CN108217852A - High life, high catalytic activity lead dioxide electrode - Google Patents
High life, high catalytic activity lead dioxide electrode Download PDFInfo
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- CN108217852A CN108217852A CN201810025550.7A CN201810025550A CN108217852A CN 108217852 A CN108217852 A CN 108217852A CN 201810025550 A CN201810025550 A CN 201810025550A CN 108217852 A CN108217852 A CN 108217852A
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- lead dioxide
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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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
-
- 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
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
Abstract
High life, high catalytic activity lead dioxide electrode, with SnO2‑Sb2O3As bottom, with α PbO2As middle layer, and with β PbO2It is prepared as surface-active layer.The obtained brown lead oxide dense uniform of the present invention, particle is smaller, has larger specific surface area.Meanwhile surface-active layer strong adhesive force, it is not easily to fall off；Surface it is smooth securely, can acid-alkali-corrosive-resisting, have good catalytic activity and service life.In addition, present invention process condition is simple, of low cost, products obtained therefrom performance is stablized, and is suitble to industrialized production, can be widely applied to the field by electro-catalytic oxidation technology treated sewage, has far-reaching market prospects.
Description
Technical field
The present invention relates to a kind of lead dioxide electrode, this electrode can be used as the anode of electro-catalysis sewage disposal.
Background technology
Sewage handling problem is all the hot spot of research all the time.With the development of industrial technology, the pollution of industrial discharge
Wastewater flow rate is also growing day by day, this causes originally shorter water resource to become more nervous.It is and most of in these pollutants
All it is organic pollution, when it is discharged in water, destruction can be generated to ecological environment.In numerous sewage disposal technologies, electricity is urged
Change that oxidizing process is low for equipment requirements, processing speed is fast, easy to operate, cleanliness without any pollution and is easy to large-scale application, be a kind of ring
Border friendly technology.It is constantly subjected to extensive concern in recent years, is an important development direction of following sewage treatment field.Positive grade
The property of electrode material has the efficiency of Electrocatalytic Oxidation crucial influence.
The steady electrode of titanium-based shape is prepared by way of heat deposition or electro-deposition with catalytic activity in titanium substrate
Metal oxide has good catalytic activity, and corrosion-resistant, preparation is simply, and chemical stability is good, in electrochemical oxidation skill
Using relatively broad in art.Preparing for lead dioxide electrode is simple, of low cost and it is with good electric conductivity so that its
It has a good application prospect in electrocatalytic oxidation field.
PbO2Although electrode has numerous advantages, some problems are also faced.Such as PbO2Have inside coating larger
Internal stress, generated nascent oxygen is easily diffused into through superficial layer in substrate in electrolytic process, so as to cause substrate
Passivation, coating come off, and reduce the electrochemical stability and service life of electrode.Therefore make while electrode catalyst activity is ensured
It is with higher service life just with vital meaning.
Invention content
An object of the present invention is to provide a kind of preparation method of lead dioxide electrode, can effectively improve electrode use
Service life is without reducing catalytic activity.
The preparation method of lead dioxide electrode according to the present invention includes：
There is provided titanium substrate and being polished be placed on oil removing cleaning treatment it is spare in absolute ethyl alcohol；
After taking out titanium substrate drying, bottom is brushed in titanium substrate using coating liquid, wherein coating liquid composition is：3~
25mL n-butanols, 0.1~8mL concentrated hydrochloric acids, 0.5~10g stannic chloride pentahydrates and 0.1~8g antimony trichlorides；
It repeats to brush bottom 5-10 times, is dried after brushing every time, 2- is finally roasted under conditions of 450-500 DEG C
4h；
α-PbO are prepared on bottom by the method for electro-deposition2Middle layer, wherein current density are 5mA/cm2~65mA/
cm2,, total electrodeposition time is 1~2h, and electrodeposition temperature is 30~80 DEG C, electrode spacing 2cm, and electrodeposit liquid composition is 0.1
The NaOH of the PbO and 1~10mol/L of~1mol/L；And
The method of electro-deposition is continued through in α-PbO2β-PbO are prepared in middle layer2Surface-active layer, wherein current density
For 20mA/cm2~85mA/cm2, total electrodeposition time is 1~2h, and electrodeposition temperature is 25~100 DEG C, electrode spacing 2cm,
Electrodeposit liquid composition is 0.1~1mol/L Pb (NO3) 2,0.05~2mol/L HBO3,0.5~2g/L NaF, 10~100mg/
L graphene oxides (GO) and 10~100mg/L nano SiCs.
The present invention using plumbi nitras, boric acid, sodium fluoride, graphene, nanometer silicon carbide as surface-active layer electrodeposit liquid into
Point, with SnO2-Sb2O3As bottom, with α-PbO2As middle layer, the titanium dioxide of even compact is prepared by ad hoc approach
Lead electrode.
Cathode used can be selected from graphite flake, copper sheet, titanium sheet, stainless steel substrates when middle layer and surface-active layer electro-deposition
And platinized platinum, anode can be titanium sheet or titanium net.Yin, yang electrode plate can select material different or of the same race.Anodic-cathodic used
Plate is preferably dimensioned to be 1 × 4cm2。
The oil removing cleaning of titanium substrate can include：It is cleaned by ultrasonic 5-15min in acetone, ethyl alcohol and deionized water respectively.
According to a preferred embodiment of the present invention, the mass ratio of butter of tin and antimony trichloride is 10 in coating liquid:1.
This bottom has excellent binding characteristic, can pass through α-PbO again2Middle layer improves the combination between surface-active layer
Power mitigates the generation of electro-deposition distortion.
The present invention also provides the lead dioxide electrodes according to prepared by the above method.This lead dioxide electrode can be
It is used as anode in electro-catalysis sewage disposal.
In a preferred embodiment of the invention, the incorporation of graphene oxide is 20~60mg/L, and nanometer silicon carbide is mixed
Enter amount for 10~50mg/L.The purpose of incorporation nanometer silicon carbide and graphene oxide is that the two is promoted to act synergistically, and is being mended
Inside full brown lead oxide while vacancy, control brown lead oxide pattern, guarantee catalytic activity, the electrode longevity of brown lead oxide is improved
Life.
The present invention had not only improved the lead dioxide electrode service life, but also did not reduced electrode catalyst activity.
In addition, the present invention controls the mixing ratio of the two also by adding two kinds of nanometer silicon carbide, graphene oxide substances
Example achievees the purpose that control brown lead oxide pattern.Obtained brown lead oxide dense uniform, particle is smaller, has larger ratio
Surface area.Meanwhile surface-active layer strong adhesive force, it is not easily to fall off.Surface it is smooth securely, can acid-alkali-corrosive-resisting, have it is good
Catalytic activity and service life.
In addition, present invention process condition is simple, of low cost, products obtained therefrom performance is stablized, and is suitble to industrialized production, can be wide
The general field being applied to through electro-catalytic oxidation technology treated sewage, has far-reaching market prospects.
Description of the drawings
Fig. 1 is the bottom scanning electron microscope (SEM) photograph prepared in titanium net substrate by coating thermolysis process；
Fig. 2 is α-PbO2The scanning electron microscope (SEM) photograph of middle layer；
Fig. 3 is the combination electrode scanning electron microscope (SEM) photograph of no nanometer silicon carbide and graphene oxide doped；
Fig. 4 is while the combination electrode scanning electron microscope (SEM) photograph of dopen Nano silicon carbide and graphene oxide.
Specific embodiment
The lead dioxide electrode preparation method of the present invention is made further below by specific embodiment and attached drawing
It is described in detail, but it is not intended to restrict the invention.
Embodiment 1
Titanium net is cleaned by ultrasonic 15min, natural air drying after taking-up by acetone, ethyl alcohol, deionized water respectively.Then lead to
The method for crossing coating thermal decomposition prepares Ti/SnO on titanium net surface2- Sb bottoms, coating liquid composition used is n-butanol 5ml, dense salt
Sour 3ml, butter of tin 3g, antimony trichloride 0.3g.When covering liquid to be coated is completely dissolved into transparent and homogeneous shape, coating is dipped by brush
Liquid is coated onto in titanium net.It is subsequently placed in Constant Temp. Oven and dries 15min under the conditions of 120 DEG C, then take out again
It is secondary to be brushed.It is so repeated after 8 times, 2h is roasted under conditions of 500 DEG C in Muffle furnace.
Continue to deposit to obtain one layer of α-PbO in electrode surface by the method for electro-deposition2Middle layer.Electrodeposit liquid used
The NaOH of PbO and 4mol/L for 0.1mol/L, current density used are 40mA/cm2.Temperature is 30 DEG C, electro-deposition 1h.
It then proceedes to obtain β-PbO in electrode surface electro-deposition2Surface-active layer, electrodeposit liquid used are 0.5mol/L
Pb(NO3)2、0.05mol/L HBO3, 0.1g/LNaF, current density used be 20mA/cm2.Temperature is 60 DEG C, electro-deposition
1h obtains undoped lead dioxide electrode.
Analytical table is carried out to the surface topography and catalytic performance of electrode with scanning electron microscope (SEM) and ultraviolet specrophotometer
Sign.
As shown in Figure 1, it can be seen that it is uniformly cracked by coating the bottom prepared by the method for thermal decomposition, it can be by titanium substrate
Basic covering.So as to enhance the binding force between substrate and each layer, and base passivation can be prevented.
As shown in Figure 2, it can be seen that the α-PbO obtained by the method for electro-deposition2Middle layer even compact, can be the bottom of by
Layer covering.The presence of middle layer can mitigate the electrodeposition distortion of overlay coating, enhancing substrate and β-PbO2Between surface-active layer
Binding force.
As shown in Figure 3, it can be seen that the undoped β-PbO obtained by the method for electro-deposition2Surface-active layer
Grain is uneven, and particle is larger, this can reduce β-PbO2Active surface, so as to influence its catalytic performance.Meanwhile β-PbO2
Surface is cracked, and undoubtedly this can reduce the difficulty that solution enters electrode interior, influences its service life.
When temperature is 50 DEG C, current density 60mA/cm2, electrode area 2cm2, use undoped brown lead oxide
Electrode carries out catalysis degeneration experiment to 2,4 di amino toluene (TDA).Wherein the initial concentration of TDA is 0.3g/L.Measure TDA's
Degradation rate is 76.6%.
Electrode life is tested by accelerated life test.Using test electrode as anode, using copper sheet as cathode, adopt
With the method for constant current, holding current density is 2A/cm2, electrode spacing 2cm, in 2mol/L H2SO4Middle carry out life test
Experiment increases to 10V using voltage and inactivates standard as electrode.As a result, it has been found that for undoped electrode, the service life is 12 small
When.
Embodiment 2
It is similar to Example 1, same method acquisition is taken to be coated with bottom and α-PbO2The electrode of middle layer, then in electricity
Pole surface obtains β-PbO by the method for electrochemical deposition2Surface-active layer, electrodeposit liquid used are 0.5mol/L Pb
(NO3)2、0.05mol/L HBO3, 0.1g/LNaF, 50mg/L graphene oxides (GO), 20mg/L nano SiCs；Electric current used
Density is 20mA/cm2.Temperature is 60 DEG C, electro-deposition 1h, so that it may obtain novel brown lead oxide combination electrode.
Analytical table is carried out to the surface topography and catalytic performance of electrode with scanning electron microscope (SEM) and ultraviolet specrophotometer
Sign.As shown in Figure 4, it can be seen that dopen Nano silicon carbide and graphene oxide answers while being obtained by the method for electro-deposition
β-the PbO on composite electrode surface2Particle even compact, and grain size is smaller.This effective catalytic surface that will increase electrode, raising are urged
Change performance.Meanwhile the nanometer silicon carbide and graphene oxide of surface doping, it can mutually cooperate with, supplement electrode surface vacancy is repaiied
Multiple vacancy, promotes electrode life.Catalysis degeneration experiment and service life are carried out to it in the same manner as shown in Example 1 to it
Test, finds after 3 hours of degrading, the degradation rate of TDA is up to 88.5%, and electrode life is up to 57 hours.
It is compared by embodiment it can be found that when the doping that nanometer silicon carbide and graphene oxide are carried out to electrode surface
When, electrode life can be significantly improved, while ensure the high catalytic activity of electrode.Electrode life after overdoping improves
4.75 times, catalytic activity also improves 1.16 times.Which solves electrode lives and electrode catalyst performance to be difficult to what is obtained simultaneously
Technical barrier, thus have a vast market application prospect.
Claims (6)
1. a kind of preparation method of lead dioxide electrode, including：
There is provided titanium substrate and being polished be placed on oil removing cleaning treatment it is spare in absolute ethyl alcohol；
After taking out titanium substrate drying, bottom is brushed in titanium substrate using coating liquid, wherein coating liquid composition is：3~25mL is just
Butanol, 0.1~8mL concentrated hydrochloric acids, 0.5~10g stannic chloride pentahydrates and 0.1~8g antimony trichlorides；
It repeats to brush bottom 5-10 times, is dried after brushing every time, 2-4h is finally roasted under conditions of 450-500 DEG C；
α-PbO are prepared on bottom by the method for electro-deposition2Middle layer, wherein current density are 5mA/cm2~65mA/cm2,,
Total electrodeposition time is 1~2h, and electrodeposition temperature is 30~80 DEG C, electrode spacing 2cm, electrodeposit liquid composition for 0.1~
The NaOH of the PbO and 1~10mol/L of 1mol/L；And
The method of electro-deposition is continued through in α-PbO2β-PbO are prepared in middle layer2Surface-active layer, wherein current density are
20mA/cm2~85mA/cm2, total electrodeposition time is 1~2h, and electrodeposition temperature is 25~100 DEG C, electrode spacing 2cm, electricity
It is 0.1~1mol/L Pb (NO3) 2,0.05~2mol/L HBO3,0.5~2g/L NaF, 10~100mg/L to deposit liquid composition
Graphene oxide (GO) and 10~100mg/L nano SiCs.
2. cathode used in preparation method according to claim 1, wherein electro-deposition is selected from graphite flake, copper sheet, titanium sheet, no
Become rusty steel disc and platinized platinum, and anode is titanium sheet or titanium net.
3. the oil removing cleaning of preparation method according to claim 1, wherein titanium substrate includes：Respectively acetone, ethyl alcohol and
It is cleaned by ultrasonic 5-15min in deionized water.
4. the mass ratio of butter of tin and antimony trichloride is 10 in preparation method according to claim 1, wherein coating liquid:
1。
5. the lead dioxide electrode prepared according to claim 1-4 the methods.
6. lead dioxide electrode according to claim 5 is used as anode in electro-catalysis sewage disposal.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109023420A (en) * | 2018-07-18 | 2018-12-18 | 昆明理工大学 | A kind of nickel electrodeposition aluminum-base composite anode and preparation method thereof |
| CN109763143A (en) * | 2019-01-22 | 2019-05-17 | 华中科技大学 | A kind of processing method for resource recovery of waste lead acid battery |
| CN109970155A (en) * | 2019-01-28 | 2019-07-05 | 中南大学 | A kind of preparation method of graphene oxide modification lead dioxide electrode |
| CN110257857A (en) * | 2019-07-15 | 2019-09-20 | 惠州市臻鼎环保科技有限公司 | The preparation method and Anodic of Anodic |
| CN112093858A (en) * | 2020-08-17 | 2020-12-18 | 浙江工业大学 | Preparation method and parameter design method of long-life lead dioxide electrode |
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| CN109970155B (en) * | 2019-01-28 | 2022-01-04 | 中南大学 | Preparation method of lead dioxide electrode modified by graphene oxide |
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| CN112093858B (en) * | 2020-08-17 | 2022-11-04 | 浙江工业大学 | Preparation method and parameter design method of long-life lead dioxide electrode |
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