CN109292918A - A kind of preparation method of DSA electrode - Google Patents
A kind of preparation method of DSA electrode Download PDFInfo
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- 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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- 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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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
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- 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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The present invention discloses a kind of preparation method of DSA electrode, is the oxide film electrode of composite material nanometer particle by the electrode prepared with sol method using composite material nanometer particle and citric acid as raw material；The degradation rate of electrode is improved using composite conducting material nanoparticle powder, is used for electrochemical treatments actual production waste water, is improved the degradation rate to toxic persistent organic pollutants；The stability of electrode is improved using the method preparation of colloidal sol, it is prepared using noble metal, material itself just has good electric conductivity and relatively stable, coating-drying-calcination process is repeated as many times, obtain certain thickness composite material nanometer particle, for coating liquid in conjunction with electrode seal, coating is not easily to fall off, effectively improves the service life of electrode.
Description
Technical field
The invention belongs to electro-catalytic oxidation technology fields, are related to a kind of preparation method of DSA electrode.
Background technique
There is electrocatalytic oxidation processing waste water redox to be easier to control, make because it is physical and chemical process
It will not lead to secondary pollution with electro-catalytic oxidation technology, and can handle toxic organic pollutant difficult to degrade in water, have good
Good application prospect.DSA electrode stability is good, electrochemical catalysis performance is high, without secondary pollution, in industries clean manufacturings such as plating
In application just constantly expand, can substitute the traditional electrodes such as lead, graphite, form new technology.And the electro catalytic activity of DSA electrode
Mostly come from the coating of metal oxides on surface, therefore the thickness of oxide coating, particle scale, porosity, crackle, crystal
Structure, surface topography etc. can all influence the performance that electrode is.
Therefore for the coating liquid of electrode, the chemistry of particle is easy to control because it is easier control nucleation using sol method
Composition, form and dimension, due to passing through solution reaction step, it is easy to mix to equal and quantitative some microelements, realize and divide
Uniform Doped in sub- level.The coating liquid of preparation can uniformly be coated in electrode surface, improve the stability of electrode, together
When allow coating liquid to be closely linked with electrode surface, coating is not easily to fall off, promoted electrode life, have good reality
Application prospect.
Summary of the invention
Present invention aims at the preparation method for proposing a kind of DSA electrode, the electrode prepared with sol method can enhance electricity
The stability and service life of pole, improve the degradation rate for toxic persistent organic pollutants.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of DSA electrode, includes the following steps:
Step a, 1:(1~3 in mass ratio) citric acid (CA) and alcohol organic solvent are weighed, it will at 60 DEG C~100 DEG C
Alcohol organic solvent and citric acid (CA) are stirred and heated to and are completely dissolved, and obtain colourless transparent solution；
1:(13~26 in mass ratio) weigh composite conducting material nanoparticle powder and alcohol organic solvent, 80 DEG C~
By composite conducting material nanoparticle powder and alcohol organic solvent 1~3h of reflux at 100 DEG C, it is then added to above-mentioned colourless
In bright solution, mixed solution is kept into 1h at 90 DEG C~110 DEG C, obtains the colloidal sol of black；
Step b, colloidal sol obtained in step a is taken to be coated on electrode holder；
Step c, by the electrode after coating at 60 DEG C~120 DEG C dry 10-20min, it is dry after electrode 350 DEG C~
10-50min is calcined at 550 DEG C；
Step d, step b and step c 5~20 times are repeated, 2h is finally calcined at 350 DEG C~650 DEG C, obtain DSA electricity
Pole.
Further, the composite conducting material nanoparticle powder is platinum ruthenium iridium, platinum ruthenium, platinoiridita, ruthenium iridium, Sb doped oxygen
Change tin or lead oxide nano particle.
Further, in stepb, colloidal sol is coated to by electricity using rotary coating, Best-Effort request, brushing or the method for spraying
On the carrier of pole.
Further, the alcohol organic solvent is ethyl alcohol, methanol, isopropanol or ethylene glycol.
Further, the electrode holder is that titanium plate, stud, special-shaped titanium, stainless steel plate, stainless steel bar or abnormity are stainless
Steel.
Further, in stepb, it on electrode holder before coating colloidal sol, is polished electrode holder, acid is handled and washed
Wash processing.
Compared with prior art, the invention has the following beneficial technical effects:
The preparation method of DSA electrode of the present invention is passed through using homemade composite material nanometer particle and citric acid as raw material
The electrode prepared with sol method, is the oxide film electrode of composite material nanometer particle.Using composite conducting material nanometer
Grain powder improves the degradation rate of electrode, is used for electrochemical treatments actual production waste water, improves to toxic difficult to degrade organic
The degradation rate of pollutant；The stability that electrode is improved using the method preparation of colloidal sol, is prepared, material itself using noble metal
Just there is good electric conductivity and relatively stable, coating-drying-calcination process is repeated as many times, and obtains certain thickness composite material
Nano particle, for coating liquid in conjunction with electrode seal, coating is not easily to fall off, effectively improves the service life of electrode.
Detailed description of the invention
Fig. 1 (a) platinum ruthenium iridium composite material nanometer mosaic electrode surface SEM photograph；
Particle SEM photograph on Fig. 1 (b) platinum ruthenium iridium composite material nanometer mosaic electrode；
The photographs of Fig. 2 platinum ruthenium iridium composite material nanometer mosaic electrode surface water droplet；
Fig. 3 platinum ruthenium iridium composite material nanometer mosaic electrode photo；
Specific embodiment
Present invention is further described in detail combined with specific embodiments below, but not as a limitation of the invention.
Embodiment 1
A, 1g ethylene glycol and 1g citric acid (CA) are stirred and heated to and are completely dissolved at 60 DEG C, obtained colorless and transparent
Solution；By 1g platinum ruthenium iridium composite material nanometer granular powder and 13g ethylene glycol reflux 3h at 80 DEG C, it is then added to above-mentioned nothing
In color clear solution, solution is kept into 1h at 90 DEG C, obtains the colloidal sol of black；
B, it using Ti electrode as carrier, needs to be polished before use, acid processing, wash；
C, the colloidal sol in electrode holder surface coating 13.81ml step a；
D, the electrode after coating is dried to 10min at 100 DEG C, electrode calcines 10min at 350 DEG C after drying；
E, c, Step d 15 times are repeated, 2h is finally calcined at 450 DEG C, obtains platinum ruthenium iridium composite material nanometer mosaic electrode.
Fig. 1 and Fig. 2 will be shown in scanning electron microscope and video contact angle analysis acquired results in embodiment 1, is observed by Fig. 1 (a)
It is more coarse to electrode surface, possess biggish surface area, and particle layer stackup rises in Fig. 1 (b), and is in porous structure, increases
Big reactivity area.Contact angle in Fig. 2 is 108 °, rough surface, and hydrophobic effect is good, and surface adsorption water is conducive to instead less
The progress answered, improves reaction rate.Fig. 3 is platinum ruthenium iridium composite material nanometer mosaic electrode photo.
Embodiment 2
A, 2g isopropanol and 1g citric acid (CA) are stirred and heated to and are completely dissolved at 70 DEG C, obtained colorless and transparent
Solution；1g platinum ruthenium composite material nanometer granular powder and 18g isopropyl alcohol reflux 2h, are then added to above-mentioned colourless at 90 DEG C
In bright solution, solution is kept into 1h at 100 DEG C, obtains the colloidal sol of black；
B, it using Ti electrode as carrier, needs to be polished before use, acid processing, wash；
C, the colloidal sol in electrode holder surface coating 25.48ml step a；
D, the electrode after coating is dried to 15min at 110 DEG C, electrode calcines 30min at 450 DEG C after drying；
E, c, Step d 18 times are repeated, 2h is finally calcined at 550 DEG C, obtains platinum ruthenium composite material nanometer mosaic electrode.
Embodiment 3
A, 3g ethyl alcohol and 1g citric acid (CA) are stirred and heated to and are completely dissolved at 85 DEG C, obtained colorless and transparent molten
Liquid；By 1g ruthenium iridium composite material nanometer granular powder and 22g alcohol reflux 3h at 100 DEG C, it is then added to above-mentioned colourless
In bright solution, solution is kept into 1h at 110 DEG C, obtains the colloidal sol of black；
B, it using Ti electrode as carrier, needs to be polished before use, acid processing, wash；
C, the colloidal sol in electrode holder surface coating 31.85ml step a；
D, the electrode after coating is dried to 10min at 110 DEG C, electrode calcines 10min at 550 DEG C after drying；
E, c, Step d 19 times are repeated, 2h is finally calcined at 650 DEG C, obtains ruthenium iridium composite material nanometer mosaic electrode.
Embodiment 4
A, 1.14g methanol and 1g citric acid are stirred and heated to and are completely dissolved at 100 DEG C, obtained colorless and transparent molten
Liquid；By 1g platinoiridita composite material nanometer granular powder and 26g methanol eddy 1h at 100 DEG C, it is then added to above-mentioned colourless
In bright solution, solution is kept into 1h at 110 DEG C, obtains the colloidal sol of black；
B, it using stainless steel electrode as carrier, needs to be polished before use, acid processing, wash；
C, the colloidal sol in electrode holder surface coating 34.57ml step a；
D, the electrode after coating is dried to 10min at 120 DEG C, electrode calcines 50min at 350 DEG C after drying；
E, c, Step d 20 times are repeated, 2h is finally calcined at 350 DEG C, obtains platinum ruthenium composite material nanometer mosaic electrode.
Embodiment 5
A, 2g methanol and 1g citric acid are stirred and heated to and are completely dissolved at 100 DEG C, obtain colorless and transparent solution；
By 1g platinoiridita composite material nanometer granular powder and 26g methanol eddy 1h at 100 DEG C, it is then added to above-mentioned colorless and transparent molten
In liquid, solution is kept into 1h at 110 DEG C, obtains the colloidal sol of black；
B, it using stainless steel electrode as carrier, needs to be polished before use, acid processing, wash；
C, the colloidal sol in electrode holder surface coating 34.57ml step a；
D, the electrode after coating is dried to 20min at 60 DEG C, electrode calcines 50min at 350 DEG C after drying；
E, c, Step d 5 times are repeated, 2h is finally calcined at 500 DEG C, obtains platinum ruthenium composite material nanometer mosaic electrode.
The homemade composite conducting material nanoparticle powder in laboratory used used in the embodiment of the present invention is platinum ruthenium
Iridium, platinum ruthenium, platinoiridita, ruthenium iridium, antimony-doped tin oxide or lead oxide nano particle, and pass through rotary coating, Best-Effort request, brushing side
Thus method, homemade composite material nanometer mosaic electrode are inferred: when using other conductive carriers, being also able to achieve of the invention
Technical effect.
Electrode used therein carrier is Ti electrode or stainless steel electrode, including titanium plate, stud, special-shaped titanium, stainless steel plate, no
Become rusty rod iron or special stainless steel electrode.
Homemade composite material nanometer mosaic electrode in the embodiment of the present invention is by rotary coating, Best-Effort request, brush
Made from the method for painting, such method belongs to the conventional application method that those skilled in the art are grasped, and is widely used in preparation electricity
Catalysis electrode, those skilled in the art can also be by other methods or approach, and the homemade composite material for obtaining same performance is received
Rice grain electrode, to realize technical effect of the invention.
Finally it should be noted that: the above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, to the greatest extent
Pipe is described the invention in detail referring to above-described embodiment, it should be understood by those ordinary skilled in the art that: still may be used
With modifications or equivalent substitutions are made to specific embodiments of the invention, and repaired without departing from any of spirit and scope of the invention
Change or equivalent replacement, should all cover in present claims range.
Claims (6)
1. a kind of preparation method of DSA electrode, it is characterised in that include the following steps:
Step a, 1:(1~3 in mass ratio) citric acid (CA) and alcohol organic solvent are weighed, by alcohols at 60 DEG C~100 DEG C
Organic solvent and citric acid (CA) are stirred and heated to and are completely dissolved, and obtain colourless transparent solution；
1:(13~26 in mass ratio) composite conducting material nanoparticle powder and alcohol organic solvent are weighed, 80 DEG C~100
By composite conducting material nanoparticle powder and alcohol organic solvent 1~3h of reflux at DEG C, it is then added to above-mentioned colorless and transparent
In solution, mixed solution is kept into 1h at 90 DEG C~110 DEG C, obtains the colloidal sol of black；
Step b, colloidal sol obtained in step a is taken to be coated on electrode holder；
Step c, 10-20min is dried at 60 DEG C~120 DEG C by the electrode after coating, the electrode after drying is 350 DEG C~550
10-50min is calcined at DEG C；
Step d, step b and step c 5~20 times are repeated, 2h is finally calcined at 350 DEG C~650 DEG C, obtain DSA electrode.
2. preparation method as described in claim 1, it is characterised in that: the composite conducting material nanoparticle powder is platinum
Ruthenium iridium, platinum ruthenium, platinoiridita, ruthenium iridium, antimony-doped tin oxide or lead oxide nano particle.
3. preparation method as described in claim 1, it is characterised in that: in stepb, using rotary coating, Best-Effort request, brush
It applies or colloidal sol is coated on electrode holder by the method for spraying.
4. preparation method as described in claim 1, it is characterised in that: the alcohol organic solvent is ethyl alcohol, methanol, isopropyl
Alcohol or ethylene glycol.
5. preparation method as described in claim 1, it is characterised in that: the electrode holder is titanium plate, stud, special-shaped titanium
Material, stainless steel plate, stainless steel bar or special stainless steel.
6. preparation method as described in claim 1, it is characterised in that: in stepb, on electrode holder before coating colloidal sol,
It is polished electrode holder, acid handles and carrying out washing treatment.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129821A (en) * | 2019-05-10 | 2019-08-16 | 上海氯碱化工股份有限公司 | Tin, Sb doped titanium-based ruthenic oxide coated electrode preparation method |
| CN111704211A (en) * | 2020-06-26 | 2020-09-25 | 陕西科技大学 | Preparation method of platinum ruthenium titanium yttrium DSA electrode |
| CN111704210A (en) * | 2020-06-26 | 2020-09-25 | 陕西科技大学 | Preparation method of quaternary DSA electrode |
| CN112607831A (en) * | 2020-12-17 | 2021-04-06 | 江苏羟源环能科技有限公司 | Active element uniformly-doped thin film electrode and preparation method thereof |
| CN113023834A (en) * | 2021-03-08 | 2021-06-25 | 北京石油化工学院 | Preparation method of composite electrode and method for disinfecting medical sewage by using anodic oxidation |
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| CN1896320A (en) * | 2006-06-19 | 2007-01-17 | 哈尔滨工业大学 | Rare-earth doped titanium-base SnO2 electrolytic electrode and its preparation |
| CN105200452A (en) * | 2015-11-02 | 2015-12-30 | 扬州大学 | Preparation method of Ti-matrix insoluble anode |
| CN105454741A (en) * | 2014-09-10 | 2016-04-06 | 谭燕 | Electrode as well as preparation method and application thereof |
| CN106745557A (en) * | 2017-03-13 | 2017-05-31 | 盐城工学院 | A kind of titanium-based tin iridium oxide electrode and preparation method thereof |
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| CN1896320A (en) * | 2006-06-19 | 2007-01-17 | 哈尔滨工业大学 | Rare-earth doped titanium-base SnO2 electrolytic electrode and its preparation |
| CN105454741A (en) * | 2014-09-10 | 2016-04-06 | 谭燕 | Electrode as well as preparation method and application thereof |
| CN105200452A (en) * | 2015-11-02 | 2015-12-30 | 扬州大学 | Preparation method of Ti-matrix insoluble anode |
| CN106745557A (en) * | 2017-03-13 | 2017-05-31 | 盐城工学院 | A kind of titanium-based tin iridium oxide electrode and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129821A (en) * | 2019-05-10 | 2019-08-16 | 上海氯碱化工股份有限公司 | Tin, Sb doped titanium-based ruthenic oxide coated electrode preparation method |
| CN111704211A (en) * | 2020-06-26 | 2020-09-25 | 陕西科技大学 | Preparation method of platinum ruthenium titanium yttrium DSA electrode |
| CN111704210A (en) * | 2020-06-26 | 2020-09-25 | 陕西科技大学 | Preparation method of quaternary DSA electrode |
| CN112607831A (en) * | 2020-12-17 | 2021-04-06 | 江苏羟源环能科技有限公司 | Active element uniformly-doped thin film electrode and preparation method thereof |
| CN112607831B (en) * | 2020-12-17 | 2022-12-23 | 江苏羟源环能科技有限公司 | Active element uniformly-doped thin film electrode and preparation method thereof |
| CN113023834A (en) * | 2021-03-08 | 2021-06-25 | 北京石油化工学院 | Preparation method of composite electrode and method for disinfecting medical sewage by using anodic oxidation |
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