CN110194519B - Method for efficiently removing 1, 4-dioxane by pulse electro-Fenton - Google Patents

Method for efficiently removing 1, 4-dioxane by pulse electro-Fenton Download PDF

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CN110194519B
CN110194519B CN201910453680.5A CN201910453680A CN110194519B CN 110194519 B CN110194519 B CN 110194519B CN 201910453680 A CN201910453680 A CN 201910453680A CN 110194519 B CN110194519 B CN 110194519B
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electrode
iron
dioxane
cathode
inert
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CN110194519A (en
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刘广立
施华磊
卢耀斌
曾翠平
骆海萍
张仁铎
崔婉俊
韦士程
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Sun Yat Sen University
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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
    • 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
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • 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
    • 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
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/026—Fenton's reagent
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/10—Biological treatment of water, waste water, or sewage

Abstract

The invention relates to a method for efficiently removing 1, 4-dioxane by pulse electro-Fenton. The method comprises the following steps: s1: constructing a reactor by taking an inert electrode and an iron electrode as anodes, an air electrode as a cathode and artificial wastewater containing 1, 4-dioxane as electrolyte; s2: alternately electrifying the inert electrode and the iron electrode, and continuously electrifying the cathode to form pulse current. The method provided by the invention electrolyzes to generate hydrogen peroxide and ferrous ions, and the hydrogen peroxide and the ferrous ions react to generate hydroxyl radicals with strong oxidizing property to perform oxidation reaction with the pollutant 1, 4-dioxane, so that the high-efficiency degradation of the pollutant is realized. Meanwhile, the content of hydrogen peroxide and ferrous ions is controlled by pulses to achieve a better reaction ratio, so that the occurrence of side reactions caused by the excessive ferrous ions is effectively reduced, the full utilization of the hydrogen peroxide is realized to a greater extent, and the energy consumption and the generation of iron mud of the method are greatly reduced.

Description

Method for efficiently removing 1, 4-dioxane by pulse electro-Fenton
Technical Field
The invention belongs to the field of electrochemical advanced oxidation, and particularly relates to a method for efficiently removing 1, 4-dioxane by pulse electro-Fenton.
Background
1, 4-dioxane is a cyclic organic pollutant which is also classified as a class 2B (possible) human carcinogen. 1, 4-dioxane is widely used as a solvent for industrial product production, a stabilizer such as paint, cosmetics, a deodorant, etc., and is also formed as a by-product in the production of other organic agents such as surfactants. Due to the stable chemical structure, the 1, 4-dioxane has the characteristics of high water solubility, difficult biodegradation and the like, so that the conventional common sewage treatment methods such as an activated sludge method, an activated carbon adsorption method, a flocculation method and the like can not effectively and efficiently remove the pollutants, and the electro-Fenton advanced oxidation technology can effectively remove the pollutants, but has the problems of high energy consumption, large amount of byproduct iron sludge and the like.
Therefore, it is necessary to develop a treatment method capable of removing 1, 4-dioxane with high efficiency and low cost.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of high energy consumption and large amount of byproduct iron mud in the existing electro-Fenton advanced oxidation technology for removing 1, 4-dioxane, and provides a method for efficiently removing 1, 4-dioxane by pulse electro-Fenton. The method provided by the invention utilizes the cathode to generate hydrogen peroxide, the iron electrode is used as a sacrificial anode to generate ferrous ions, and the hydrogen peroxide and the ferrous ions react to generate hydroxyl radicals with strong oxidizing property to perform oxidation reaction with the 1, 4-dioxane of the pollutant, thereby realizing the high-efficiency degradation of the pollutant. Meanwhile, the content of hydrogen peroxide and ferrous ions is controlled by pulses to achieve a better reaction ratio, so that the occurrence of side reactions caused by the excessive ferrous ions is effectively reduced, the full utilization of the hydrogen peroxide is realized to a greater extent, and the energy consumption and the generation of iron mud of the method are greatly reduced. The pulse electro-Fenton method provided by the invention can remove more than 95% of 200mg/L, 2, 4-dioxane within 2h, so that the pollutants are efficiently removed, and meanwhile, compared with the traditional electro-Fenton method, the pulse electro-Fenton method has the advantages of low energy consumption, small amount of byproduct iron mud and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for efficiently removing 1, 4-dioxane by pulse electro-Fenton comprises the following steps:
s1: constructing a reactor by taking an inert electrode and an iron electrode as anodes, an air electrode as a cathode and artificial wastewater containing 1, 4-dioxane as electrolyte;
s2: alternately electrifying the inert electrode and the iron electrode, and continuously electrifying the cathode to form pulse current; the ratio of the current passing through the inert electrode once to the current passing through the iron electrode is 4-6: 1; the ratio of the electrifying time of the single inert electrode to the electrifying time of the iron electrode is 1-8: 1.
When the inert electrode and the cathode are electrified, the cathode is in contact with air, and water molecules are catalyzed to generate hydrogen peroxide under the action of electricity; when the iron electrode and the cathode are electrified, the iron electrode is used as a sacrificial anode to generate ferrous ions, hydrogen peroxide reacts with the ferrous ions to generate hydroxyl radicals with strong oxidizing property to perform oxidation reaction with 1, 4-dioxane of pollutants, and efficient degradation of the pollutants is realized. Meanwhile, the content of hydrogen peroxide and ferrous ions is controlled by pulses to achieve a better reaction ratio, so that the occurrence of side reactions caused by the excessive ferrous ions is effectively reduced, the full utilization of the hydrogen peroxide is realized to a greater extent, and the energy consumption and the generation of iron mud of the method are greatly reduced. The pulse electro-Fenton method provided by the invention can remove more than 95% of 200mg/L, 2, 4-dioxane within 2h, so that the pollutants are efficiently removed, and meanwhile, compared with the traditional electro-Fenton method, the pulse electro-Fenton method has the advantages of low energy consumption, small amount of byproduct iron mud and the like.
Inert electrodes conventionally used in the art for the electrolytic generation of hydrogen peroxide may be used in the present invention.
Preferably, the inert electrode in S1 is a platinum electrode, an iridium ruthenium electrode, a titanium plate, or a graphite electrode.
The electrodes are conventional oxygen evolution anodes with better performance.
More preferably, the inert electrode in S1 is a platinum electrode.
The iron electrode may be in a conventional electrode configuration.
Preferably, the iron electrode in S1 is an iron mesh, an iron sheet, or an iron plate.
More preferably, the iron electrode in 1 is an iron mesh.
Air electrodes conventional in the art may be used in the present invention.
Preferably, the air electrode in S1 includes a catalytic layer and a diffusion layer; the catalyst layer is one or more of activated carbon, carbon black or graphite; the diffusion layer is one or more of carbon black, activated carbon or graphite.
Preferably, the catalytic layer is carbon black and the diffusion layer is carbon black.
Specifically, the air electrode is prepared by the following method:
the gas diffusion cathode consists of a diffusion layer, a stainless steel metal net and a catalytic layer. Firstly, a diffusion layer is loaded on one surface of a stainless steel metal net, and carbon black (Vulcan XR-72, Cabot corp., USA) is dissolved by absolute ethyl alcohol and is evenly mixed by ultrasonic stirring, and then the weight ratio of the carbon black is as follows: adding PTFE emulsion into Polytetrafluoroethylene (PTFE) according to the mass ratio of 3:7, stirring and mixing uniformly again, then heating to volatilize absolute ethyl alcohol to prepare dough, rolling to a stainless steel metal net through a rolling machine, and heating for 30min at the temperature of 340 ℃; then a catalytic layer is loaded on the other side of the stainless steel metal mesh, and carbon black (EC-300J, Hesen electric co.ltd., Shanghai, China) is dissolved by absolute ethyl alcohol and mixed uniformly by ultrasonic stirring, and then the mixture is mixed according to the ratio of carbon black: adding PTFE emulsion into Polytetrafluoroethylene (PTFE) according to the mass ratio of 3:1, stirring and uniformly mixing the mixture again, then heating and volatilizing absolute ethyl alcohol to prepare a dough shape, rolling the dough shape to the other surface of the stainless steel metal net loaded with the diffusion layer through a roller press, and airing and volatilizing residual absolute ethyl alcohol.
Preferably, the electrolyte in S1 is circulated.
More preferably, the flow rate of the electrolyte in S1 is 5-50 mL/min.
Most preferably, the electrolyte is circulated in S1 at a flow rate of 35 mL/min.
Preferably, the iron electrode in S1 is disposed between the inert electrode and the cathode; the distance between the inert electrode and the cathode electrode is 2.5-4.0 cm, and the distance between the iron electrode and the cathode electrode is 1.0-3.0 cm.
More preferably, the distance between the inert electrode and the cathode electrode is 3.5cm, and the distance between the iron electrode and the cathode electrode is 2.0 cm.
Preferably, the ratio of the current passing through the inert electrode and the current passing through the iron electrode in a single pass in S2 is 5: 1; the ratio of the energization time of the single inert electrode to the energization time of the iron electrode was 4: 3.
More preferably, the current passing through the inert electrode in the S2 is 35mA for a single time, and the electrifying time is 0.4S; in S2, the current passing through the iron electrode in a single pass was 7mA, and the energization time was 0.3S.
Under the condition, the content of hydrogen peroxide and ferrous ions can be controlled to achieve the optimal proportion of the reaction, the occurrence of side reactions caused by the excessive ferrous ions is effectively reduced, the full utilization of the hydrogen peroxide is realized to the maximum extent, and the energy consumption and the generation of iron mud of the method are greatly reduced.
Preferably, the total time of energization in S2 is not less than 2 h.
Preferably, the energization time is controlled using a time relay in S2.
Compared with the prior art, the invention has the following beneficial effects:
the method provided by the invention utilizes the cathode to generate hydrogen peroxide, the iron electrode is used as a sacrificial anode to generate ferrous ions, and the hydrogen peroxide and the ferrous ions react to generate hydroxyl radicals with strong oxidizing property to perform oxidation reaction with the 1, 4-dioxane of the pollutant, thereby realizing the high-efficiency degradation of the pollutant. Meanwhile, the content of hydrogen peroxide and ferrous ions is controlled by pulses to achieve a better reaction ratio, so that the occurrence of side reactions caused by the excessive ferrous ions is effectively reduced, the full utilization of the hydrogen peroxide is realized to a greater extent, and the energy consumption and the generation of iron mud of the method are greatly reduced. The pulse electro-Fenton method provided by the invention can remove more than 95% of 200mg/L, 2, 4-dioxane within 2h, so that the pollutants are efficiently removed, and meanwhile, compared with the traditional electro-Fenton method, the pulse electro-Fenton method has the advantages of low energy consumption, small amount of byproduct iron mud and the like.
Drawings
FIG. 1 is a schematic diagram of the connection of a pulse electro-Fenton reaction system;
FIG. 2 is a graph of 1, 4-dioxane concentration ratio versus time under different gradient of platinum electrode to iron electrode energization time ratios according to the method provided in example 1;
FIG. 3 is a graph of energy consumption-removal rate per unit mass of 1, 4-dioxane removed by the method provided in example 1 under different power-on time proportional gradients of a platinum electrode and an iron electrode;
FIG. 4 is a graph of 1, 4-dioxane concentration ratio versus time for different switching frequency gradients of a platinum electrode and an iron electrode according to the method provided in example 1;
FIG. 5 is a graph of energy consumption per unit mass of 1, 4-dioxane removal rate versus different switching frequency gradients of a platinum electrode and an iron electrode according to the method provided in example 1;
FIG. 6 is a 1, 4-dioxane concentration ratio versus time curve for the process provided in comparative example 1;
FIG. 7 is a graph of energy consumption per unit mass of 1, 4-dioxane and removal rate for the process provided in comparative example 1.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specifying specific conditions in the examples below, generally according to conditions conventional in the art or as recommended by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
1, 4-dioxane is dissolved in 100mmol/L sodium sulfate solution to prepare the artificial wastewater with the concentration of 200 mg/L. The concentration condition is far higher than the concentration of 1, 4-dioxane in the conventional sewage, and the artificial wastewater is used as the liquid to be treated (electrolyte) in each embodiment and comparative example of the invention.
The concentration and degradation path of the pollutant in the wastewater are analyzed by utilizing High Performance Liquid Chromatography (HPLC), Ion Chromatography (IC) and gas chromatography-mass spectrometry (GC-MS) together, and the removal effect of the pollutant 1, 4-dioxane in each embodiment and comparative example is determined.
Example 1
This example provides a method for removing 1, 4-dioxane with high efficiency by pulsed electro-fenton, which comprises the following steps.
(1) As shown in figure 1, the anode of the reaction system is a platinum electrode and an iron net, the distance between the platinum electrode and the cathode is 3.5cm and 2.0cm respectively, wherein the iron net is oxidized under the action of electricity to generate ferrous ions to participate in Fenton reaction. The cathode consists of a catalyst layer and a diffusion layer, the diffusion layer is directly contacted with air, the catalyst layer catalyzes water molecules to generate hydrogen peroxide to participate in Fenton reaction under the action of electricity, and the cathode is prepared by the following processes: the gas diffusion cathode consists of a diffusion layer, a stainless steel metal net and a catalytic layer. Firstly, a diffusion layer is loaded on one surface of a stainless steel metal net, and carbon black (Vulcan XR-72, Cabot corp., USA) is dissolved by absolute ethyl alcohol and is evenly mixed by ultrasonic stirring, and then the weight ratio of the carbon black is as follows: adding PTFE emulsion into Polytetrafluoroethylene (PTFE) according to the mass ratio of 3:7, stirring and mixing uniformly again, then heating to volatilize absolute ethyl alcohol to prepare dough, rolling to a stainless steel metal net through a rolling machine, and heating for 30min at the temperature of 340 ℃; secondly, a catalytic layer is loaded on the other side of the stainless steel metal net, and carbon black (EC-300J, Hesen electric Co. Ltd., Shanghai, China) is dissolved in absolute ethyl alcohol and is uniformly mixed by ultrasonic stirring, and then the mixture is mixed according to the proportion of carbon black: adding PTFE emulsion into Polytetrafluoroethylene (PTFE) according to the mass ratio of 3:1, stirring and mixing uniformly again, then heating and volatilizing absolute ethyl alcohol to prepare a dough shape, rolling the dough shape to the other surface of the stainless steel metal net loaded with the diffusion layer through a rolling machine, and airing.
(2) Injecting artificial wastewater containing 1, 4-dioxane from a hole above the reactor, and circulating and fully mixing the solutions on the left side and the right side of the iron mesh anode by using a peristaltic pump, wherein the circulating flow rate is about 35 mL/min.
(3) When the reactor is operated, corresponding current density is applied to the platinum electrode and the iron net, and the reasonable proportion of the electrifying time of the platinum electrode and the iron net is controlled by the time relay to achieve the purpose of applying pulse current, so that the amount of the generated hydrogen peroxide and the ferrous ions reaches the optimal proportion.
The specific results are as follows:
in this example, 35mA and 7mA were selected as currents to be applied to the platinum electrode and the iron mesh anode, i.e., the current densities were 5mA/cm, respectively2And 1mA/cm2. Meanwhile, different energization time ratios of the platinum electrode and the iron mesh anode, 4:4, 4:3, 4:2, 4:1 and 4:0.5, were set, and the results of comparing the removal speed of the pollutants within 120min and the energy consumption under the same removal efficiency are shown in fig. 2 and 3: with the increase of the power-on time proportion, the removal rate is gradually increased, and meanwhile, the energy consumption required for reaching the same removal rate is also obviously increased.
Considering the overall removal rate and energy consumption, different switching frequencies of 4:3, 2:1.5, 1.2:0.9, 0.8:0.6 and 0.4:0.3 are set at the same power-on time ratio of 4:3 (with 1s as the basic unit, i.e. 4:3 for 4s:3s and 0.4:0.3 for 0.4s:0.3s), and the results are shown in fig. 4 and 5 by further comparing the removal speed of the pollutants within 120min and the energy consumption at the same removal efficiency: with increasing switching frequency, the removal rate is increased gradually, while the energy consumption required to achieve the same removal rate is significantly reduced. Therefore, 0.4:0.3 is the optimum switching frequency in the gradient of the conditions set in this embodiment.
Comparative example 1
This comparative example provides a conventional electro-fenton treatment process, as follows.
This comparative example selects the same currents as in example 1, i.e., 35mA and 7mA, as the currents applied to the platinum electrode and the iron mesh anode at current densities of 5mA/cm, respectively2And 1mA/cm2And 1, 4-dioxane with the same concentration as in example 1 was degraded by continuous energization. The results are shown in FIGS. 6 and 7: compared with the optimal switching frequency in the example 1, the removal rate of the comparative example is approximately equivalent to that of the example 1, but the energy consumption for achieving the same removal rate is obviously higher than that of the example 1, and the iron mud generated in the reaction process is obviously increased due to the fact that the energizing time of the iron mesh electrode is greatly increased.
From the above, compared with the traditional electro-Fenton treatment method, the pulse electro-Fenton treatment method has the advantages of high removal rate, low energy consumption and greatly reduced amount of byproduct iron sludge.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A method for efficiently removing 1, 4-dioxane by pulse electro-Fenton is characterized by comprising the following steps:
s1: constructing a reactor by taking an inert electrode and an iron electrode as anodes, an air electrode as a cathode and artificial wastewater containing 1, 4-dioxane as electrolyte;
s2: alternately electrifying the inert electrode and the iron electrode, and continuously electrifying the cathode to form pulse current; the ratio of the current passing through the inert electrode once to the current passing through the iron electrode is 5: 1; the electrifying time of the single inert electrode is 0.4s, and the electrifying time of the single iron electrode is 0.3 s;
in S1, an iron electrode is arranged between the inert electrode and a cathode; the distance between the inert electrode and the cathode electrode is 2.5-4.0 cm, and the distance between the iron electrode and the cathode electrode is 1.0-3.0 cm;
the current densities of the inert electrode and the iron electrode in S2 are respectively 5mA/cm2And 1mA/cm2。
2. The method of claim 1, wherein the inert electrode in S1 is a platinum electrode, an iridium ruthenium electrode, a titanium plate, or a graphite electrode; the iron electrode is an iron net, an iron sheet or an iron plate.
3. The method of claim 1, wherein the air electrode in S1 includes a catalytic layer and a diffusion layer; the catalyst layer is one or more of activated carbon, carbon black and graphite, and the diffusion layer is one or more of carbon black, activated carbon and graphite.
4. The method of claim 1, wherein the electrolyte is circulated in S1.
5. The method as claimed in claim 1, wherein the electrolyte is circulated in S1 at a flow rate of 10-50 mL/min.
6. The method of claim 1, wherein the total time of the energization in S2 is not less than 2 h.
7. The method according to claim 1, wherein the energizing time is controlled by a time relay in S2.
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CN102633322A (en) * 2012-04-17 2012-08-15 西安建筑科技大学 Semi-coke waste water pretreatment method based on Electro-Fenton oxidization technology
CN106277215A (en) * 2016-07-20 2017-01-04 中山大学 A kind of electricity Fenton produces free radical control method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102633322A (en) * 2012-04-17 2012-08-15 西安建筑科技大学 Semi-coke waste water pretreatment method based on Electro-Fenton oxidization technology
CN106277215A (en) * 2016-07-20 2017-01-04 中山大学 A kind of electricity Fenton produces free radical control method

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