CN110453244A - A kind of composite interlayer that ti-lead dioxide anode can be made to lengthen the life and its preparation and application - Google Patents
A kind of composite interlayer that ti-lead dioxide anode can be made to lengthen the life and its preparation and application 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
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- 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
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Abstract
A kind of composite interlayer that ti-lead dioxide anode can be made to lengthen the life of the present invention, expression formula are α-PbO2(Nano WC), preparation method have good conductive in addition using anode composite electrodeposition method, prepare α-PbO in the PbO alkali plating solution with " eka-platinium " nanoparticle WC particle2(Nano WC) composite interlayer.The composite interlayer can be used as ti-lead dioxide anode middle layer.α-the PbO is prepared on through the good Titanium base of oil removing and acid corroding pretreatment2(Nano WC) composite interlayer, and after after circulating water is washed and is neutralized, be put into plumbi nitras tank liquor, in α-PbO2(Nano WC) composite interlayer Anodic electro-deposition β-PbO2Active layer finally obtains Ti/ α-PbO2‑(Nano WC)/β‑PbO2The coated anode of structure.The present invention is to prepare composite interlayer using electrochemistry coelectrodeposition to become the effective ways for controllably constructing titanium-based metal oxide electrode, both the advantage of composite multifunction coating had been given full play to, firm coated electrode basis can be prepared by composite interlayer again, realizes the permanent reliable use of titanium-based metal oxide electrode.
Description
Technical field
The invention belongs to brown lead oxide dimensional stable anode preparation technical fields, in particular to a kind of that ti-supported lead dioxide electric can be made positive
The composite interlayer simple preparation method that pole is lengthened the life.
Background technique
Should at least have three conditions for the insoluble anode in electrolytic industry: high electric conductivity, preferable electro-catalysis are living
Property and good corrosion resistance.Ti-lead dioxide anode is a kind of novel insoluble petal oxide anode material, due to it
Have many characteristics, such as that oxygen evolution potential is high, oxidability is strong, corrosion resistance is good, good conductivity, can be widely used in smelting by high current
It is also widely used on the electrolytic preparation of gold, environmental protection and each type organic and inorganic matter.Although PbO2Ti electrode has numerous
Advantage, but due to β-PbO2With biggish internal stress, coating is caused crack occur, TiO is generated on matrix2, cause β-PbO2
It is easy to fall off with basal body binding force decline coating, cause the service life of electrode to shorten dramatically, seriously affects reliability in engineering
And economic benefit.Electrode is modified to solve the above problems, being concentrated mainly on two aspects at present: (1) being by addition
Interbed increases the comprehensive performances such as the combination between surface-active layer and matrix to improve the service life of electrode；It (2) is by right
Surface-active layer such as is doped at the modified stability etc. to improve electrode.It is alternative wherein in terms of middle layer preparation
Method, which has, brushes thermal decomposition, electro-deposition etc..Brushing thermal decomposition, there are organic gaseous volatilizations, can injure operator's own health and danger
Evil environment, moreover, the crystallization of pyrolysis temperature too low then metal oxide not enough influences electrode catalyst activity, and temperature is excessively high causes
The peroxidating of titanium-based material or even middle layer thermal damage and cause conductive bad.Though electro-deposition method controllability is strong, however, deposition gold
Belong to layer or α-PbO2All effect is unobvious.Using titanium silk material in-situ oxidation/nitridation, preparation process is cumbersome, and there are performance regulations
Limited drawback not easy to control.Though increasing corrosion resistance, electric conductivity using conductive noble metal middle layer, helps to improve electrode and stablize
Property, but be doomed can not engineer application for its high cost.And it is pyrolyzed, electro-deposition α-PbO2Multilayer transition layer can also play certain growth
The effect (Wang Shichuan, Chen Buming, Huang Hui, etc. material science and technique, 2018,26 (6): 89-96) in service life, but complexity is made,
Quality control difficulty increases.
Summary of the invention
In order to solve the problems, such as that durability present in Ti-based anode technology of preparing is poor and energy consumption is high, mesh of the invention
Be a kind of composite interlayer simple preparation method that ti-lead dioxide anode can be made to lengthen the life is provided, be based on composite electrodeposition
The strategy of lengthening the life for preparing high performance single middle layer, by adding good conductivity, the nanoparticle tungsten carbide of " eka-platinium " attribute
(WC) one step of codeposition of WC particles prepares single layer α-PbO2(Nano WC) composite interlayer, it is brilliant that composite particles WC plays refinement
Grain, and change α-PbO2The preferred orientation of crystal grain, co-deposition can reduce α-PbO2Tank voltage during the preparation process, WC and α-PbO2
Co-deposition improves α-PbO2The microhardness and corrosion resistance of coating improve titanium-based PbO2The usage durability of coated electrode；This hair
It is bright be prepared using electrochemistry coelectrodeposition composite interlayer become controllably construct the effective of titanium-based metal oxide electrode
Method had not only given full play to the advantage of composite multifunction coating, but also can prepare firm coated electrode by composite interlayer
The permanent reliable use of titanium-based metal oxide electrode is realized on basis.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of composite interlayer that ti-lead dioxide anode can be made to lengthen the life, expression formula are α-PbO2-(Nano WC)。
The preparation method of the composite interlayer that ti-lead dioxide anode can be made to lengthen the life, using anode composite electrodeposition
Method has good conductive in addition, prepares α-PbO in the PbO alkali plating solution with " eka-platinium " nanoparticle WC particle2-
(Nano WC) composite interlayer.
It include PbO and NaOH in the PbO alkali plating solution, after nanometer WC particle is added, under surfactant SBS dispersion
Composite electrodeposition is carried out, α-PbO is prepared2(Nano WC) composite interlayer coating.
As deposition solution is added after WC and surfactant SBS in the PbO alkali plating solution, PbO in deposition solution
Concentration is 20~30g/L, and the concentration of NaOH is 130~160g/L, and the concentration of WC is 5~20g/L, and surfactant SBS's adds
Adding concentration is 20~50mg/L.
The composite electrodeposition is that the stainless steel using pretreated titanium-base as anode, with homalographic is cathode, connection
Carrying out DC electrodeposition on constant voltage dc source, deposition thickness controls 10~50 μm, direct current deposition anodic current density 1~
3A/dm2, temperature is 40~50 DEG C, 1~3h of time, 500~1000r/min of stirring rate.Sample distilled water is taken out after the completion
It rinses well, dries up, the uniform α-PbO in surface can be obtained2(Nano WC) composite interlayer.
The composite interlayer that ti-lead dioxide anode can be made to lengthen the life can be used as ti-lead dioxide anode middle layer.
α-the PbO is prepared on through the good Titanium base of oil removing and acid corroding pretreatment2(Nano WC) composite interlayer, and
After washing and neutralized by flowing, it is put into plumbi nitras tank liquor, in α-PbO2(Nano WC) composite interlayer Anodic
Electro-deposition β-PbO2Active layer finally obtains Ti/ α-PbO2-(Nano WC)/β-PbO2The coated anode of structure.
The pretreatment of the Titanium base includes that cutting polishing, oil removing alkali cleaning and oxalic acid etch three links, titanium plate after processing
Surface forms rough pitted skin layer, and gray loses metallic luster, obtains the clean surface without greasy dirt and oxide skin.
The neutralization is carried out in the nitric acid solution of mass concentration 20%.
Anodic electrodeposition β-the PbO2When active layer, with Ti/ α-PbO2(Nano WC) is used as anode, two pieces of homalographics
Stainless steel plate be cathode, be placed in (the NO of Pb containing main salt3)2, pH adjusting agent HNO3And in the mixed solution of other auxiliary additives into
The preparation of row electroxidation, clean to prepared anode distilled water flushing later, cold wind drying, obtain surface compact, uniformly, it is steady
Qualitative and active good Ti/ α-PbO2-(Nano WC)/β-PbO2Dimensional stable anode material.
Wherein Pb (NO3)2Solution concentration is 0.4~0.6mol/L, passes through pH adjusting agent HNO3Dosage control anodic deposition
The pH value 2~4 of solution, addition ionic liquid 1- ethyl -3- methyl-imidazoles tetrafluoroborate be additive, additional amount be 5~
50mg/L。
Anodic electrodeposition β-the PbO2The electrodeposition temperature of active layer be 30~50 DEG C, electrodeposition time be 30~
300min, current density are 10~20mA/cm2。
Compared with prior art, the present invention prepares simple single layer α-using one step of composite electrodeposition technique on Titanium base
PbO2(Nano WC) composite interlayer, then prepares Ti/ α-PbO using anodizing technology2-(Nano WC)/PbO2Sun
Pole.The middle layer for introducing " eka-platinium " Nanocomposites can realize that firm connection, densification is anti-corrosion, and composite conductive is good, and imparting is urged
Change performance, achieve the purpose that electrode is lengthened the life, the preparation of this method is simple, controllable, and avoids the quality of multilayer transition layer preparation
It controls risk.Composite electrodeposition prepares α-PbO2(Nano WC) composite interlayer, which is simplified, prepares the numerous of intermediate with brushing method
Circlet section reduces cost using precious metal as intermediate, and composite electrodeposition technological operation is convenient, controllability is strong.With phase
The Ti/PbO of middle layer preparation is not added under the conditions of2Dimensional stable anode is compared, Ti/ α-PbO2-(Nano WC)/PbO2Dimensional stable anode
Crystallization is thinner, crystallization degree is more preferable, electro catalytic activity is higher, the service life is longer, electrocatalytic oxidation organic wastewater and etc. answer
It can be reduced with middle institute's power consumption.
Detailed description of the invention
Fig. 1 is α-PbO2(Nano WC) composite interlayer pattern.
Fig. 2 is α-PbO2(Nano WC) composite interlayer power spectrum.
Fig. 3 is Different electrodes in 1MH2SO4Middle accelerated aging contrast schematic diagram.
Fig. 4 is Ti/ α-PbO2-(Nano WC)/PbO2Surface topography.
Specific embodiment
The embodiment that the present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment 1
It uses the titanium plate Jing Guo polishing, alkali cleaning, pickling for matrix first, is prepared using one step of electrochemical co-deposition technology
Single layer α-PbO2(Nano WC) composite interlayer, then again with α-PbO2(Nano WC) electrode material is anode, and homalographic is big
Small stainless steel is cathode, and anodic oxidation prepares β-PbO2Active layer, to obtain Ti/ α-PbO2-(Nano WC)/PbO2
Dimensional stable anode.α-PbO2(Nano WC) composite interlayer preparation technology parameter: deposition solution PbO:25g/L, NaOH:150/
L, WC:10g/L, the concentration of surfactant SBS are 30mg/L, and deposition thickness controls 40 μm, direct current deposition anodic current density:
1A/dm2, time 1h, stirring rate 800r/min, electrodeposition temperature is 50 DEG C, and electrodeposition time 1h takes out sample after the completion
Clean with 20% nitric acid neutralising flush, the uniform α-PbO in surface can be obtained in drying2(Nano WC) composite interlayer electrode
Sample.β-PbO2Active layer anodic electrodeposition condition is as follows: Pb (NO3)2: 0.45mol/L, HNO31.4mL/L, pH value 2.4,
It is 1- ethyl -3- methyl-imidazoles tetrafluoroborate as additive using ionic liquid, concentration 30mg/L；Electrodeposition temperature is
40 ± 5 DEG C, electrodeposition time 60min, current density 10mA/cm2.By the Ti/ α-PbO of preparation2-(Nano WC)/PbO2
Electrode distilled water flushing is clean, and cold wind drying obtains surface compact, uniform dimensional stable anode.With Ti/PbO2Dimensional stable anode phase
Than Ti/ α-PbO2-(Nano WC)/PbO2β-the PbO of electrode surface2Preferably, homogeneous grain size, surface causes for active layer crystallization
It is close more smooth, no packing phenomenon.To Ti/ α-PbO2-(Nano WC)/PbO2Electrode carries out showing morphology characterization (Fig. 4), to α-
PbO2The composite interlayer surface (Nano WC) carries out XRD analysis (Fig. 2), electrode accelerated aging comparative test (Fig. 3).It can see
Out, Ti/ α-PbO2-(Nano WC)/PbO2The accelerated test service life of electrode is 41h, is without middle layer Ti/PbO2Electrode
2.1 times, it is seen that the Ti base PbO for not adding intermediate is substantially better than using electrode life prepared by the method for the invention2Anode.
Embodiment 2
It uses the titanium plate Jing Guo polishing, alkali cleaning, pickling for matrix, single layer α-is prepared using one step of composite electrodeposition technique
PbO2(Nano WC) composite interlayer, then again with α-PbO2(Nano WC) is anode, and the stainless steel of homalographic size is yin
Pole, anodic oxidation prepare β-PbO2Active layer, to obtain Ti/ α-PbO2-(Nano WC)/PbO2Dimensional stable anode.To system
Standby composite interlayer carries out SEM, EDX characterization (Fig. 1,2).Show that WC is compound into α-PbO2In middle layer, by scanning electron microscope (SEM) photograph
It can be seen that after the compound particle into WC, obtained α-PbO2(Nano WC) composite interlayer is more fine and close.
To sum up, it is anti-corrosion, conductive to prepare single layer using anode electrochemical co-deposition one-step method that the invention discloses a kind of
α-PbO2Composite interlayer realizes the method that ti-lead dioxide anode is lengthened the life.It is by through oil removing and acid corroding pretreatment
Titanium base surface α-PbO is prepared by electrochemical co-deposition2Composite interlayer, in anodic electrodeposition β-PbO thereon again2Activity
Layer, to obtain Ti/ α-PbO2-(Nano WC)/PbO2Coated anode.Wherein α-the PbO of introduced preparation2(Nano WC) is multiple
Closing middle layer is using nanometer tungsten carbide (WC) particle for adding " eka-platinium " attribute in alkaline PbO plating solution, to eliminate simple α-
PbO2Though middle layer α-PbO2Crystal grain is thin, stability is good, and but electro-chemical activity is low, electric conductivity and corrosion resistance are poor, to significantly improve
α-PbO2Coated conductive assigns its electro catalytic activity, reduces matrix and coating internal stress, enhances surface layer β-PbO2Active layer
Firmness in conjunction with electrode Titanium base mitigates the generation of electrodeposition distortion in coating, and composite interlayer dense uniform plays good
The effects of barrier protection got well, to significantly extend the anode usage service life.The preparation of this one step of process, it is easy to be easy
Control.In addition, significantly improving the electric conductivity with middle layer titanium substrate since nanometer WC particle is compound makes active β-PbO2Electrification
The tank voltage for learning deposition preparation process significantly reduces, and decreases production energy consumption.
Single layer is prepared using anode electrochemical co-deposition one-step method to a kind of provided by present invention implementation above
Anti-corrosion, conductive α-PbO2The method that composite interlayer realizes that ti-lead dioxide anode is lengthened the life is described in detail, Wen Zhong
Applying specific embodiment, principle and implementation of the present invention are described, and the explanation of above example is only intended to sides
Assistant solves method and its core concept of the invention；And for those of ordinary skill in the art, according to the thought of the present invention, In
Specific reality range apply mode and application it is upper there will be changes, therefore the content of the present specification should not be construed as to limit of the invention
System.
Claims (10)
1. a kind of composite interlayer that ti-lead dioxide anode can be made to lengthen the life, which is characterized in that its expression formula is α-PbO2-
(Nano WC)。
2. a kind of preparation method for the composite interlayer that ti-lead dioxide anode can be made to lengthen the life described in claim 1, feature
It is, α-PbO is prepared in the PbO alkali plating solution for being added to nanometer WC particle using anode composite electrodeposition method2-
(Nano WC) composite interlayer.
3. the preparation method for the composite interlayer that ti-lead dioxide anode can be made to lengthen the life according to claim 2, feature
Be, in the PbO alkali plating solution include PbO and NaOH, be added nanometer WC particle after, surfactant SBS dispersion under into
Row composite electrodeposition prepares α-PbO2(Nano WC) composite interlayer coating.
4. the preparation method for the composite interlayer that ti-lead dioxide anode can be made to lengthen the life according to claim 3, feature
It is, as deposition solution is added after WC and surfactant SBS in the PbO alkali plating solution, the concentration of PbO in deposition solution
For 20~30g/L, the concentration of NaOH is 130~160g/L, and the concentration of WC is 5~20g/L, and the concentration of surfactant SBS is
20~50mg/L.
5. special according to the preparation method of the composite interlayer that ti-lead dioxide anode can be made to lengthen the life of claim 3 or 4
Sign is that the deposition thickness of the composite electrodeposition controls 20~50 μm, 1~3A/dm of direct current deposition anodic current density2, temperature
Degree is 40~50 DEG C, 1~3h of time, 500~1000r/min of stirring rate.
6. the composite interlayer that ti-lead dioxide anode can be made to lengthen the life described in claim 1 is used as in ti-lead dioxide anode
The application of interbed.
7. applying according to claim 6, which is characterized in that prepare institute on through the good Titanium base of oil removing and acid corroding pretreatment
State α-PbO2(Nano WC) composite interlayer, and after after circulating water is washed and is neutralized, be put into plumbi nitras tank liquor, in α-
PbO2(Nano WC) composite interlayer Anodic electro-deposition β-PbO2Active layer finally obtains Ti/ α-PbO2-(Nano WC)/
β-PbO2The coated anode of structure.
8. applying according to claim 7, which is characterized in that it is described neutralization be in the nitric acid solution of mass concentration 20% into
Row.
9. applying according to claim 7, which is characterized in that the anodic electrodeposition β-PbO2Pb (NO when active layer3)2It is molten
Liquid concentration is 0.4~0.6mol/L, passes through pH adjusting agent HNO3Dosage control anodic deposition solution pH value 2~4, with ion
Liquid 1- ethyl -3- methyl-imidazoles tetrafluoroborate is additive, and addition concentration is 5~50mg/L.
10. applying according to claim 9, which is characterized in that the anodic electrodeposition β-PbO2The electrodeposition temperature of active layer
It is 30~50 DEG C, electrodeposition time is 30~300min, and current density is 10~20mA/cm2。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111607805A (en) * | 2020-06-27 | 2020-09-01 | 赵玉平 | Long-life anode material |
| CN111910189A (en) * | 2020-07-14 | 2020-11-10 | 广东省稀有金属研究所 | Method for removing dirt on surface of noble metal oxide electrode |
| CN112830554A (en) * | 2020-12-29 | 2021-05-25 | 西安赛尔电子材料科技有限公司 | Titanium-based composite PbO for water treatment2Method for preparing anode |
| CN113293411A (en) * | 2021-05-24 | 2021-08-24 | 昆明理工大学 | Gradient composite lead dioxide anode plate and preparation method and application thereof |
| CN113862759A (en) * | 2021-10-29 | 2021-12-31 | 昆明理工大学 | Titanium-based gradient lead dioxide composite electrode material for copper electrodeposition and preparation method thereof |
| CN114133003A (en) * | 2021-12-31 | 2022-03-04 | 西安建筑科技大学 | Construction method of magnetic sandwich titanium-based composite anode |
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| CN103700813A (en) * | 2013-11-07 | 2014-04-02 | 西安建筑科技大学 | New method for preparing Ti base PbO2 dimensionally-stable anode |
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| CN111607805A (en) * | 2020-06-27 | 2020-09-01 | 赵玉平 | Long-life anode material |
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| CN112830554A (en) * | 2020-12-29 | 2021-05-25 | 西安赛尔电子材料科技有限公司 | Titanium-based composite PbO for water treatment2Method for preparing anode |
| CN113293411A (en) * | 2021-05-24 | 2021-08-24 | 昆明理工大学 | Gradient composite lead dioxide anode plate and preparation method and application thereof |
| CN113862759A (en) * | 2021-10-29 | 2021-12-31 | 昆明理工大学 | Titanium-based gradient lead dioxide composite electrode material for copper electrodeposition and preparation method thereof |
| CN114133003A (en) * | 2021-12-31 | 2022-03-04 | 西安建筑科技大学 | Construction method of magnetic sandwich titanium-based composite anode |
| CN114133003B (en) * | 2021-12-31 | 2022-11-11 | 西安建筑科技大学 | Construction method of magnetic sandwich titanium-based composite anode |
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