CN110255677A - Multicomponent is co-doped with modified ti-supported lead dioxide electric pole and preparation method thereof - Google Patents
Multicomponent is co-doped with modified ti-supported lead dioxide electric pole and preparation method thereof Download PDFInfo
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- CN110255677A CN110255677A CN201910608311.9A CN201910608311A CN110255677A CN 110255677 A CN110255677 A CN 110255677A CN 201910608311 A CN201910608311 A CN 201910608311A CN 110255677 A CN110255677 A CN 110255677A
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- doped
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- multicomponent
- titanium
- electric pole
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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
- C02F1/467—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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
Modified ti-supported lead dioxide electric pole and preparation method thereof is co-doped with the invention discloses multicomponent, including Titanium base, middle layer (tin-antimony oxide), active layer (multicomponent is co-doped with), compared to undoped electrode, multicomponent is co-doped with pattern, higher current efficiency, the longer reinforcing life that modified electrode has more dense uniform, wherein F‑、Co2+, that polyethylene glycol is co-doped with modified electrode performance is best, reinforcing life, which is compared, improves 32.4% undoped with electrode；The invention also discloses the preparation methods of above-mentioned ti-supported lead dioxide electric pole, the preparation method synthesizes tin-antimony oxide bottom and as anode using sol-gel method on pretreated titanium-base, titanium plate is as cathode, the electro-deposition active layer in the nitrate containing different dopant and acetic acid salt blend deposit liquid system is realized using electrochemical method, it obtains multicomponent and is co-doped with modified ti-supported lead dioxide electric pole, the preparation method simplifies production technology, while improving product quality.
Description
Technical field
The present invention relates to electrochemical catalytic oxidation water process and field of hydrometallurgy, and in particular to multicomponent is co-doped with modified
Ti-supported lead dioxide electric pole and preparation method thereof.
Background technique
Although cost is relatively low for the bioanalysis in traditional water process, seem incompetent for some persistent organic pollutants
For power；Chemical treatment needs additional chemical reagent, has high-cost while there is also secondary pollution risk；Emerging electrolysis
Method processing water have many advantages, such as need not add chemical agent, equipment volume is small, land occupation is little, do not generate secondary pollution and by pass
Note has been used for the waste water for handling the organic pollutants such as alcohol-containing, aldehyde, phenol and dyestuff, according to electrochemical oxidation process water process electrode
Requirement, need efficiently, the new electrode materials that the service life is long, energy consumption is low.And it needs to avoid analysis oxygen during electrocatalytic oxidation
The generation of side reaction, this requires anodes higher oxygen evolution potential.It take dimensional stable anode (DSA) as the electrochemistry skill of electrode material
Art starts to attract much attention, which overcomes the presence such as traditional graphite electrode, platinum electrode, lead-containing alloy electrode
Some shortcomings, as the Typical Representative of insoluble anode, ti-supported lead dioxide electric pole is that generally acknowledged at present have greater advantage
Electro catalytic electrode, have that oxygen evolution potential is high, oxidability is strong, corrosion resistance when ti-supported lead dioxide electric pole is electrolysed in aqueous solution
Good, good conductivity, can be by characteristics such as larger current, therefore be widely used in water process and field of hydrometallurgy.Although titanium-based
Lead dioxide electrode has above-mentioned multiple advantages, but it still has biggish improvement space, it is easy to pass through modification (coating knot
Structure is co-doped with situation etc.) improve oxygen evolution potential and the service life of electrode.
Due to conventional anode β-PbO2Adhesive force of the active layer on Titanium base is low, easy peeling, the service life in electrolytic process
It is short, for this purpose, the present invention is in Titanium base and β-PbO2Between introduce middle layer, on the one hand middle layer is played β-PbO2Layer is very well
Ground is bonded on matrix, on the other hand can effectively slow down the corrosion of Titanium base, while multicomponent is co-doped with modified brown lead oxide sun
It can be extremely effectively improved anode surface pattern, improve its catalytic activity.
Summary of the invention
Modified ti-supported lead dioxide electric pole, the modified electricity of multi-component doped are co-doped with the purpose of the present invention is to provide multicomponent
The great pattern for having more dense uniform, higher current efficiency, longer reinforcing life；Preparation method simplifies production work
Skill, while improving product quality.
It includes prepared by Titanium base, sol-gel method that multicomponent, which is co-doped with modified ti-supported lead dioxide electric pole, in the present invention
Tin-antimony oxide bottom and electro-deposition multicomponent are co-doped with modified β-PbO2Active layer, the Titanium base are titanium silk, titanium tube, titanium net
Or the substances such as titanium plate.
Multicomponent is co-doped with the preparation method of modified ti-supported lead dioxide electric pole in the present invention, includes the following steps:
Step 1: Titanium base is pre-processed；
Step 2: tin-antimony oxide bottom is prepared by sol-gel method；
Step 3: multicomponent being prepared by electrodeposition process and is co-doped with modified β-PbO2 active layer；
Step 4: the sol-gel method is prepared into the titanium-base in tin antimony oxide coated as anode, the titanium-based
Plate is as cathode, the electro-deposition active layer in nitrate and acetic acid salt blend deposit liquid system, and electro-deposition current density is 10~
500A/m2, 30~70 DEG C of electrodeposition temperature, 1~4h of electrodeposition time；In the nitrate and acetic acid salt blend deposit liquid system
Dopant contains F-, polyethylene glycol, Co2+/Fe2+/Zn2+/Ce3+In any metal ion.
Nitrate and acetic acid salt blend deposit liquid system are configured using deionized water, wherein containing 50~150g/L Pb2+,
20~100g/L Cu2+, 0.2~0.9g/L F-, 0.2~1.0g/L Co2+/Fe2+/Zn2+/Ce3+With 0.2~1.0g/L PEG.
The preparation step of tin-antimony oxide bottom is prepared in the present invention to the pretreatment of Titanium base and sol-gel method,
It is specific as follows:
Wherein, the pretreatment process of Titanium base are as follows: by Titanium base cutting, blasting treatment, remove surface scale, then exist
10~20min of ultrasonic oil removing in ethanol solution is finally placed it in and is etched 1~3h in slightly boiled oxalic acid solution, after the completion of etching
It is rinsed with deionized water spare.
Sol-gel method prepares tin-antimony oxide bottom process are as follows: tin alkoxide and antimony alkoxide are dissolved in ethanol solution and being made
At precursor liquid, a small amount of deionized water is then added and is stirred continuously, is allowed to that hydrolysis, polycondensation reaction occurs, forms colloidal sol, and then
Colloidal sol is coated in step 1 on the surface of spare Titanium base, then in air dry oven dry 5 at 100~130 DEG C~
Dry Titanium base is placed in Muffle furnace at 450~550 DEG C after being sintered 50~70min by 10min, and taking-up naturally cools to room
Temperature.
Oxalic acid etching liquid is prepared using deionized water, and mass concentration is 3%~10%.
Precursor liquid is prepared using ethyl alcohol, wherein containing 450~600g/L C2H5OH, 60~100g/L Sn4+With 20
~40g/L Sb3+。
Beneficial effect of the invention is that
(1), using titanium plate as matrix, tin-antimony oxide layer is bottom, is free of α-PbO2Middle layer, in tin-antimony oxide layer
Outer Direct precipitation multicomponent is co-doped with modified β-PbO2Active layer.
(2), the present invention is co-doped with by multi-component, is improved electro catalytic activity, is co-doped with modification using multicomponent of the present invention
Ti-supported lead dioxide electric pole improve the current efficiency of acid copper.
(3), multicomponent of the present invention is co-doped with the reinforcing life of modified ti-supported lead dioxide electric pole and does not mix in the prior art
Miscellaneous ti-supported lead dioxide electric is compared, wherein F-、Co2+, polyethylene glycol is co-doped with the reinforcing life of modified electrode and improves 32.4%.
The preparation method is that β-PbO is directly carried out on the Titanium base that sol-gel method is prepared with tin-antimony oxide bottom2
The deposition of active layer eliminates α-PbO2The preparation section of layer, simplifies the preparation method of ti-supported lead dioxide electric pole, preparation side
The simplification of method can be such that the preparation efficiency of ti-supported lead dioxide electric pole is improved, due to eliminating α-PbO2The preparation section of layer,
Also the technological parameter for needing to adjust and control in the process is eliminated accordingly, is conducive to the raising of the product qualified rate of product,
And thus reduce production cost.
Detailed description of the invention
Below in conjunction with attached drawing, invention is further described in detail.
Fig. 1 is the structural schematic diagram that multicomponent of the present invention is co-doped with modified anode of lead dioxide.
Fig. 2 is the undoped and F of the present invention-、Co2+, polyethylene glycol be co-doped with modified β-PbO2The powder of active layer electrode spreads out
Penetrate map.
Fig. 3, Fig. 4 are the present invention undoped with F-、Co2+, polyethylene glycol be co-doped with modified β-PbO2The high definition of active layer electrode
Figure.
Fig. 5, Fig. 6 are the undoped and F of the present invention-、Co2+, polyethylene glycol be co-doped with modified β-PbO2The SEM of active layer electrode
Figure.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
F-、Co2+, polyethylene glycol be co-doped with modified ti-supported lead dioxide electric pole, refering to fig. 1, specific structure includes:
Titanium base pretreatment；
Sol-gel method prepares tin-antimony oxide bottom；
Electro-deposition F-、Co2+, polyethylene glycol be co-doped with modified β-PbO2Active layer.
In the present embodiment, Titanium base uses titanium net.
F-、Co2+, polyethylene glycol be co-doped with the specific of modified ti-supported lead dioxide electric pole the preparation method is as follows:
(1) pretreatment of Titanium base: by Titanium base cutting, blasting treatment, remove surface scale, then in ethanol solution
Middle ultrasound oil removing 10min, finally places it in 3% slightly boiled oxalic acid solution and etches 2h, rushed after the completion of etching with deionized water
It washes spare；
(2) sol-gel method prepares tin-antimony oxide bottom: tin alkoxide and antimony alkoxide are dissolved in front of being made in ethanol solution
Liquid is driven, a small amount of deionized water is then added and is stirred continuously, is allowed to that hydrolysis, polycondensation reaction occurs, forms colloidal sol, it and then will be molten
Glue is coated on the surface of Titanium base spare in step 1, is then dried 5min at 100 DEG C in air dry oven, will be dried
Titanium base be placed in Muffle furnace at 500 DEG C be sintered 60min after, take out cooled to room temperature.
(3) electro-deposition F-、Co2+, polyethylene glycol be co-doped with modified β-PbO2Active layer: sol-gel method is prepared into tin antimony
The titanium-base of oxide underlayer is as anode, and titanium-base is as cathode, the electricity in nitrate and acetic acid salt blend deposit liquid system
Active layer deposited, electro-deposition current density are 50 A/m2, 50 DEG C of electrodeposition temperature, electrodeposition time 2h；The nitrate and vinegar
Hydrochlorate, which is blended in deposit liquid system, contains 60g/L Pb2+, 40g/L Cu2+, 0.5g/L F-, 0.8g/L Co2+And 0.8g/L
PEG。
To undoped ti-supported lead dioxide electric pole and F-、Co2+, polyethylene glycol be co-doped with modified ti-supported lead dioxide electric pole
It is detected.
Reinforcing life test: tap water prepares 15% sulfuric acid, in 40 DEG C, 20000 A/m of current density2Under conditions of into
Row, the reinforcing life undoped with ti-supported lead dioxide electric pole are 600h, are co-doped with the reinforcing longevity of modified ti-supported lead dioxide electric pole
Life is 887h, and the reinforcing life of electrode improves 32.4%.
Undoped ti-supported lead dioxide electric pole and F-、Co2+, polyethylene glycol be co-doped with modified ti-supported lead dioxide electric pole
Powder diffraction spectrum comparison diagram, referring to Fig.2, by F-、Co2+, polyethylene glycol is to β-PbO2Active layer is co-doped with modified diffraction pattern
Spectrum is coincide well with undoped map, is illustrated to be co-doped with and is had no effect on β-PbO2Structure.
Undoped ti-supported lead dioxide electric pole and F-、Co2+, polyethylene glycol be co-doped with modified ti-supported lead dioxide electric pole
High definition figure, refering to Fig. 3, Fig. 4, by F-、Co2+, polyethylene glycol is to β-PbO2Active layer is co-doped with modification, the surface topography of electrode
Biggish change is obtained, apparently seems more smooth exquisiteness, is conducive to the raising of anode life.
Undoped ti-supported lead dioxide electric pole and F-、Co2+, polyethylene glycol be co-doped with modified ti-supported lead dioxide electric pole
SEM figure, refering to Fig. 5, Fig. 6, by F-、Co2+, polyethylene glycol is to β-PbO2Active layer is co-doped with modification, and electrode surface particle becomes
The compactness of more fine uniform small, that structure becomes, microstructure increases, and reduces β-PbO2The internal stress of active layer improves
β-PbO2The stability of active layer, β-PbO2Active layer and tin-antimony oxide bottom are provided with better binding ability, make to be modified
The service life of electrode is extended afterwards.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention, for this field skill
For art personnel, it is clear that invention is not limited to the details of the above exemplary embodiments.
In the case where the spirit or essential attributes of invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the embodiments should be taken as exemplary, and is non-limiting, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
Further, it is understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (5)
1. multicomponent is co-doped with modified ti-supported lead dioxide electric pole, it is characterised in that prepared including Titanium base, sol-gel method
Tin-antimony oxide bottom and electro-deposition multicomponent are co-doped with modified β-PbO2Active layer, the Titanium base are titanium silk, titanium tube, titanium net
Or the substances such as titanium plate.
Multicomponent is co-doped with the preparation method of modified ti-supported lead dioxide electric pole, which comprises the steps of:
Step 1: Titanium base is pre-processed；
Step 2: tin-antimony oxide bottom is prepared by sol-gel method；
Step 3: multicomponent being prepared by electrodeposition process and is co-doped with modified β-PbO2 active layer；
Step 4: the sol-gel method being prepared into the titanium-base in tin antimony oxide coated as anode, the titanium-base is made
For cathode, the electro-deposition active layer in nitrate and acetic acid salt blend deposit liquid system, electro-deposition current density is 10~500A/
m2, 30~70 DEG C of electrodeposition temperature, 1~4h of electrodeposition time；It is adulterated in the nitrate and acetic acid salt blend deposit liquid system
Agent contains F-, polyethylene glycol, Co2+/Fe2+/Zn2+/Ce3+In any metal ion.
2. the preparation method that multicomponent as claimed in claim 2 is co-doped with modified ti-supported lead dioxide electric pole, it is characterised in that
The detailed process of the step 1 are as follows: by Titanium base cutting, blasting treatment, remove surface scale, then surpass in ethanol solution
Sound 10~20min of oil removing finally places it in 1~3h of etching in slightly boiled oxalic acid etching liquid, uses deionized water after the completion of etching
It rinses spare.
3. the preparation method that multicomponent as claimed in claim 2 is co-doped with modified ti-supported lead dioxide electric pole, it is characterised in that
The detailed process of the step 2 are as follows: tin alkoxide and antimony alkoxide are dissolved in ethanol solution and precursor liquid are made, is then added and goes on a small quantity
Ionized water is simultaneously stirred continuously, and is allowed to that hydrolysis, polycondensation reaction occurs, is formed colloidal sol, is and then coated on colloidal sol spare in step 1
Titanium base surface on, then dry 5~10min at 100~130 DEG C in air dry oven, dry Titanium base is set
After being sintered 50~70min at 450~550 DEG C in Muffle furnace, cooled to room temperature is taken out.
4. the preparation method that multicomponent as described in claim 1 is co-doped with modified ti-supported lead dioxide electric pole, it is characterised in that
The detailed process of the step 3 are as follows: nitrate and acetic acid salt blend deposition liquid are prepared in a cell and are heated to 30~70 DEG C,
Then three kinds of dopants are added according to quantity, stir evenly, then by the titanium-base of the tin-antimony oxide bottom of sol-gel method preparation
It as anode and titanium plate as cathode, is individually fixed in electrolytic cell, 1~4h of the deposition that is powered.
5. the preparation method that multicomponent as described in claim 1 is co-doped with modified ti-supported lead dioxide electric pole, it is characterised in that
The oxalic acid etching liquid mass concentration is 3%~10%；The precursor liquid is prepared using ethyl alcohol, wherein containing 450~
600g/L C2H5OH, 60~100g/L Sn4+With 20~40g/L Sb3+；The nitrate and acetic acid salt blend deposit liquid
System is configured using deionized water, wherein containing 50~150g/L Pb2+, 20~100g/L Cu2+, 0.2~0.9g/L F-, 0.2~
1.0g/L Co2+/Fe2+/Zn2+/Ce3+With 0.2~1.0g/L PEG.
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Cited By (3)
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| CN111606395A (en) * | 2020-05-20 | 2020-09-01 | 重庆科技学院 | Preparation method and application of polythiophene modified metal bismuth-doped lead dioxide electrode |
| CN115626693A (en) * | 2022-12-22 | 2023-01-20 | 深圳永清水务有限责任公司北京分公司 | Lead-antimony coating titanium anode plate with intermediate layer and preparation method and application thereof |
| CN115676983A (en) * | 2022-12-29 | 2023-02-03 | 深圳永清水务有限责任公司北京分公司 | Lead-antimony coating titanium anode with cerium-doped intermediate layer and preparation method thereof |
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