fenton cathode material and the counter electrode are combined to form an electrolytic cell, and the water flow state is static or flowing and is 0-20 mA/cm2And does not include 0mA/cm2The electrolytic reaction is carried out at a current density.
7. Use according to claim 6, wherein hydrogen peroxide is generated in situ by injection of air or oxygen in the cathode region or by oxygen generated by electrolysis of water at the anode.
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