CN104591342B - For the Ti/Ebonex/PbO of advanced treatment of wastewater2The preparation method of electrode - Google Patents
For the Ti/Ebonex/PbO of advanced treatment of wastewater2The preparation method of electrode Download PDFInfo
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- CN104591342B CN104591342B CN201410643042.7A CN201410643042A CN104591342B CN 104591342 B CN104591342 B CN 104591342B CN 201410643042 A CN201410643042 A CN 201410643042A CN 104591342 B CN104591342 B CN 104591342B
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- ebonex
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Classifications
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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
-
- 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
Abstract
The present invention relates to a kind of Ti/Ebonex/PbO2The preparation method of electrode.The method is comprised the following steps：Ti substrate pretreated steps, Ebonex intermediate layers preparation process and Ti/Ebonex/PbO2Electrode preparation process, wherein, the Ti substrate pretreateds step carries out blasting treatment using the diamond dust of 300～500 mesh；Ebonex intermediate layers preparation process, under protective atmosphere, sub- titanium dioxide powder is prepared in the way of plasma spraying；Ti/Ebonex/PbO2Electrode preparation process, the electrode based on the Ti/Ebonex electrodes of the preparation, is obtained by electro-deposition.The Ti/Ebonex/PbO prepared by above method2Electrode has extremely excellent stability and excellent electro catalytic activity.
Description
Technical field
The present invention relates to a kind of Ti/Ebonex/PbO for advanced treatment of wastewater2The preparation method of electrode, using Ti/
Ebonex/PbO2The Ti/Ebonex/PbO that the preparation method of electrode is prepared2Electrode, using Ti/Ebonex/PbO2Electrode enters
The method of row advanced treatment of wastewater, belongs to water process electrochemical field.
Background technology
With the development of modern agriculture, the demand of agricultural chemicals gradually increases.Modern is various in style, but produces the mistake of agricultural chemicals
Journey generates substantial amounts of industrial wastewater.Agricultural chemicals waste water water quality is complicated, and which is mainly characterized by：1) pollutant levels are higher, and COD (changes
Learn oxygen demand) up to per liter of tens thousand of milligram；2) toxicity is big, except external containing agricultural chemicals and centre in waste water, also containing phenol, arsenic, mercury
Deng the material that noxious material and many biologies are difficult to degrade；3) foul smelling, it is irritant to the respiratory tract and mucous membrane of people；4) water
Matter, the water yield are unstable.Therefore, pollution of the agricultural chemicals waste water to environment is very serious.The purpose of agricultural chemicals waste water process is to reduce agricultural chemicals
Production Pollutants in Wastewater concentration, improves recovery utilization rate, makes every effort to reach innoxious, but treatment technology is not perfect.It is conventional
Method it is a lot, including biochemical process, absorption method, extraction, liquid membrane separating method and oxidizing process etc..
Electrocatalytic Oxidation can improve the biodegradability of waste water, virulent organic matter can be converted into low toxicity harmless
Material, while also have the advantages that simple to operate, reaction condition is gentle, non-secondary pollution, therefore Electrocatalytic Oxidation has very
Good application prospect.One of key problem using Electrocatalytic Oxidation degradable organic pollutant is exactly to prepare high performance electrode
Material, especially exploitation are with the strong anode material of catalysis activity height, good conductivity, stability.Research can meet industrial production
Anode material be always problem of concern.Through the discovery that studies for a long period of time, ti-supported lead dioxide electric pole chemical stability and
Conduct electricity very well, overpotential for oxygen evolution is higher, be a kind of functional, low-cost insoluble anode material.Due to Titanium
Corrosion-resistant, light weight, intensity are big, and the coefficient of thermal expansion of titanium is close to the coefficient of thermal expansion of brown lead oxide, is advantageously accounted for by temperature
The degree deposition layer that causes of change comes off problem.
One main cause of ti-supported lead dioxide electric pole failure is the nascent oxygen atoms permeating produced in electrolytic process
TiO is formed to Titanium base surface2Insulating barrier, is easily caused surface-active layer and comes off.Therefore, Titanium base and top layer active layer it
Between design one layer of intermediate layer, prevent TiO2The formation of insulating barrier, so as to increasing the stability of electrode and extending the life-span.It is middle
Layer should possess three primary conditions：1) can combine closely with Titanium base and active layer；2) resistance to strong acid corrosion and opposing are newborn
State oxygen attack；3) good electric conductivity.Precious metals pt, Pd and Ag etc. are significantly improved as the stability of intermediate layer electrode, but
Noble metal price is high, limits its industrial applications.Therefore, more there is practical application valency as intermediate layer using base metal oxide
Value, has attracted the concern of researchers.At present, many achievements are had been achieved with the research in class intermediate layer, wherein studying most extensive
For SnO2- Sb intermediate layers.SnO2With TiO2With β-PbO2Rutile-type crystallographic system is belonged to, its unit cell dimension is in TiO2With β-PbO2
Between.Therefore, with SnO2There is both sides advantage as intermediate layer：1)SnO2TiO can be reduced2With β-PbO2Between by
The internal stress for producing is mismatched in lattice；2)SnO2Easily and TiO2Solid solution is formed, so as to prevent TiO2The formation of insulating barrier.So
And, SnO2- Sb layers are mainly prepared by sol-gel technology, need roast repeatedly, and technique is loaded down with trivial details, and easily occurs uneven
Phenomenon, is unfavorable in industrial mass production.
The content of the invention
It is an object of the invention to provide a kind of Ti/Ebonex/PbO2The preparation method of electrode, the method include following step
Suddenly：Ti substrate pretreated steps, Ebonex intermediate layers preparation process and Ti/Ebonex/PbO2Electrode preparation process, its feature exist
In：
Wherein, the Ti substrate pretreateds step, is polished with sand paper to Ti matrixes, removes oxide on surface, then
1～2h in the sodium hydroxide solution of the 5%～10% of 100 DEG C of immersion, to remove the greasy dirt on surface, taking-up is cleaned with distilled water and is dried in the air
It is dry, blasting treatment is carried out using 300 mesh diamond dust afterwards；
In the preparation process of the Ebonex intermediate layers, under reproducibility or inert protective atmosphere, by sub- titanium dioxide powder with
It is prepared by the mode of plasma spraying；
The Ti/Ebonex/PbO2In electrode preparation process, 0.5molL is formulated as-1Pb(NO3)2、0.1mol·L- 1HNO3And 0.5gL-1The electrodeposit liquid of NaF compositions, the electrode based on the Ti/Ebonex electrodes of preparation are obtained by electro-deposition
Arrive.
Ti/Ebonex/PbO of the present invention2The preparation method of electrode, in the preparation process of the Ebonex intermediate layers,
Described protective atmosphere is reproducibility or inert protective atmosphere.
Ti/Ebonex/PbO of the present invention2The preparation method of electrode, in the preparation process of the Ebonex intermediate layers,
The reproducibility or inert protective atmosphere are selected from helium, nitrogen, argon gas or hydrogen.
Ti/Ebonex/PbO of the present invention2The preparation method of electrode, in the preparation process of the Ebonex intermediate layers,
The sub- titanium dioxide powder is chemical formula TinO2n-1Shown compound or with chemical formula TinO2n-1Shown compound
For the mixture of Main Ingredients and Appearance, wherein, n is selected from 3<n<The integer of 10 scopes.
Ti/Ebonex/PbO of the present invention2The preparation method of electrode, in the preparation process of the Ebonex intermediate layers,
The sub- titanium dioxide powder is Ti4O7Or Ti5O9, or, with Ti4O7Or Ti5O9For the mixture of main component.
Ti/Ebonex/PbO of the present invention2The preparation method of electrode, in the electrodeposition step, electrodeposit liquid
Fill a prescription and be：200mg L-1Pb(NO3)2；0.5mg L-1NaF；0.1mmolL-1HNO3。
Ti/Ebonex/PbO of the present invention2The preparation method of electrode, in the electrodeposition step, electro-deposition ginseng
Number is：Deposition current is 200A m-2, electrode spacing is 1～3cm.
The present invention also provides a kind of Ti/Ebonex/PbO2Electrode, prepares according to above-mentioned preparation method.
Ti/Ebonex/PbO of the present invention2Electrode, the sub- titanium oxide layer thickness are 200 μm.
The present invention further provides a kind of advanced treatment method for sewage water, using Ti/Ebonex/PbO of the present invention2Electricity
Extremely anode is electrolysed.
The present inventor Jing concentrates on studies, it is found that Ebonex intermediate layers prepared by plasma spray technology are stable, sub- oxidation
Titanium powder is stronger with the basic adhesions of Ti；The Ti/Ebonex/PbO that electrode deposition is obtained based on Ti/Ebonex electrodes2Electricity
Have good stability and excellent catalysis activity, and then, electrode life significantly improves.The electricity prepared by the present invention
Pole, chemical stability and conducts electricity very well, and overpotential for oxygen evolution is higher, is a kind of functional, low-cost insoluble anode
Material.And the coefficient of thermal expansion of titanium is close to the coefficient of thermal expansion of brown lead oxide, advantageously accounts for being sunk by the electricity that temperature change causes
Lamination comes off problem.By the preparation method of the present invention, it is not necessary to roast repeatedly, process is simple, and easily prepare it is uniform in
Interbed, can be applied to industrialized large-scale production.Meanwhile, pollutant levels in pesticide wastewater are reduced, is improved and is reclaimed
Utilization rate, reaches innoxious.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photograph of the Ti/Ebonex electrodes under different multiplying；
Fig. 2 is the accelerated aging curve of different ti-supported lead dioxide electric poles；
Fig. 3 is degradation rate of the different intermediate layer ti-supported lead dioxide electric poles to PFOS.
Specific embodiment
Below, by with reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out detailed
Description, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based on this
Embodiment in bright, the every other reality obtained on the premise of creative work is not made by those of ordinary skill in the art
Example is applied, the scope of protection of the invention is belonged to.
It should be noted that herein, term " including ", "comprising" or its any other variant are intended to non-row
His property is included, so that a series of process, method, article or equipment including key elements not only include those key elements, and
And also include other key elements being not expressly set out, or also include for this process, method, article or equipment institute inherently
Key element.
In the present invention, Fig. 1 is scanning electron microscope (SEM) photograph of the Ti/Ebonex electrodes under different multiplying；Fig. 2 is different titanium-baseds two
The accelerated aging curve of lead dioxide electrode；Fig. 3 is degradation rate of the different intermediate layer ti-supported lead dioxide electric poles to PFOS.
The present invention provides a kind of Ti/Ebonex/PbO for agricultural chemicals waste water process2The preparation method of electrode, including it is following
Step：
Ti substrate pretreateds：It is that Ti matrixes are polished with sand paper first, removes oxide on surface, be then immersed in 100
DEG C 5%～10% sodium hydroxide solution in 1～2h, to remove the greasy dirt on surface, taking-up is cleaned with distilled water and is dried, afterwards
Blasting treatment is carried out using 300 mesh diamond dust, increases the roughness of Ti matrix surfaces；
It is prepared by Ebonex intermediate layers：Under nitrogen protection atmosphere, sub- titanium dioxide powder is sprayed by using plasma flush coater
The Ti matrix surfaces Jing after blasting treatment are applied to, Ti/Ebonex base electrodes are prepared, sub- titanium oxide layer thickness is 200 μm left
It is right；
The Ti/Ebonex electrode surface patterns of preparation are as shown in Figure 1.There is certain hole knot in electrode surface as can be seen from Figure 1
Structure, with compared with Large ratio surface, this is PbO2Deposition good carrier is provided.
In the present invention, Ti/Ebonex/PbO2It is prepared by electrode：Prepare 0.5mol L-1Pb(NO3)2、0.1mol L-1HNO3
With 0.5g L-1The electrodeposit liquid of NaF compositions, using Ti/Ebonex electrodes as base electrode, with Ti as negative electrode, electrode spacing is
3cm, is 200A m in electric current-2Under carry out electro-deposition 60min and prepare Ti/Ebonex/PbO2Electrode.
In the present invention, described protective atmosphere is reproducibility or inert protective atmosphere.Be preferably selected from helium, nitrogen,
Argon gas or hydrogen.
In the present invention, the sub- titanium dioxide powder is chemical formula TinO2n-1Shown compound, wherein, n is selected from 3<n
<The integer of 10 scopes；It is preferably selected from the integer of 4≤n≤6 scope.The sub- titanium dioxide powder is Ti4O7Or Ti5O9Or with Ti4O7
Or Ti5O9For the mixture of main component.
In the present invention, PbO2Electrode electrodeposit liquid formula is：200mg L-1Pb(NO3)2；0.5mg L-1NaF；
0.1mmol L-1HNO3。
Ti/Ebonex/PbO of the present invention2The preparation method of electrode, it is characterised in that PbO2Electrode electro-deposition parameter
For：Deposition current is 200A m-2, 1～3cm of electrode spacing.
In the present invention, Ti/Ebonex/PbO is prepared using said method2Electrode, under protective atmosphere, by sub- oxygen
Change about 200 μm of the thickness in the Ebonex intermediate layers that titanium powder is prepared in the way of plasma spraying.
In the present invention, using heretofore described Ti/Ebonex/PbO2Electrode carries out electrolysis process for anode.Will
High-concentration waste water is by with Ti/Ebonex/PbO2Electrolytic cell of the electrode for anode；Persistently process under certain current density useless
Water is for a period of time.The present invention uses Ti/Ebonex/PbO2Electrolysis process pesticide producing during produce high concentration, height
Salt, difficult biochemical waste water, as a result show：Under the conditions of certain pH, current density and process time, agricultural chemicals waste water COD clearances
Reaching more than 60%, BOD/COD and more than 0.3 being increased to from less than 0.1, biodegradability is greatly improved.Using the Ti/ of the present invention
Ebonex/PbO2The high-concentration waste water biochemical degradation that the electrochemical oxidation of electrode is produced in being especially suitable for various pesticide producings it is pre-
Process.
Embodiment 1
Fig. 2 for whether there is intermediate layer ti-supported lead dioxide electric pole under the conditions of accelerating lifetime testing tank voltage with electrolysis when
Between change.Test condition is 1.0mol L-1H2SO4, current density is 0.5A cm-2, electrode spacing is 1cm.As shown in Figure 2
Sub- titania coating and traditional SnO2- Sb can significantly improve the life-span of electrode as intermediate layer.Dioxy without intermediate layer
The accelerated aging for changing lead electrode is very short, less than 10h, and increased SnO2The ti-supported lead dioxide electric electricity of-Sb and sub- titania coating
The accelerated aging of pole respectively reaches 430h and 632h.So as to substantially increase the life-span of electrode, the purpose of reinforcing life is reached.
Embodiment 2
Fig. 3 is Ti/Ebonex/PbO of the present invention2Electrode and conventional Ti/SnO2-Sb/PbO2Electrode degrading PFOS
(PFOS) design sketch.PFOS initial concentrations are 1mg L-1, support electrolysis for 10mmol L-1NaClO4, electrolytic current density is
10mA cm-2, polar plate spacing is 1cm.From the figure 3, it may be seen that traditional Ti/SnO2-Sb/PbO2Electrode effectively can not be degraded PFOS, and
Ti/Ebonex/PbO of the present invention2Electrode effectively can be degraded PFOS, process through 60min electrolysis, and the PFOS for having 78.7% is dropped
Solution.
By the Ti/Ebonex/PbO of the present invention2The preparation method of electrode, is prepared by plasma spray technology
Ebonex intermediate layers are stable, and sub- titanium dioxide powder is stronger with the basic adhesions of Ti；The electrode deposition based on Ti/Ebonex electrodes
The Ti/Ebonex/PbO for obtaining2Electrode has good stability and excellent catalysis activity, and then, electrode life significantly carries
It is high.The electrode prepared by the present invention, chemical stability and is conducted electricity very well, and overpotential for oxygen evolution is higher, be it is a kind of it is functional,
Low-cost insoluble anode material.And the coefficient of thermal expansion of titanium is close to the coefficient of thermal expansion of brown lead oxide, is advantageously accounted for
Come off problem by the deposition layer that temperature change causes.By the preparation method of the present invention, it is not necessary to roast repeatedly, technique letter
It is single, and uniform intermediate layer is easily prepared, industrialized large-scale production can be applied to.Meanwhile, reduce pesticide wastewater
Middle pollutant levels, improve recovery utilization rate, reach innoxious.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and apply the present invention.
Any those of ordinary skill in the art the invention discloses technical scope in, various repairing can be made easily to the present embodiment
Change, and principle described herein is applied to other examples and apply without through creative work.Therefore, the invention is not restricted to this
In embodiment, without departing from scope it is made improvement and modification should all be included within the scope of the present invention.
Claims (8)
1. a kind of Ti/Ebonex/PbO2The preparation method of electrode, the method are comprised the following steps：Ti substrate pretreated steps,
Ebonex intermediate layers preparation process and Ti/Ebonex/PbO2Electrode preparation process, it is characterised in that：
Wherein, the Ti substrate pretreateds step, is polished with sand paper to Ti matrixes, is removed oxide on surface, is then immersed in
1～2h in the sodium hydroxide solution of the 5%～10% of 100 DEG C, to remove the greasy dirt on surface, taking-up is cleaned with distilled water and is dried,
Blasting treatment is carried out using 300 mesh diamond dust afterwards；
In the preparation process of the Ebonex intermediate layers, under reproducibility or inert protective atmosphere, by sub- titanium dioxide powder with wait from
It is prepared by the mode of son spraying；
The Ti/Ebonex/PbO2In electrode preparation process, 0.5molL is formulated as-1Pb(NO3)2、0.1mol·L-1HNO3With
0.5g·L-1The electrodeposit liquid of NaF compositions, the electrode based on the Ti/Ebonex electrodes of preparation are obtained by electro-deposition.
2. Ti/Ebonex/PbO according to claim 12The preparation method of electrode, it is characterised in that in the Ebonex
In interbed preparation process, the reproducibility or inert protective atmosphere are selected from helium, nitrogen, argon gas or hydrogen.
3. Ti/Ebonex/PbO according to claim 12The preparation method of electrode, it is characterised in that in the Ebonex
In interbed preparation process, the sub- titanium dioxide powder is chemical formula TinO2n-1Shown compound or with chemical formula
TinO2n-1Mixture of the shown compound for Main Ingredients and Appearance, wherein, n is selected from 3<n<The integer of 10 scopes.
4. Ti/Ebonex/PbO according to claim 32The preparation method of electrode, it is characterised in that in the Ebonex
In interbed preparation process, the sub- titanium dioxide powder is Ti4O7Or Ti5O9, or, with Ti4O7Or Ti5O9For the mixed of main component
Compound.
5. Ti/Ebonex/PbO according to claim 12The preparation method of electrode, it is characterised in that in the Ti/
Ebonex/PbO2In electrode preparation process, electro-deposition parameter is：Deposition current is 200A m-2, electrode spacing is 1～3cm.
6. a kind of Ti/Ebonex/PbO2Electrode, it is characterised in that the electrode is according to any one of Claims 1 to 5
What preparation method was prepared.
7. Ti/Ebonex/PbO according to claim 62Electrode, it is characterised in that the sub- titanium oxide layer thickness is 200
μm。
8. a kind of advanced treatment method for sewage water, it is characterised in that using the Ti/Ebonex/PbO described in claim 6 or 72Electrode
It is electrolysed for anode.
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| CN105058916A (en) * | 2015-07-20 | 2015-11-18 | 昆明理工大学 | Electrode material with intermediate Ti4O7 coating |
| WO2018035474A1 (en) * | 2016-08-19 | 2018-02-22 | University Of Georgia Research Foundation, Inc. | Methods and systems for electrochemical oxidation of polyfluoroalkyl and perfluroalkyl contaminants |
| CN107190303B (en) * | 2017-03-27 | 2019-01-18 | 天能电池集团有限公司 | A kind of lead storage battery grid and preparation method thereof with composite coating |
| CN110316917A (en) * | 2019-07-01 | 2019-10-11 | 任丘市谛赛驷环保科技有限公司 | A kind of preparation method for the advanced oxidation system handling oily sludge |
| CN111003759A (en) * | 2019-12-24 | 2020-04-14 | 广东省稀有金属研究所 | Coated electrode containing titanium suboxide intermediate layer, preparation method and application thereof, and electrochemical water treatment equipment |
| CN111170415B (en) * | 2020-01-08 | 2020-10-09 | 江苏省环境科学研究院 | Titanium oxide/ruthenium oxide composite electrode and preparation method and application thereof |
| CN111186883B (en) * | 2020-01-09 | 2021-08-24 | 青岛理工大学 | Novel preparation technology of lead dioxide electrode modified by titanium tetroxide nanotube |
| CN112250145B (en) * | 2020-10-30 | 2021-11-30 | 南京理工大学 | Preparation and application of porous titanium-based titanium suboxide nanotube lead dioxide electrode |
| CN113149156A (en) * | 2021-06-07 | 2021-07-23 | 陕西科技大学 | Preparation method of titanium suboxide DSA anode |
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