CN110104737A - A kind of novel lead dioxide electrode preparation method and application with electrocatalytic oxidation property - Google Patents

A kind of novel lead dioxide electrode preparation method and application with electrocatalytic oxidation property Download PDF

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Publication number
CN110104737A
CN110104737A CN201910407331.XA CN201910407331A CN110104737A CN 110104737 A CN110104737 A CN 110104737A CN 201910407331 A CN201910407331 A CN 201910407331A CN 110104737 A CN110104737 A CN 110104737A
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lead dioxide
dioxide electrode
stereotype
electrode
application
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谢光炎
陈卓瑶
许燕滨
周晓
梅志纲
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Guangdong University of Technology
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Guangdong University of Technology
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/34Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • C02F2001/46133Electrodes characterised by the material

Abstract

The invention belongs to fields, more particularly to a kind of novel lead dioxide electrode preparation method and application with electrocatalytic oxidation property.The preparation method of the lead dioxide electrode of the application, comprising the following steps: step 1 successively using aqueous slkali and acid solution cleans stereotype, and be eluted with water pre-processed after stereotype;Step 2 mixes stereotype after pretreatment with the concentrated sulfuric acid, and is eluted with water to obtain stereotype after acid is handled;Step 3 is used as electrode using stereotype after acid processing, and using dilute sulfuric acid and metal cation solution as electrolyte, progress cell reaction obtains lead dioxide electrode.The application second aspect provides application of the lead dioxide electrode of lead dioxide electrode and the application in sewage treatment.The present invention provides a kind of lead dioxide electrodes and its preparation method and application, for solving the technological deficiency that the lead dioxide electrode service life is short, oxygen evolution potential is low and oxidation susceptibility is poor in the prior art.

Description

A kind of novel lead dioxide electrode preparation method with electrocatalytic oxidation property and Using
Technical field
The invention belongs to fields, more particularly to a kind of novel lead dioxide electrode preparation with electrocatalytic oxidation property Method and application.
Background technique
Lance as the animal husbandry of scale is fast-developing, between the disposal of pollutants of aquaculture bring and environmental protection Shield becomes increasingly conspicuous, and does not meet present requirement yet after conventional physics, chemistry, biological means processing breeding wastewater, treated Wastewater biological degradability is low, and high-level oxidation technology comes into being and has remarkable break-throughs at this time.High-level oxidation technology (Advanced Oxidation Technologies, abbreviation AOT) advanced oxidation processes are also known as, it is to utilize the extremely strong free radical of activity (such as OH organic matter difficult to degrade) is made to be converted into the novel oxidized decontamination dyeing technique of low evil or harmless small-molecule substance.OH's Standard oxidationreduction potential is up to 2.8V, than other common oxidant (F2Except) there is higher oxidability, make in water Organic substance be oxidized rapidly and degraded, and final oxygenolysis is CO2And H2O makes the COD value of organic sewage significantly It reduces, it is especially effective to high stability, organic pollutant difficult to degrade in water, it has been increasingly becoming the heat of water treatment technology research Point.
At present high-level oxidation technology include electrochemical oxidation, photochemical oxidation, catalytic wet oxidation, ozone oxidation, Fenton oxidation etc..The first, electrochemical oxidation process refers to the process of through electrode reaction oxidation removal dirt water pollutant, is somebody's turn to do Method can also be divided into direct oxidation and indirect oxidation, wherein it is higher to refer to that positive metal-oxide is changed into for electrochemistry direct oxidation The metal ion of valence state obtains electronic capability with stronger since its is unstable, under the positive action of electric field, in solution directly It is seized with the share electron pair of active groups certain on the organic matter of positive contact, chemical bond rupture or structure are changed Become, most important feature is redox reaction generation in electrode surface, and during direct oxidation, is precipitated in oxygen Potential region, water generate hydroxyl radical free radical (OH) in electrode surface discharge, and the reaction mechanism is as follows:
MOx+H2O→MOx(·OH)+H++e-
MOx(·OH)→MOx+1+H++e-
MOx(·OH)+R→MOx+CO2+H++e-
MOx+1+R→MOx+RO。
The principle of electrochemistry indirect oxidation, indirect oxidation is, in a cell certain existing ion or substance, in electrode On react and generate the substance with strong oxidizing property, the Cl of variable valence is such as added in the electrolytic solution-, Cl-In the work of anode It is changed into the ClO of high-valence state with lower discharge-, to have oxidability.The second, photochemical oxidation method, due to reaction condition Mildly, the strong photochemical oxidation method of oxidability rapidly develops in recent years, but due to the limitation of reaction condition, photochemical method processing has A variety of aromatic series organic intermediates can be generated when machine object, cause organic matter degradation not thorough enough, this, which becomes photochemical oxidation, needs Overcome the problems, such as.Photochemical oxidation method includes light excitation oxidizing process (such as O3/ UV) and photocatalytic oxidation (such as TiO2/ UV), In, light excites oxidizing process mainly with O3、H2O2、O2With air as oxidant, OH is generated under thermal effect;Photocatalysis Oxidation rule is that a certain amount of semiconductor catalyst is added in reaction solution, it is made to generate OH under the irradiation of ultraviolet light, Both organic pollutant is handled by the strong oxidation of OH.Third, catalytic wet air oxidation (CWAO) are Refer under the conditions of high temperature (123 DEG C~320 DEG C), high pressure (0.5~10MPa) and catalyst (oxide, noble metal etc.) are existing, By the organic pollutant and NH in sewage3- N oxygenolysis is at CO2、N2And H2The method of the innocuous substances such as O.4th, ozone oxidation Method mainly passes through directly reaction and two kinds of approach of indirect reaction and is achieved.Wherein directly reaction refers to ozone and organic matter It directly reacts, this mode has stronger selectivity, usually organic matter of the attack with double bond, usually to unsaturation Aliphatic hydrocarbon and compound fragrant hydrocarbon are more effective;Indirect reaction refers to that ozone decomposes and generates OH, by OH and organic matter into Row oxidation reaction, this mode do not have selectivity.5th, Fenton oxidation method is a kind of advanced oxidation processes, that is, utilizes Fe and H2O2Between chain reaction catalysis generate OH free radical, and OH free radical have strong oxidizing property, can aoxidize various toxic With organic compound difficult to degrade, to achieve the purpose that remove pollutant, it is especially suitable for bio-refractory or general chemistry The oxidation processes of organic wastewater hard to work such as landfill leachate are aoxidized, Fenton method handles the influence factor of landfill leachate Predominantly pH, H2O2Dosage and molysite dosage, the 6th, Fenton-like method are to utilize the substantially former of Fenton method Reason, by UV, O3Therefore in broad terms, H can be passed through in addition to Fenton method with introducing reaction systems such as photoelectric effect2O2 Other all technologies for generating hydroxyl radical free radical processing organic matter are referred to as Fenton-like method.Change as to Fenton oxidation method Into the development potentiality of Fenton-like method is bigger.
Currently, sewage handling problem mostly uses electrochemical oxidation process, preparing for lead dioxide electrode be simple, it is low in cost simultaneously And it is with good electric conductivity, so that it has a good application prospect in sewage treatment field.Although lead dioxide electrode With numerous advantages, but also face some problems.For example there is biggish internal stress inside lead dioxide plating coat, it had been electrolysed Generated nascent oxygen easily penetrates superficial layer and is diffused into substrate in journey, to can make base passivation, coating falls off, drop The electrochemical stability and service life of low electrode.
Summary of the invention
The first purpose of the application is to provide a kind of oxygen evolution potential height, the good lead dioxide electrode of oxidation susceptibility and its preparation Method, the second purpose are to provide a kind of application of oxidation-reduction electrode that can be used for sewage treatment.
In view of this, the application first aspect provides the preparation method of lead dioxide electrode, comprising the following steps:
Step 1 successively using aqueous slkali and acid solution cleans stereotype, and be eluted with water pre-processed after lead Plate;
Step 2 mixes stereotype after the pretreatment with the concentrated sulfuric acid, and is eluted with water to obtain stereotype after acid is handled;
Step 3, using stereotype after the acid processing as electrode, using dilute sulfuric acid and metal cation solution as electrolyte, Cell reaction is carried out, lead dioxide electrode is obtained.
Specifically, the long * wide of stereotype is 40*30cm.
Preferably, the aqueous slkali includes NaOH, Na in step 12CO3、NaSiO3、Na3PO4·12H2O and water.
Preferably, the aqueous slkali includes following components in step 1:
More preferably, the aqueous slkali includes following components in step 1: the Na of NaOH, 20g/L of 10g/L2CO3、5g/L NaSiO3, 10g/L Na3PO4·12H2O and excess water.The aqueous slkali is used to remove the grease on stereotype surface.
Preferably, the acid solution is selected from HCl in step 1, the volume fraction range of the HCl is 10%-20%; The water is 80 DEG C of water.The acid solution is used to remove oxide existing for stereotype surface.Specifically, the water is deionization Water can sufficiently remove the acid solution on stereotype surface using high temperature deionized water.
Preferably, the volume fraction of the concentrated sulfuric acid is 98% in step 2.
Specifically, stereotype after the pretreatment is mixed 2 hours with the concentrated sulfuric acid in step 2.Dense sulphur is removed with deionized water The residual of acid.
Preferably, the volume fraction of the dilute sulfuric acid is 10%-20% in step 3.It the use of dilute sulfuric acid is that electrolyte can To guarantee pH value when electrolysis, be conducive to β-PbO2Formation.
Preferably, the metal cation of the metal cation solution is selected from Fe in step 32+、Bi3+Or Co2+In It is a kind of.Wherein, the metal cation of the metal cation solution is 0.01M.
More preferably, the metal cation of the metal cation solution is selected from Fe in step 32+
Preferably, the impressed DC voltage of the cell reaction is 1.5-2V in step 3;The cell reaction when Between be 4-7 hours.Wherein, it is stirred while being electrolysed.
The application second aspect provides lead dioxide electrode, which is characterized in that is prepared including above-mentioned preparation method Lead dioxide electrode.The surface of the lead dioxide electrode of the application forms β-PbO2
The application third aspect provides lead dioxide electrode made from method made above or the above lead dioxide electrode Application in sewage treatment.
Specifically, above-mentioned sewage treatment is to carry out redox processing to sewage.
The purpose of the present invention is for the lead dioxide electrode service life short defect low with oxygen evolution potential in the prior art.For upper The problem of stating provides a kind of can simplify simultaneously and prepares lead dioxide electrode using lead as substrate and improve the processing method of electro-chemical activity. The preparation method of the application is reacted using the concentrated sulfuric acid with lead, lead sulfate film is formed on stereotype, and using dilute sulfuric acid as electrolyte, Stereotype is that electrode carries out electrochemical oxidation, and dilute sulfuric acid is stablized, and guarantees the pH range of electrolyte, the brown lead oxide electricity being prepared Pole forms β-PbO2, to improve the electro-chemical activity and current efficiency of lead dioxide electrode.From the experimental results, this Shen β-the PbO on the surface of lead dioxide electrode please2Structure is uniformly and fine and close, not easily to fall off, meanwhile, the analysis oxygen of lead dioxide electrode Current potential is high, and oxidation susceptibility is more preferable.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described.
Fig. 1 shows the LSV result for the lead dioxide electrode that the embodiment of the present application 1 provides;
Fig. 2 shows the XRD result for the lead dioxide electrode that the embodiment of the present application 1 provides;
Fig. 3 shows the Electronic Speculum result for the lead dioxide electrode that the embodiment of the present application 1 provides;
Fig. 4 is the structure chart of sewage-treatment plant provided by the embodiments of the present application;
Wherein, appended drawing reference, electrolytic cell 1, power supply 2 and electrode 3.
Specific embodiment
The present invention provides a kind of novel lead dioxide electrode preparation method and application with electrocatalytic oxidation property, For solving the technological deficiency that the lead dioxide electrode service life is short, oxygen evolution potential is low and oxidation susceptibility is poor in the prior art.
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
Wherein, it is commercially available or self-control that following embodiment is raw materials used.
Embodiment 1
The embodiment of the present application provides a kind of lead dioxide electrode, specific preparation method (using 98% dense sulfuric acid treatment and Potentiostatic deposition processing is carried out under 20% dilute sulfuric acid) as follows:
(1) pretreatment of stereotype: into stereotype (40*30cm) put to (aqueous slkali includes 10g/L's added with aqueous slkali The Na of NaOH, 20g/L2CO3, 5g/L NaSiO3, 10g/L Na3PO4·12H2O and excess water) rinse bath in mix, alkali Then solution places into the cleaning added with acid solution (acid solution includes the HCl that volume fraction is 20%) for removing grease It is mixed in slot, acid solution is used to remove the oxide on surface of stereotype, finally, the deionized water using 80 DEG C is cleaned, obtains pre- place Stereotype after reason.
(2) sulfuric acid treatment of stereotype: stereotype after the pretreatment in (1) is put into reactive tank, is soaked in 98% concentrated sulfuric acid Bubble 2 hours, is then washed with deionized water, and obtains stereotype after acid processing.
(3) lead sulfate electrolysis is handled: stereotype after the acid processing in (2) being placed in electrolytic cell, is made with 20% dilute sulfuric acid For electrolyte, and the Fe of 0.01M is added2+, it is electrolysed 8 hours at 2V, is during which stirred with blender, obtains brown lead oxide Electrode.
The lead dioxide electrode of the present embodiment is subjected to oxidation susceptibility and characterization is verified:
(1) oxidation susceptibility: being scanned verifying by lead dioxide electrode of the electrochemical workstation to the present embodiment, LSV curve such as Fig. 1, it is seen that the lead dioxide electrode that lead dioxide electrode (1.9V vs.SCE) ratio of the present embodiment is not modified The oxygen evolution potential of (1.65V vs.SCE) wants high, illustrates that the oxidation susceptibility of the lead dioxide electrode of the present embodiment is more preferable, wherein this The lead dioxide electrode of embodiment not being modified the preparation method comprises the following steps: using existing conventional sedimentation, in impressed current Under effect, redox reaction is occurred into the solution for stereotype matrix (40*30cm), the ionizable metal salt in solution system occurs Redox reaction, to be deposited on the process of matrix surface);
(2) it characterizes: characterization verifying is carried out to the lead dioxide electrode system of the present embodiment by scanning XRD and scanning electron microscope, As a result as shown in Figures 2 and 3.The XRD spectrum of the lead dioxide electrode of the present embodiment such as Fig. 2, it is seen that the dioxy of this method preparation Change lead electrode and generate β-PbO2, the oxidation susceptibility of electrode can be improved.Its electron microscope such as Fig. 3, passes through electron microscope, it can be seen that this Ten surfaces of lead dioxide electrode of embodiment are uniform, that is, can illustrate the surface knot of the lead dioxide electrode of the present embodiment Structure is close, it is not easy to fall off, greatly improve service life.
Embodiment 2
The embodiment of the present application is application of the lead dioxide electrode in sewage treatment, the specific steps are as follows:
Referring to Fig. 4, Fig. 4 is the structure chart of sewage-treatment plant provided by the embodiments of the present application, sewage-treatment plant packet Include electrolytic cell 1, power supply 2 and electrode 3, electrolytic cell 1 is a length of 15m, width 10m, the cuboid of a height of 3m, is had inside electrolytic cell 1 10 volumes are 3*5*3m3Compartment, using the lead dioxide electrode that embodiment 1 is prepared as anode, it is of the same area not Steel plate become rusty as cathode, is placed in electrolytic cell 1 in parallel, forms 10 pairs of electrodes pair, cathode and anode are connect with power supply 2.200- 300m3The sewage A (COD of sewage A is 12000-15000mg/L, BOD 5400-6000mg/L) of/d passes through UASB reactor After Air Exposure 48 hours, the COD and BOD of sewage A is reduced, and obtains sewage B, sewage B is placed in electrolytic cell, and 10 groups The electrolytic cell of 50L is into 200-300m3The sewage B of/d, the COD of sewage B is 500mg/L, BOD 100-200mg/L, through embodiment After 1 lead dioxide electrode is handled 30 minutes, the COD for the sewage that redox is handled is 300mg/L, BOD 150mg/ L, it is 36mg/L that TN (nitrogen pool), which is 148mg/L, TP (total phosphorus content),.
Embodiment 3
The embodiment of the present application is application of the lead dioxide electrode in sewage treatment, the specific steps are as follows:
Referring to Fig. 4, Fig. 4 is sewage-treatment plant provided by the embodiments of the present application, sewage-treatment plant includes electrolytic cell 1, power supply 2 and electrode 3, electrolytic cell 1 is a length of 15m, width 10m, the cuboid of a height of 3m, has 10 volumes inside electrolytic cell 1 For 3*5*3m3Compartment, using the lead dioxide electrode that embodiment 1 is prepared as anode, stainless steel plate of the same area is made It for cathode, is placed in electrolytic cell 1 in parallel, forms 10 pairs of electrodes pair, cathode and anode are connect with power supply 2.200-300m3The dirt of/d Water A (COD of sewage A is 12000-15000mg/L, BOD 5400-6000mg/L) passes through UASB reactor and Air Exposure 48 After hour, the COD and BOD of sewage A are reduced, and obtain sewage B, sewage B is placed in electrolytic cell, the electrolytic cell of 10 groups of 50L into 200-300m3The sewage B of/d, the COD of sewage B are 500mg/L, BOD 100-200mg/L, the brown lead oxide electricity through embodiment 1 Pole is handled after twenty minutes, and the COD for the sewage that redox is handled is 350mg/L, BOD 160mg/L, TN (nitrogen pool) are 148mg/L, TP (total phosphorus content) are 36mg/L.
Embodiment 4
The embodiment of the present application is application of the lead dioxide electrode in sewage treatment, the specific steps are as follows:
Referring to Fig. 4, Fig. 4 is sewage-treatment plant provided by the embodiments of the present application, sewage-treatment plant includes electrolytic cell 1, power supply 2 and electrode 3, electrolytic cell 1 is a length of 15m, width 10m, the cuboid of a height of 3m, has 10 volumes inside electrolytic cell 1 For 3*5*3m3Compartment, using the lead dioxide electrode that embodiment 1 is prepared as anode, stainless steel plate of the same area is made It for cathode, is placed in electrolytic cell 1 in parallel, forms 10 pairs of electrodes pair, cathode and anode are connect with power supply 2.200-300m3The dirt of/d Water A (COD of sewage A is 12000-15000mg/L, BOD 5400-6000mg/L) passes through UASB reactor and Air Exposure 48 After hour, the COD and BOD of sewage A are reduced, and obtain sewage B, sewage B is placed in electrolytic cell, the electrolytic cell of 10 groups of 50L into 200-300m3The sewage B of/d, the COD of sewage B are 500mg/L, BOD 100-200mg/L, the brown lead oxide electricity through embodiment 1 After pole is handled 25 minutes, the COD for the sewage that redox is handled is 320mg/L, BOD 150mg/L, TN (nitrogen pool) are 148mg/L, TP (total phosphorus content) are 36mg/L.
From embodiment 2-4 as it can be seen that by the lead dioxide electrode of the present embodiment 1 after oxidization-reduction is handled, sewage COD decline, BOD are risen, and TN is declined, and TP is declined.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of lead dioxide electrode, which comprises the following steps:
Step 1 successively using aqueous slkali and acid solution cleans stereotype, and be eluted with water pre-processed after stereotype;
Step 2 mixes stereotype after the pretreatment with the concentrated sulfuric acid, and is eluted with water to obtain stereotype after acid is handled;
Step 3 is carried out using stereotype after the acid processing as electrode using dilute sulfuric acid and metal cation solution as electrolyte Cell reaction obtains lead dioxide electrode.
2. preparation method according to claim 1, which is characterized in that in step 1, the aqueous slkali include NaOH, Na2CO3、NaSiO3、Na3PO4·12H2O and water.
3. preparation method according to claim 2, which is characterized in that the aqueous slkali includes following components:
4. preparation method according to claim 1, which is characterized in that in step 1, the acid solution is selected from HCl, described The volume fraction range of HCl is 10%-20%;The temperature of the water is 80 DEG C 70 DEG C -100 DEG C.
5. preparation method according to claim 1, which is characterized in that in step 2, the volume fraction of the concentrated sulfuric acid 60%-98%.
6. preparation method according to claim 1, which is characterized in that in step 3, the volume fraction of the dilute sulfuric acid is 10%-20%.
7. preparation method according to claim 1, which is characterized in that in step 3, the metal of the metal cation solution Cation is selected from Fe2+、Bi3+Or Co2+One of.
8. preparation method according to claim 1, which is characterized in that in step 3, the applying direct current of the cell reaction Pressure is 1.5-2V;The time of the cell reaction is 4-7 hours.
9. a kind of lead dioxide electrode, which is characterized in that be prepared into including such as described in any item preparation methods of claim 1-8 The lead dioxide electrode arrived.
10. lead dioxide electrode made from the described in any item preparation methods of claim 1-8 or dioxy as claimed in claim 9 Change application of the lead electrode in sewage treatment.
CN201910407331.XA 2019-05-15 2019-05-15 A kind of novel lead dioxide electrode preparation method and application with electrocatalytic oxidation property Pending CN110104737A (en)

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