CN106315772A - N-doped lead dioxide electrode and preparation method and application thereof - Google Patents
N-doped lead dioxide electrode and preparation method and application thereof Download PDFInfo
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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
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Abstract
The invention provides an N-doped lead dioxide electrode and a preparation method thereof and application of 4-CP in wastewater treatment. The N-doped lead dioxide electrode is sequentially composed of a titanium substrate, an alpha-PbO2 bottom layer electrically deposited on the titanium substrate and an N-doped beta-PbO2 active layer electrically deposited on the alpha-PbO2 bottom layer. The preparation process is simple, the effect of removing 4-CP in wastewater is obvious, and the obtained electrode has the advantages of being low in manufacturing cost, high in activity, long in service life and the like, and has the wide market development prospect in application of electro-catalysis treatment of 4-CP in wastewater.
Description
Technical field
The present invention relates to a kind of N doping lead dioxide electrode and preparation method thereof, and use N doping lead dioxide electrode
Electro-catalysis processes the application of parachlorophenol (4-CP) in organic wastewater.
Background technology
Chlorophenols compound can enter water environment by number of ways, is producing timber preservative, antibacterial, weeding
In the industry such as agent, antirust agent, pesticide and papermaking, chlorophenols compound can enter water body as product or intermediate product.Chlorophenols
Compound has the strongest chemical stability and heat stability, therefore degrades in nature slowly, and the harm cycle is the longest,
Water body and soil can be polluted, especially Mollusca, fish and mammal can be caused serious harm, easily pass through food
Chain is enriched with in vivo, causes huge harm to human health.Chlorophenols compound has severe toxicity, and zest is strong, easily quilt
Skin absorption, therefore has strong impulse effect to eyes, mucosa, respiratory tract and skin.Bronchus may be caused after suction
Inflammation, edema, spasm, chemical pneumonitis, pulmonary edema and lethal.When in waste water, the mass concentration of chlorophenol is more than 200mg/L,
Biological treatment will be produced inhibitory action, and the water that human body long-term drink is polluted by chlorophenol can cause the symptom such as giddy, anemia,
Even cause people and animal central nervous systems, hepatic and/or renal infringement.Therefore administering these waste water containing chlorophenols compound is
The task that scientific research and production unit are duty-bound.
Electrocatalytic oxidation processes useless Organic substance in water and has special degradation capability, because it has multifunctionality, height
Motility, it is prone to the feature such as automatization, non-secondary pollution and treatment effeciency is high, easy and simple to handle and the advantage such as environmental compatible, tool
There is a boundless application prospect, and the attention of researcher extremely both at home and abroad.
Summary of the invention
For solving the deficiencies in the prior art, the invention provides a kind of lead dioxide electrode for processing used water difficult to degradate
Preparation method, this electrode is the method utilizing electro-deposition, by nitrogen-doping to the top layer of ti-supported lead dioxide electric pole, system
The N doping lead dioxide electrode cost height low, active, the life-span that obtain are long.The present invention, with 4-CP for representative pollutant, carries out electricity
Catalytic oxidation treatment removes hardly degraded organic substance 4-CP in waste water.
The present invention is achieved by the following technical solutions:
A kind of N doping lead dioxide electrode, described N doping lead dioxide electrode is with the pure titanium sheet of the roughened process in surface
For matrix, by galvanoplastic the most successively at described matrix surface electro-deposition α-PbO2Bottom electro-deposition and β-PbO2Live
Property layer prepare.
A kind of preparation method of N doping lead dioxide electrode, described preparation method comprises the following steps:
(1) Titanium base surface coarsening processes: by pure titanium sheet sand papering, after making surface present silvery white metallic luster
Rinse with water；Using NaOH solution to soak subsequently, taking-up water rinses；Finally etch with oxalic acid solution, rinse with water and remove titanium
The oxalic acid of matrix surface remaining and titanium oxalate, obtain the Titanium base of pretreatment；
(2) electro-deposition α-PbO2Bottom: be negative electrode as anode, platinized platinum using the Titanium base that step (1) prepares, is placed in alkalescence
Electro-deposition α-PbO in electroplate liquid2Bottom；Described alkaline Bath is dissolved in water by PbO, NaOH and forms, described PbO Yu NaOH thing
The ratio of the amount of matter is 1:30～40；The volumetric usage of described aqueous solvent is calculated as 5～10L/mol with the amount of the material of PbO；
(3) electro-deposition β-PbO2Active layer: the α-PbO prepared with step (2)2The electrode of bottom is anode, and platinized platinum is cloudy
Pole, the β-PbO of electro-deposition N doping in acidic Bath2Surface activity layer；Described acidic Bath is by Pb (NO3)2、NaF、
Cu(NO3)2, carbamide be dissolved in water composition, described Pb (NO3)2: NaF:Cu (NO3)2: the amount of carbamide material than for 1:0.02～
0.03:0.5～0.6:0.08～0.4；The volumetric usage of described aqueous solvent is with Pb (NO3)2The amount of material be calculated as 1.11～
2.21L/mol。
In step (1), the mass fraction of described NaOH solution is 30%～40%, and soak time is 1.5～3 hours；Institute
The mass fraction stating oxalic acid solution is 15%～20%, and etch period is 1.5～3 hours, etching temperature 70～90 DEG C.
Further, in step (1), described pretreated Titanium base leaves the oxalic acid that mass fraction is 0.5～1.5% in
In save backup.
Further, in step (1), washing for the first time and second time washing use deionized water, third time washing to use
Distilled water.
In step (2), described electro-deposition α-PbO2In underlying process, constant current density is 6～15mA/cm2, electrode spacing is
1～2cm, electroplating time is 1～2 hour, and temperature of electroplating solution is 30～45 DEG C.
Further, in step (3), described electro-deposition β-PbO2During active layer, electrode spacing is 2～4cm, during plating
Between be 2～3 hours, temperature of electroplating solution is 50～95 DEG C.
Further, the invention still further relates to a kind of N doping lead dioxide electrode as in Electrocatalysis Degradation waste water 4-CP should
With.In described application, as indicated with 1, in described Electrocatalysis Degradation waste water, 4-CP device is by electrolyzer 1 and electrification for its Experimental equipment
Learning work station 2 to be composed in series, described electrolyzer comprises to be deposited the anode pool a of anolyte 1-3 and anode 1-1, deposits catholyte 1-5
And the cathode pool b of negative electrode 1-2, cation exchange membrane 1-4, described anode 1-1 is arranged over sample tap 1-6.Described anode
Be communicated with pipeline bottom 1-1 and negative electrode 1-2, described connecting pipe set cation exchange membrane by deposit in the anolyte of anode with
The catholyte depositing in negative electrode separates.Generally, described anode 1-1 elects the N doping lead dioxide electrode preparing gained as, described
Negative electrode 1-2 is Pt electrode, and described anolyte 1-3 is the mixed liquor of sodium sulfate and 4-CP, and described catholyte 1-5 is that sodium sulfate is molten
Liquid.
The beneficial effects are mainly as follows: N doping lead dioxide electrode have cheap, oxygen evolution potential is high,
The features such as catalysis strong, the length in service life of activity.Utilize N doping lead dioxide electrode can realize water by electrochemical oxidation method
Effective removal of middle organic pollution, simple to operate, convenient management, there is Social and economic benef@widely.
Accompanying drawing explanation
Fig. 1 is that the N doping lead dioxide electrode electro-catalysis used by embodiment processes the experimental provision of 4-CP in organic wastewater
Figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This:
Embodiment 1
(1) N doping lead dioxide electrode preparation method: a, Titanium base surface coarsening process: be 1mm by thickness, size
For 6cm2The pure titanium sheet of (2cm × 3cm) is successively with 800# and 1200# sand papering so that surface presents silvery white metal light
Deionized water rinsing is used behind pool；The NaOH solution using mass fraction to be 40% soaks 3h, taking-up deionized water rinsing；Finally
Under the conditions of 90 DEG C, etch 3h with the oxalic acid solution that mass fraction is 20%, remove Titanium base surface remaining with distilled water flushing
Oxalic acid and titanium oxalate, obtain the Titanium base of pretreatment；Pretreated Titanium base, is placed in the oxalic acid that mass fraction is 1.5%
Save backup；B, basic plating α-PbO2Bottom: with step a prepare electrode as anode, the platinized platinum (2cm × 2cm) of homalographic
For negative electrode, it is placed in electro-deposition α-PbO in alkaline Bath2Bottom, electrode spacing is 2cm, and controlling bath temperature is 45 DEG C, electric current
Density is 15mA/cm2, electroplating time is 2h, prepares α-PbO2The electrode of bottom.Described alkaline Bath is by forming preparation as follows:
PbO be 0.1mol/L, NaOH be 4.0mol/L, solvent is water；The volumetric usage of described aqueous solvent is calculated as with the amount of the material of PbO
10L/mol.Take PbO22.32g and NaOH 160g during concrete preparation to be dissolved in successively in 1L water, take 90mL every time during plating and use；
C, acid electroplating N doping β-PbO2Active layer: be coated with α-PbO with prepare in step b2The electrode of bottom is anode, homalographic
Platinized platinum be negative electrode, the β-PbO of electro-deposition N doping in acidic Bath2Surface activity layer, electrode spacing is 4cm, controls
Bath temperature is 95 DEG C, constant voltage 3V and pulse voltage 3V (20s), OCP 0.85V (20s), and electroplating time is 3h, preparation
Obtain the lead dioxide electrode of N doping.Described acidic Bath is by forming preparation as follows: Pb (NO3)2For 0.453mol/L, NaF
For 0.0136mol/L, Cu (NO3)2For 0.272mol/L, carbamide is 0.100mol/L, and solvent is water, the volume of described aqueous solvent
Consumption is with Pb (NO3)2The amount of material be calculated as 2.21L/mol.Pb (NO is taken during concrete preparation3)2150g, NaF 0.571g, Cu
(NO3)251.02g and carbamide 6.006g is dissolved in 1L water successively, takes 125mL every time and use during plating.
(2) electrode prepared with above-mentioned steps (1) is as anode, and platinum electrode is negative electrode, and electrode area is 6cm2(2cm×
3cm), supporting electrolyte is the metabisulfite solution of 0.5mol/L, and constant current density is 17mA/cm2, electrode spacing is 4cm, simulation
Waste water is 0.5mmol/L4-CP, and reaction volume is 500mL, and degradation reaction proceeds to be sampled the most in the same time analyzing, tool
Body device figure such as Fig. 1.After N doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 72.39%.
Embodiment 2
It is 0.0362mol/L that the preparation of N doping lead dioxide electrode removes the concentration of carbamide in step (1) c, and remaining operation is all
Identical with embodiment 1 step (1).
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, and remaining operation is strictly according to the facts
Executing example 1 step (2), after N doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 60.43%.
Embodiment 3
The preparation of N doping lead dioxide electrode except in step (1) c the concentration of carbamide be 0.181mol/L, remaining operation all with
Embodiment 1 step (1) is identical.
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, and remaining operation is strictly according to the facts
Executing example 1 step (2), after N doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 58.27%.
Embodiment 4
N doping lead dioxide electrode preparation manipulation is all identical with embodiment 1 step (1).
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, denitrogenates doping dioxy
Constant current density when changing lead electrode Electrocatalysis Degradation 4-CP is 40mA/cm2, remaining operation such as embodiment 1 step (2), nitrogen is mixed
After miscellaneous lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 88.14%.
Embodiment 5
It is 0.0362mol/L that the preparation of N doping lead dioxide electrode removes the concentration of carbamide in step (1) c, and remaining operation is all
Identical with embodiment 1 step (1).
Using N doping lead dioxide electrode made above is anode, processes the 4-CP of 0.5mmol/L, denitrogenates doping two
Constant current density during lead dioxide electrode Electrocatalysis Degradation 4-CP is 40mA/cm2, remaining operation is such as embodiment 1 step (2), nitrogen
After doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 69.32%.
Embodiment 6
The preparation of N doping lead dioxide electrode except in step (1) c the concentration of carbamide be 0.181mol/L, remaining operation all with
Embodiment 1 step (1) is identical.
Using N doping lead dioxide electrode made above is anode, processes the 4-CP of 0.5mmol/L, denitrogenates doping two
Constant current density during lead dioxide electrode Electrocatalysis Degradation 4-CP is 40mA/cm2, remaining operation is such as embodiment 1 step (2), nitrogen
After doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 70.26%.
Embodiment 7
N doping lead dioxide electrode preparation manipulation is all identical with embodiment 1 step (1).
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, denitrogenates doping dioxy
Constant current density when changing lead electrode Electrocatalysis Degradation 4-CP is 70mA/cm2, remaining operation such as embodiment 1 step (2), nitrogen is mixed
After miscellaneous lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 75.04%.
Embodiment 8
It is 0.0362mol/L that the preparation of N doping lead dioxide electrode removes the concentration of carbamide in step (1) c, and remaining operation is all
Identical with embodiment 1 step (1).
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, denitrogenates doping dioxy
Constant current density when changing lead electrode Electrocatalysis Degradation 4-CP is 70mA/cm2, remaining operation such as embodiment 1 step (2), nitrogen is mixed
After miscellaneous lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 60.53%.
Embodiment 9
The preparation of N doping lead dioxide electrode except in step (1) c the concentration of carbamide be 0.181mol/L, remaining operation all with
Embodiment 1 step (1) is identical.
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, denitrogenates doping dioxy
Constant current density when changing lead electrode Electrocatalysis Degradation 4-CP is 70mA/cm2, remaining operation such as embodiment 1 step (2), nitrogen is mixed
After miscellaneous lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 56.24%.
Embodiment 10
(1) N doping lead dioxide electrode preparation method: a, be 1mm, a size of 6cm by thickness2(2cm × 3cm's)
Pure titanium sheet is successively with 800# and 1200# sand papering so that deionized water rinsing is used after presenting silvery white metallic luster in surface；
The NaOH solution using mass fraction to be 30% soaks 1.5h, taking-up deionized water rinsing；It is finally 15% with mass fraction
Oxalic acid solution under the conditions of 70 DEG C, etch 1.5h, with distilled water flushing remove Titanium base surface remaining oxalic acid and titanium oxalate,
Obtain the Titanium base of pretreatment；Pretreated Titanium base, is placed in the oxalic acid that mass fraction is 0.5% and saves backup；B, with
The electrode that above-mentioned steps a prepares is anode, and the platinized platinum (2cm × 2cm) of homalographic is negative electrode, is placed in electro-deposition in alkaline Bath
α-PbO2Bottom, electrode spacing is 1cm, and controlling bath temperature is 30 DEG C, and electric current density is 6mA cm-2, electroplating time is 1h,
Prepare α-PbO2The electrode of bottom.Described alkaline Bath by form as follows preparation: PbO be 0.2mol/L, NaOH be 6.0mol/
L, solvent is water, and the volumetric usage of described aqueous solvent is calculated as 5L/mol with the amount of the material of PbO；PbO is taken during concrete preparation
22.32g and NaOH 120g is dissolved in 500mL water successively, takes 90mL every time and use during plating；C, with in above-mentioned steps b prepare
It is coated with α-PbO2The electrode of bottom is anode, and the platinized platinum of homalographic is negative electrode, in acidic Bath the β of electro-deposition N doping-
PbO2Surface activity layer, electrode spacing is 2cm, and controlling bath temperature is 50 DEG C, and constant voltage 3V and pulse voltage 3V (20s) are opened
Road current potential 0.85V (20s), electroplating time is 2h, prepares the lead dioxide electrode of N doping；Described acidic Bath is by such as
Lower composition preparation: Pb (NO3)2It is 0.0181mol/L, Cu (NO for 0.906mol/L, NaF3)2For 0.454mol/L, carbamide is
0.2mol/L, solvent is water, and the volumetric usage of described aqueous solvent is with Pb (NO3)2The amount of material be calculated as 1.11L/mol.Specifically join
Pb (NO is taken time processed3)2150g, NaF 0.380g, Cu (NO3)242.58g and carbamide 6.01g is dissolved in 500mL water successively, often
Take 125mL during secondary plating to use.
(2) electrode prepared with above-mentioned steps (1) is as anode, and platinum electrode is negative electrode, and electrode area is 6cm2(2cm×
3cm), supporting electrolyte is the metabisulfite solution of 0.5mol/L, and constant current density is 17mA/cm2, electrode spacing is 4cm, simulation
Waste water is 0.5mmol/L4-CP, and reaction volume is 500mL, and degradation reaction proceeds to be sampled the most in the same time analyzing, tool
Body device figure such as Fig. 1.After N doping lead dioxide electrode electrochemical degradation 4-CP 18h, the clearance of TOC is 69.25%.
Embodiment 11
It is 0.0724mol/L that the preparation of N doping lead dioxide electrode removes the concentration of carbamide in step (1) c, and remaining operation is all
Identical with embodiment 10 step (1).
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, and remaining operation is strictly according to the facts
Executing example 10 step (2), after N doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 58.23%.
Embodiment 12
The preparation of N doping lead dioxide electrode except in step (1) c the concentration of carbamide be 0.362mol/L, remaining operation all with
Embodiment 10 step (1) is identical.
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, and remaining operation is strictly according to the facts
Executing example 10 step (2), after N doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 56.31%.
Embodiment 13
N doping lead dioxide electrode preparation manipulation is all identical with embodiment 10 step (1).
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, denitrogenates doping dioxy
Constant current density when changing lead electrode Electrocatalysis Degradation 4-CP is 40mA/cm2, remaining operation such as embodiment 10 step (2), nitrogen is mixed
After miscellaneous lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 83.54%.
Embodiment 14
It is 0.0724mol/L that the preparation of N doping lead dioxide electrode removes the concentration of carbamide in step (1) c, and remaining operation is all
Identical with embodiment 10 step (1).
Using N doping lead dioxide electrode made above is anode, processes the 4-CP of 0.5mmol/L, denitrogenates doping two
Constant current density during lead dioxide electrode Electrocatalysis Degradation 4-CP is 40mA/cm2, remaining operation is such as embodiment 10 step (2), nitrogen
After doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 66.43%.
Embodiment 15
The preparation of N doping lead dioxide electrode except in step (1) c the concentration of carbamide be 0.362mol/L, remaining operation all with
Embodiment 10 step (1) is identical.
Using N doping lead dioxide electrode made above is anode, processes the 4-CP of 0.5mmol/L, denitrogenates doping two
Constant current density during lead dioxide electrode Electrocatalysis Degradation 4-CP is 40mA/cm2, remaining operation is such as embodiment 10 step (2), nitrogen
After doping lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 67.26%.
Embodiment 16
N doping lead dioxide electrode preparation manipulation is all identical with embodiment 10 step (1).
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, denitrogenates doping dioxy
Constant current density when changing lead electrode Electrocatalysis Degradation 4-CP is 70mA/cm2, remaining operation such as embodiment 10 step (2), nitrogen is mixed
After miscellaneous lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 76.24%.
Embodiment 17
It is 0.0724mol/L that the preparation of N doping lead dioxide electrode removes the concentration of carbamide in step (1) c, and remaining operation is all
Identical with embodiment 10 step (1).
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, denitrogenates doping dioxy
Constant current density when changing lead electrode Electrocatalysis Degradation 4-CP is 70mA/cm2, remaining operation such as embodiment 10 step (2), nitrogen is mixed
After miscellaneous lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 58.56%.
Embodiment 18
The preparation of N doping lead dioxide electrode except in step (1) c the concentration of carbamide be 0.362mol/L, remaining operation all with
Embodiment 10 step (1) is identical.
Using N doping lead dioxide electrode made above is anode, processes 0.5mmol/L4-CP, denitrogenates doping dioxy
Constant current density when changing lead electrode Electrocatalysis Degradation 4-CP is 80mA/cm2, remaining operation such as embodiment 10 step (2), nitrogen is mixed
After miscellaneous lead dioxide electrode electrochemical degradation 4-CP 9h, the clearance of TOC is 53.67%.
Claims (8)
1. a N doping lead dioxide electrode, it is characterised in that: described N doping lead dioxide electrode is with roughened place, surface
Reason pure titanium sheet be matrix, by galvanoplastic the most successively at described matrix surface electro-deposition α-PbO2Bottom and electricity are heavy
Long-pending β-PbO2Active layer prepares.
2. the preparation method of a N doping lead dioxide electrode, it is characterised in that described preparation method comprises the following steps:
(1) Titanium base surface coarsening processes: by pure titanium sheet sand papering, make surface use water after presenting silvery white metallic luster
Rinse；Using NaOH solution to soak subsequently, taking-up water rinses；Finally etch with oxalic acid solution, rinse with water and remove Titanium base
The oxalic acid of surface remaining and titanium oxalate, obtain the Titanium base of pretreatment；
(2) electro-deposition α-PbO2Bottom: be negative electrode as anode, platinized platinum using the Titanium base that step (1) prepares, is placed in basic plating
Electro-deposition α-PbO in liquid2Bottom；Described alkaline Bath is dissolved in water by PbO, NaOH and forms, described PbO Yu NaOH material
The ratio of amount is 1:30～40；The volumetric usage of described aqueous solvent is calculated as 5～10L/mol with the amount of the material of PbO；
(3) electro-deposition β-PbO2Active layer: the α-PbO prepared with step (2)2The electrode of bottom is anode, and platinized platinum is negative electrode,
β-the PbO of electro-deposition N doping in acidic Bath2Surface activity layer；Described acidic Bath is by Pb (NO3)2、NaF、Cu
(NO3)2, carbamide be dissolved in water composition, described Pb (NO3)2: NaF:Cu (NO3)2: the amount of carbamide material is than for 1:0.02～0.03:
0.5～0.6:0.08～0.4；The volumetric usage of described aqueous solvent is with Pb (NO3)2The amount of material be calculated as 1.11～2.21L/
mol。
3. preparation method as claimed in claim 2, it is characterised in that: in step (1), the mass fraction of described NaOH solution is
30%～40%, soak time is 1.5～3 hours；The mass fraction of described oxalic acid solution is 15%～20%, and etch period is
1.5～3 hours, etching temperature 70～90 DEG C.
4. preparation method as claimed in claim 2, it is characterised in that: in step (1), described pretreated Titanium base is deposited
The oxalic acid that mass fraction is 0.5%～1.5% saves backup.
5. preparation method as claimed in claim 2, it is characterised in that: in step (1), washing for the first time and second time washing are adopted
With deionized water, third time washing uses distilled water.
6. preparation method as claimed in claim 2, it is characterised in that: in step (2), described electro-deposition α-PbO2Underlying process
Middle constant current density is 6～15mA/cm2, electrode spacing is 1～2cm, and electroplating time is 1～2 hour, and temperature of electroplating solution is 30
～45 DEG C.
7. preparation method as claimed in claim 2, it is characterised in that: in step (3), described electro-deposition β-PbO2Active layer mistake
In journey, electrode spacing is 2～4cm, and electroplating time is 2～3 hours, and temperature of electroplating solution is 50～95 DEG C.
A kind of N doping lead dioxide electrode the most as claimed in claim 1 is as the application of 4-CP in Electrocatalysis Degradation waste water.
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| CN201610677730.4A CN106315772B (en) | 2016-08-17 | 2016-08-17 | A kind of N doping lead dioxide electrode and its preparation method and application |
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| CN201610677730.4A CN106315772B (en) | 2016-08-17 | 2016-08-17 | A kind of N doping lead dioxide electrode and its preparation method and application |
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| CN106315772B CN106315772B (en) | 2019-06-14 |
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| CN102774932A (en) * | 2012-07-16 | 2012-11-14 | 浙江工业大学 | Method for removing COD (chemical oxygen demand) and ammonia nitrogen from wastewater by using titanium-base lead peroxide composite electrode |
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| EP2687483A1 (en) * | 2012-07-16 | 2014-01-22 | Basf Se | Graphene containing nitrogen and optionally iron and/or cobalt |
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