CN110194519A - A kind of method that pulse electricity Fenton efficiently removes 1,4- dioxane - Google Patents

A kind of method that pulse electricity Fenton efficiently removes 1,4- dioxane Download PDF

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CN110194519A
CN110194519A CN201910453680.5A CN201910453680A CN110194519A CN 110194519 A CN110194519 A CN 110194519A CN 201910453680 A CN201910453680 A CN 201910453680A CN 110194519 A CN110194519 A CN 110194519A
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electrode
iron
dioxane
inert
electric current
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CN110194519B (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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National 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Abstract

The present invention relates to a kind of methods that pulse electricity Fenton efficiently removes 1,4- dioxane.Described method includes following steps: S1: using inert electrode and iron electrode as anode, using air electrode as cathode, as electrolyte, to construct reactor containing Isosorbide-5-Nitrae-dioxane artificial wastewater；S2: being alternately powered to inert electrode and iron electrode, and cathode is persistently powered, and forms pulse current.Method electrolysis provided by the invention generates hydrogen peroxide and ferrous ion, and the two reaction generates the hydroxyl radical free radical with strong oxidizing property and oxidation reaction occurs for pollutant Isosorbide-5-Nitrae-dioxane, realizes the efficient degradation of pollutant.Reaction optimal components ratio is reached by pulse control hydrogen peroxide and ferrous ion content simultaneously, the generation of side reaction caused by effectively reducing because of ferrous ion excess, it largely realizes making full use of for hydrogen peroxide, substantially reduces the generation of the energy consumption and iron cement of this method.

Description

A kind of method that pulse electricity Fenton efficiently removes 1,4- dioxane
Technical field
The invention belongs to electrochemical advanced oxidation fields, and in particular to a kind of pulse electricity Fenton efficiently removes Isosorbide-5-Nitrae-dioxy six The method of ring.
Background technique
Isosorbide-5-Nitrae-dioxane is a kind of cyclic annular organic pollutant, is also listed in 2B class (possible) human carcinogen.1,4- Dioxane be widely used as industrial products production solvent, stabilizer such as paint, cosmetics and deodorant, while can also be used as secondary Product is formed in the production of other organic reagents such as surfactant.Due to its stable chemical structure, Isosorbide-5-Nitrae-dioxane Have the characteristics that highly-water-soluble and difficult for biological degradation, at present common sewage water treatment method for example activated sludge process, activated carbon adsorption, Flocculence etc. all can not effectively accomplish and efficiently removal effective to it, and can be effectively removed using electric Fenton high-level oxidation technology The problems such as pollutant is high but there are energy consumptions, and by-product iron cement amount is big.
Therefore, develop it is a kind of can efficient low-consume removal Isosorbide-5-Nitrae-dioxane processing method it is very necessary.
Summary of the invention
It is an object of the invention to overcome existing electric Fenton high-level oxidation technology to remove 1,4- dioxane that there are energy consumptions is high, By-product iron cement amount big defect and deficiency provide a kind of pulse electricity Fenton and efficiently remove Isosorbide-5-Nitrae-dioxane method.This hair The method of bright offer using cathode generate hydrogen peroxide, iron electrode as sacrificial anode generate ferrous ion, hydrogen peroxide with Ferrous ion reaction generates the hydroxyl radical free radical with strong oxidizing property and oxidation reaction occurs for pollutant Isosorbide-5-Nitrae-dioxane, real The efficient degradation of existing pollutant.Reaction optimal components ratio is reached by pulse control hydrogen peroxide and ferrous ion content simultaneously, The abundant benefit of hydrogen peroxide is largely realized in the generation of side reaction caused by effectively reducing because of ferrous ion excess With substantially reducing the generation of the energy consumption and iron cement of this method.Pulse electro-fenton process provided by the invention can be in 2h by 200mg/ L, 95% or more 2,4- dioxane removal, realizes the efficient removal of pollutant, while comparing and having with traditional electro-fenton process There is the advantages that low energy consumption, and by-product iron cement amount is few.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of pulse electricity Fenton efficiently removes Isosorbide-5-Nitrae-dioxane method, includes the following steps:
S1: using inert electrode and iron electrode as anode, using air electrode as cathode, containing Isosorbide-5-Nitrae-dioxane people Work waste water constructs reactor as electrolyte；
S2: being alternately powered to inert electrode and iron electrode, and cathode is persistently powered, and forms pulse current；Once-through inertia The electric current of electrode and the ratio for passing through the electric current of iron electrode are 4~6:1；The conduction time of single inert electrode and leading to for iron electrode The ratio of electric time is 1~8:1.
When being powered to inert electrode and cathode, cathode is contacted with air, and it is raw that hydrone is catalyzed under the action of electricity At hydrogen peroxide；When being powered to iron electrode and cathode, iron electrode generates ferrous ion, peroxidating as sacrificial anode Hydrogen and ferrous ion reaction generate the hydroxyl radical free radical with strong oxidizing property and the generation oxidation of pollutant 1,4- dioxane is anti- It answers, realizes the efficient degradation of pollutant.It is preferable that reaction is reached by pulse control hydrogen peroxide and ferrous ion content simultaneously Filling for hydrogen peroxide is largely realized in proportion, the generation of side reaction caused by effectively reducing because of ferrous ion excess Divide and utilize, substantially reduces the generation of the energy consumption and iron cement of this method.Pulse electro-fenton process provided by the invention can be incited somebody to action in 2h 200mg/L, 95% or more 2,4- dioxane removal, realizes the efficient removal of pollutant, at the same with traditional electro-fenton process phase Than having many advantages, such as that low energy consumption again, by-product iron cement amount is few.
This field is used equally in the present invention conventionally used for the inert electrode that electrolysis generates hydrogen peroxide.
Preferably, inert electrode described in S1 is platinum electrode, iridium ruthenium electrode, titanium plate or graphite electrode.
Above-mentioned electrode is routine and performance preferably analyses oxygen anodes.
It is further preferable that inert electrode described in S1 is platinum electrode.
Iron electrode can be conventional electrode shape.
Preferably, extremely iron net, iron plate or the iron plate of ferroelectricity described in S1.
It is further preferable that the extremely iron net of ferroelectricity described in 1.
Air electrode conventional in the art is used equally in the present invention.
Preferably, air electrode described in S1 includes Catalytic Layer and diffusion layer；The Catalytic Layer is active carbon, carbon black or stone One or more of ink；The diffusion layer is one or more of carbon black, active carbon or graphite.
Preferably, the Catalytic Layer is carbon black, and the diffusion layer is carbon black.
Specifically, the air electrode is prepared via a method which to obtain:
The gas diffusion cathode is collectively constituted by diffusion layer, stainless steel wire mesh and Catalytic Layer.First in stainless steel gold The one side for belonging to net loads diffusion layer, and carbon black (Vulcan XR-72, Cabot Corp., USA) is dissolved and led to via dehydrated alcohol Cross after ultrasonic agitation mixes by carbon black: polytetrafluoroethylene (PTFE) (PTFE) mass ratio 3:7 is added PTFE emulsion and is again stirring for mixing, then Dough is made by heating volatilization dehydrated alcohol, then by roll squeezer roll-in to stainless steel metal on the net and in 340 DEG C of conditions Lower heating 30min is made；Then in stainless steel wire mesh another side supported catalyst layer, by carbon black (EC-300J, Hesen Electric Co.Ltd., Shanghai, China) it dissolves and passes through after ultrasonic agitation mixes by carbon black via dehydrated alcohol: it is poly- Tetrafluoroethene (PTFE) mass ratio 3:1 is added PTFE emulsion and is again stirring for mixing, and is then made up of heating volatilization dehydrated alcohol Dough, then the nothing by drying volatile residue after roll squeezer roll-in to the another side for the stainless steel wire mesh for having loaded diffusion layer Water-ethanol.
Preferably, electrolyte circulation is passed through in S1.
It is further preferable that the flow velocity that electrolyte circulation is passed through in S1 is 5~50mL/min.
Most preferably, the flow velocity that electrolyte circulation is passed through in S1 is 35mL/min.
Preferably, iron electrode is set between the inert electrode and cathode in S1；The inert electrode and negative electrode Distance is 2.5~4.0cm, and the distance of the iron electrode and negative electrode is 1.0~3.0cm.
It is further preferable that the distance of the inert electrode and negative electrode is 3.5cm, the distance of the iron electrode and negative electrode For 2.0cm.
Preferably, the electric current of once-through inert electrode and the ratio by the electric current of iron electrode are 5:1 in S2；Single is lazy Property electrode conduction time and iron electrode conduction time ratio be 4:3.
It is further preferable that the electric current of once-through inert electrode is 35mA, conduction time 0.4s in S2；Single is logical in S2 The electric current for crossing iron electrode is 7mA, conduction time 0.3s.
Under this condition, controllable hydrogen peroxide and ferrous ion content reach reaction optimum proportioning, effectively reduce because of two The generation of side reaction caused by valence iron ion excess realizes making full use of for hydrogen peroxide to the greatest extent, substantially reduces this The generation of the energy consumption and iron cement of method.
Preferably, the total time being powered in S2 is not less than 2h.
Preferably, conduction time is controlled using the time relay in S2.
Compared with prior art, the invention has the following beneficial effects:
Method provided by the invention using cathode generate hydrogen peroxide, iron electrode as sacrificial anode generation ferrous iron from Son, hydrogen peroxide and ferrous ion reaction generate the hydroxyl radical free radical with strong oxidizing property and pollutant Isosorbide-5-Nitrae-dioxane is sent out Raw oxidation reaction, realizes the efficient degradation of pollutant.Reached simultaneously by pulse control hydrogen peroxide and ferrous ion content Optimal components ratio is reacted, the generation of side reaction, largely realizes peroxide caused by effectively reducing because of ferrous ion excess Change making full use of for hydrogen, substantially reduces the generation of the energy consumption and iron cement of this method.Pulse electro-fenton process provided by the invention can be with In 2h by 200mg/L, the efficient removal of pollutant is realized in 95% or more 2,4- dioxane removal, while fragrant with traditional electricity The method of pausing has many advantages, such as that low energy consumption compared to again, and by-product iron cement amount is few.
Detailed description of the invention
Fig. 1 is pulse electro-Fenton reaction system connection schematic diagram；
Fig. 2 is 1,4- bis- of the method that provides of embodiment 1 under platinum electrode and iron electrode difference conduction time ratio gradient Six ring concentration ratio of oxygen-time graph；
Fig. 3 is removal list of the method that provides of embodiment 1 under platinum electrode and iron electrode difference conduction time ratio gradient Position quality 1,4- dioxane energy consumption-removal rate curve；
Fig. 4 is 1,4- dioxy six of the method that provides of embodiment 1 under platinum electrode and iron electrode different switching frequency gradient Ring concentration ratio-time graph；
Fig. 5 is removal unit matter of the method that provides of embodiment 1 under platinum electrode and iron electrode different switching frequency gradient Measure 1,4- dioxane energy consumption-removal rate curve；
Fig. 6 is the 1,4- dioxane concentration ratio-time graph for the method that comparative example 1 provides；
Fig. 7 is the unit mass 1,4- dioxane energy consumption-removal rate curve for the method that comparative example 1 provides.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention And replacement belongs to scope of the present invention.
Isosorbide-5-Nitrae-dioxane is dissolved in 100mmol/L metabisulfite solution, the concentration being configured to is the artificial of 200mg/L Waste water.The concentration conditions much higher than Isosorbide-5-Nitrae-dioxane concentration in conventional sewage, select by various embodiments of the present invention and comparative example Use the artificial wastewater as liquid to be processed (electrolyte).
Together using high performance liquid chromatography (HPLC), ion chromatography (IC) and gas chromatography-mass spectrometry (GC-MS) etc. The concentration and degradation pathway of the pollutant in waste water are analyzed, determined in each embodiment and comparative example to pollutant Isosorbide-5-Nitrae-two The removal effect of six ring of oxygen.
Embodiment 1
The present embodiment provides a kind of pulse electricity Fentons efficiently to remove Isosorbide-5-Nitrae-dioxane method, and process is as follows.
(1) as shown in Figure 1, the anode of the reaction system be platinum electrode and iron net, with cathode spacing be respectively 3.5cm and 2.0cm, wherein iron net aoxidizes under the action of electricity generates ferrous ion participation Fenton's reaction.Cathode is by Catalytic Layer and diffusion layer Composition, diffusion layer are directly contacted with air, and it is anti-that Catalytic Layer is catalyzed hydrone generation hydrogen peroxide participation Fenton under the action of electricity Answer, cathode is prepared by following process: the gas diffusion cathode is common by diffusion layer, stainless steel wire mesh and Catalytic Layer Composition.Diffusion layer is loaded in the one side of stainless steel wire mesh first, by carbon black (Vulcan XR-72, Cabot Corp., USA) Dissolve and pass through after ultrasonic agitation mixes by carbon black via dehydrated alcohol: PTFE is added in polytetrafluoroethylene (PTFE) (PTFE) mass ratio 3:7 Lotion is again stirring for mixing, and dough then is made by heating volatilization dehydrated alcohol, then pass through roll squeezer roll-in to stainless steel 30min is heated on metal mesh and under the conditions of 340 DEG C to be made；Secondly in stainless steel wire mesh another side supported catalyst layer, by charcoal Black (EC-300J, Hesen electric Co.Ltd., Shanghai, China) is dissolved via dehydrated alcohol and is stirred by ultrasound Mix after mixing by carbon black: polytetrafluoroethylene (PTFE) (PTFE) mass ratio 3:1 is added PTFE emulsion and is again stirring for mixing, and then passes through heating Dough is made in volatilization dehydrated alcohol, then by after roll squeezer roll-in to the another side for the stainless steel wire mesh for having loaded diffusion layer It dries.
(2) it will be injected out of hole above reactor containing Isosorbide-5-Nitrae-dioxane artificial wastewater, and using peristaltic pump to iron Solution recycle and is sufficiently mixed uniformly at left and right sides of net anode, and rate of circulating flow is about 35mL/min.
(3) when reactor is run, corresponding current density is applied to platinum electrode and iron net, and control by the time relay Platinum electrode and the rational proportion of iron net conduction time achieve the purpose that application pulse current, make the hydrogen peroxide and ferrous iron generated The amount of ion reaches optimal proportion.
Concrete outcome is as follows:
The present embodiment selects 35mA and 7mA as the electric current being applied on platinum electrode and iron net anode, i.e. current density point It Wei not 5mA/cm2And 1mA/cm2.Meanwhile provided with the platinum electrode conduction time ratio 4:4,4:3 different with iron net anode, 4:2,4: 1 and 4:0.5 compares the pollutant removal speed in 120min and the energy consumption under identical removal efficiency, as a result such as Fig. 2 and Shown in Fig. 3: with the increase of conduction time ratio, removal rate is gradually accelerated, while the energy consumption needed for reaching identical removal rate Also obvious to rise.
Comprehensive removal rate and energy consumption consider, be provided with identical conduction time ratio 4:3 (using 1s as basic unit, i.e., 4:3 represents 4s:3s, and 0.4:0.3 represents 0.4s:0.3s) under, different conversion frequency 4:3,2:1.5,1.2:0.9,0.8:0.6 And 0.4:0.3, further compare the pollutant removal speed in 120min and the energy consumption under identical removal efficiency, as a result As shown in Figure 4 and Figure 5: with the quickening of conversion frequency, removal rate is gradually accelerated, while the energy needed for reaching identical removal rate Consumption is but substantially reduced.Therefore, 0.4:0.3 is the best transition frequency in condition gradient set by the present embodiment.
Comparative example 1
This comparative example provides a kind of conventional electric Fenton processing method, and detailed process is as follows.
This comparative example selects electric current i.e. 35mA and 7mA identical with example 1 as being applied on platinum electrode and iron net anode Electric current, current density is respectively 5mA/cm2And 1mA/cm2, and take the mode pair of lasting energization and 1 same concentrations of example 1,4- dioxane is degraded.As a result as shown in Figure 6 and Figure 7: compared with best transition frequency in embodiment 1, this comparative example Removal rate and embodiment 1 it is roughly the same, but energy consumption needed for reaching identical removal rate is significantly higher than embodiment 1, simultaneously The substantial increase of iron net electrode conduction time, generated iron cement also increased significantly in reaction process.
It can be seen from the above, pulse electricity Fenton has removal rate high compared with traditional electric Fenton processing method, low energy consumption, secondary The advantage that product iron cement amount greatly reduces.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (10)

1. a kind of pulse electricity Fenton efficiently removes Isosorbide-5-Nitrae-dioxane method, which comprises the steps of:
S1: using inert electrode and iron electrode as anode, using air electrode as cathode, with artificial useless containing Isosorbide-5-Nitrae-dioxane Water constructs reactor as electrolyte；
S2: being alternately powered to inert electrode and iron electrode, and cathode is persistently powered, and forms pulse current；Once-through inert electrode Electric current and the ratio that passes through the electric current of iron electrode be 4~6:1；When the energization of conduction time of single inert electrode and iron electrode Between ratio be 1~8:1.
2. method according to claim 1, which is characterized in that inert electrode described in S1 is platinum electrode, iridium ruthenium electrode, titanium plate Or graphite electrode；The ferroelectricity extremely iron net, iron plate or iron plate.
3. method according to claim 1, which is characterized in that air electrode described in S1 includes Catalytic Layer and diffusion layer；Institute Stating Catalytic Layer is one or more of active carbon, carbon black or graphite, and the diffusion layer is one in carbon black, active carbon or graphite Kind is several.
4. method according to claim 1, which is characterized in that electrolyte circulation is passed through in S1.
5. method according to claim 1, which is characterized in that the flow velocity that electrolyte circulation is passed through in S1 is 10~50mL/ min。
6. method according to claim 1, which is characterized in that in S1 iron electrode be set to the inert electrode and cathode it Between；The distance of the inert electrode and negative electrode is 2.5~4.0cm, the distance of the iron electrode and negative electrode is 1.0~ 3.0cm。
7. method according to claim 1, which is characterized in that the electric current of once-through inert electrode and pass through iron electrode in S2 Electric current ratio be 5:1；The ratio of the conduction time of the conduction time and iron electrode of single inert electrode is 4:3.
8. method according to claim 7, which is characterized in that the electric current of once-through inert electrode is 35mA in S2, is powered Time is 0.4s；The electric current of once-through iron electrode is 7mA, conduction time 0.3s in S2.
9. method according to claim 1, which is characterized in that the total time being powered in S2 is not less than 2h.
10. method according to claim 1, which is characterized in that control conduction time using the time relay in S2.
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Cited By (1)

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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
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Publication number Priority date Publication date Assignee Title
CN111206259A (en) * 2020-01-14 2020-05-29 武汉科技大学 Preparation method of novel carbon black air diffusion cathode sheet capable of efficiently and stably producing hydrogen peroxide
CN111206259B (en) * 2020-01-14 2021-03-19 武汉科技大学 Preparation method of novel carbon black air diffusion cathode sheet capable of efficiently and stably producing hydrogen peroxide

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