CN104030403A - Preparation method of porous nanocrystal Ti/SnO2-Sn/Ce-PbO2 electrode - Google Patents
Preparation method of porous nanocrystal Ti/SnO2-Sn/Ce-PbO2 electrode Download PDFInfo
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- CN104030403A CN104030403A CN201410279964.4A CN201410279964A CN104030403A CN 104030403 A CN104030403 A CN 104030403A CN 201410279964 A CN201410279964 A CN 201410279964A CN 104030403 A CN104030403 A CN 104030403A
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Abstract
The invention discloses a preparation method of a porous nanocrystal Ti/SnO2-Sn/Ce-PbO2 electrode, and belongs to the technical field of electrochemistry. The preparation method comprises the steps of electrolyzing and oxidizing perfluoro caprylic acid-containing wastewater by taking the porous nanocrystal Ti/SnO2-Sn/Ce-PbO2 electrode as an anode and taking Ti or taking 304 stainless steel as a cathode. The preparation method is characterized in that perfluoro caprylic acid can be efficiently mineralized under a gentle condition. The preparation method disclosed by the invention adopts an electrochemical oxidizing method, is simple in process flow, convenient to operate, gentle in reaction condition, good in treatment effect, stable and reliable, and easy to realize industrial application. The adopted porous nanocrystal Ti/SnO2-Sn/Ce-PbO2 electrode has the advantages of strong oxidizing capacity, long service life and the like, and is easy to process and cheap.
Description
The present invention's denomination of invention that to be applicant submit on July 17th, 2012 is the divisional application of preparation method and the application thereof of brilliant electrode " a kind of porous receive ", the application number application that is 201210172442.5.
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to a kind of porous and receive the preparation method of brilliant electrode.
Background technology
Perfluorocaprylic Acid (PFOA, C
7f
15cOOH), as tensio-active agent, stain control agent, additive, fire foam, macromolecule emulsifier and agrochemical, its production and use have exceeded 50 years.Perfluorocaprylic Acid is one of main home to return in environment as perfluorochemical (PFCs), its stable chemical property, characteristic not volatile and that can not be degraded by the ecosystem are extensively present in natural water, settling, animal and human body it, and ecotope and HUMAN HEALTH in serious threat.At present, global Perfluorocaprylic Acid pollutes and the impact of HUMAN HEALTH has been caused to showing great attention to of national governments and scientific circles, in June, 2000 EPA (USEPA) starts the harm of noticing that Perfluorocaprylic Acid is possible, proposing low-level Perfluorocaprylic Acid and salt thereof exposes and may be harmful to HUMAN HEALTH, Perfluorocaprylic Acid can residue in human body for a long time, therefore according to " U.S.'s TSCA ", Perfluorocaprylic Acid was listed in forbidding chemical directoryof in 2003, on December 30th, 2009, USEPA has issued first " chemical action plan ", health and environmental problem that long-chain perfluorochemical to including Perfluorocaprylic Acid is caused are processed.In addition, European Union combine in European Parliament and council of ministers on December 27th, 2006 and issued " about restriction Perfluorooctane sulfonates sell and the finger that uses with ", suspect that Perfluorocaprylic Acid and salt thereof also exist the risk level that is similar to Perfluorooctane sulfonates, and promise to undertake and the discharge of Perfluorocaprylic Acid and the content in product thereof were reduced to 95% in 2010, by 2015, it is eliminated completely.
At present, the existing relevant domestic patent for Perfluorocaprylic Acid degradation technique in water body is recorded only 1, number of patent application is 200510011126.X (Granted publication CN100347137C), name is called " a kind of method of defluorinating and degrading complete fluorine substituted compounds ", disclose a kind of under 185nm and 172nm ultraviolet condition the degradation method of photodissociation and photocatalytic degradation Perfluorocaprylic Acid or perfluoro octane sulfonate.
So far, there is no and adopt electrochemistry Perfluorocaprylic Acid in water to be carried out to the report of efficient mineralising purification techniques.
Summary of the invention
The object of the invention is to prevent and treat the environmental pollution of Perfluorocaprylic Acid, for the deficiencies in the prior art, provide a kind of can be under mild conditions to water in Perfluorocaprylic Acid carry out the new type purification technology of efficient mineralising.
The object of the present invention is achieved like this, the invention provides a kind of porous and receive brilliant Ti/SnO
2-Sn/Ce-PbO
2the preparation method of electrode, it is characterized in that, comprise the following steps: Ti substrate pretreated, to the capable polishing of Ti matrix, remove oxide on surface with 200 order sand paper, then immerse 1h in 8% the sodium hydroxide solution of 100 DEG C, to remove surperficial greasy dirt, after taking-up, clean with distilled water, etching 2.5h in 100 DEG C of oxalic acid solutions of 10% afterwards, to obtain grey even curface; The polymerization forerunner colloidal sol preparation of tin antimony: at 60 DEG C of temperature, a certain amount of citric acid is dissolved in ethylene glycol, after dissolving completely, steady temperature 30min, with fully esterified, is then heated to 90 DEG C, adds SnCl
45H
2o and SbCl
3, fully stir until complete dissolving, be warming up to afterwards 100 DEG C and constant temperature 1～3h, after naturally cooling, obtain the polymeric precursor colloidal sol of tin-antimony, wherein ethylene glycol: citric acid: SnCl
45H
2o: SbCl
3mol ratio be 120: 30: 9: 1; Ti/SnO
2-Sb electrode preparation: adopt and draw formulation that the polymeric precursor colloidal sol of the tin-antimony of preparation is overlayed on Ti matrix, in the baking oven of 140 DEG C, keep afterwards 15min to make colloidal sol transfer gel to, then proceed in 500 DEG C of retort furnaces roasting 15min in air atmosphere, after taking out naturally cooling cleaning, drying, repeat again front process, 20 times repeatedly, when last roasting, 2h annealing naturally, make Ti/SnO
2-Sb electrode; Porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode preparation: the electrodeposit liquid of preparation 0.5mol/L lead nitrate, 0.001mol/L cerous nitrate and 0.5g/L Sodium Fluoride composition, and with nitre acid for adjusting pH value to 1.4, with Ti/SnO
2-Sb electrode, as base electrode, taking Ti as negative electrode, is 200A/m at electric current
2under carry out galvanic deposit 20min and prepare porous and receive brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode.
In addition, the invention provides a kind of porous and receive brilliant Ti/SnO
2-Sn/Ce-PbO
2the preparation method of electrode, comprises the following steps:
1. Ti substrate pretreated: be first that Ti matrix sand paper is polished, remove oxide on surface, then immerse 1～2h in 5%～10% the sodium hydroxide solution of 100 DEG C, to remove surperficial greasy dirt, taking-up is cleaned with distilled water, etching 2～3h in 100 DEG C of oxalic acid solutions of 10%～15% afterwards, to obtain grey even curface;
2. the polymerization forerunner colloidal sol of tin antimony preparation: at 50～70 DEG C of temperature, a certain amount of citric acid is dissolved in to (citric acid and ethylene glycol mol ratio are 1:4～6) in ethylene glycol, after dissolving completely, steady temperature 30～60min, with fully esterified, is then heated to 90 DEG C, adds SnCl
45H
2o and SbCl
3(citric acid and SnCl
45H
2o mol ratio is 1:0.05～0.1; SnCl
45H
2o and SbCl
3mol ratio is 1:0.1～0.2), fully stir until complete dissolving, be warming up to afterwards 100 DEG C and constant temperature 1～3h, after naturally cooling, obtain the polymeric precursor colloidal sol of tin-antimony;
3. Ti/SnO
2-sb electrode preparation: adopt and draw formulation that the polymeric precursor colloidal sol of the tin-antimony of preparation is overlayed on Ti matrix, in the baking oven of 120～160 DEG C, keep afterwards 10～20min to make colloidal sol transfer gel to, then proceed in 450～550 DEG C of retort furnaces roasting 10～30min in air atmosphere, after taking out naturally cooling cleaning, drying, repeat again front process, 20～40 times repeatedly, when last roasting, 1～3h annealing naturally, make Ti/SnO
2-Sb electrode;
4. porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode preparation: first prepare electrodeposit liquid, composition 0.5mol/L lead nitrate, 0.001mol/L cerous nitrate and 0.2～1.0g/L Sodium Fluoride, and with nitre acid for adjusting pH value to 1.2～1.8, with Ti/SnO
2-Sb electrode, as base electrode, taking Ti as negative electrode, is 100～200A/m at electric current
2under carry out galvanic deposit 10～30min and prepare porous and receive brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode.
In addition Perfluorocaprylic Acid technical scheme in electrochemical oxidation mineralized water: preparation is containing the solution of 5～1000mg/L Perfluorocaprylic Acid taking 1.0～2.0g/L sodium perchlorate as supporting electrolyte.Porous with preparation is received brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode is anode, and taking Ti or 304 stainless steels as negative electrode, at room temperature carrying out the processing of electrochemical oxidation mineralising containing Perfluorocaprylic Acid waste water, actuating current is 5～40mA/cm
2, polar plate spacing is 5～20mm.
As seen from the above technical solution provided by the invention, the method for the efficient mineralising of Perfluorocaprylic Acid in water provided by the invention, owing to adopting electrochemical oxidation process, there is technical process simple, easy to operate, reaction conditions gentleness, treatment effect is good and reliable and stable, is easy to realize industrial applications.The porous adopting is received brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode has that oxidation capacity is strong, work-ing life is strong, be easy to processing and the advantage such as cheap.
Brief description of the drawings
Fig. 1 is that porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode surface pattern.
The setting drawing of Perfluorocaprylic Acid in the efficient mineralized water of electrochemical oxidation that Fig. 2 provides for the embodiment of the present invention, wherein: 1-direct supply, 2-electrolyzer, 3-terminal stud, 4-pneumatic outlet, 5-negative electrode, 6-anode.
Fig. 3 is that electrochemical oxidation is to Perfluorocaprylic Acid degraded and mineralising effect and treatment time graph of a relation.
Embodiment
Below in conjunction with accompanying drawing, the embodiment of the present invention is described in further detail.
The method of Perfluorocaprylic Acid in the efficient mineralized water of a kind of electrochemical oxidation of the present invention, its preferably embodiment comprise step:
Porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode preparation:
1. first with 200 order sand paper to the capable polishing of Ti matrix, then immerse 1h in 8% the sodium hydroxide solution of 100 DEG C, for taking out, distilled water cleans, etching 2.5h in 100 DEG C of oxalic acid solutions of 10% afterwards;
2. at 60 DEG C of temperature, a certain amount of citric acid is dissolved in ethylene glycol, steady temperature 30min after dissolving completely, is then heated to 90 DEG C, adds SnCl
45H
2o and SbCl
3, fully stir until complete dissolving, be warming up to afterwards 100 DEG C and constant temperature 1～3h, after naturally cooling, obtain the polymeric precursor colloidal sol of tin-antimony, wherein ethylene glycol: citric acid: SnCl
45H
2o:SbCl
3mol ratio be 120:30:9:1;
3. adopt and draw formulation that the polymeric precursor colloidal sol of the tin-antimony of preparation is overlayed on Ti matrix, in the baking oven of 140 DEG C, keep afterwards 15min to make colloidal sol transfer gel to, then proceed in 500 DEG C of retort furnaces roasting 15min in air atmosphere, after taking out naturally cooling cleaning, drying, repeat again front process, 20 times repeatedly, when last roasting, 2h annealing naturally, make Ti/SnO
2-Sb electrode;
4. prepare the electrodeposit liquid of 0.5mol/L lead nitrate, 0.001mol/L cerous nitrate and 0.5g/L Sodium Fluoride composition, and with nitre acid for adjusting pH value to 1.4, with Ti/SnO
2-Sb electrode, as base electrode, taking Ti as negative electrode, is 200A/m at electric current
2under carry out galvanic deposit 20min and prepare porous and receive brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode.
The porous of preparation is received brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode surface pattern as shown in Figure 1.Electrode surface becomes vesicular as can be seen from Figure 1, is conducive to pollutent and adsorbs at electrode surface; PbO
2granular size is hundreds of nanometers, is nanomorphic and surface compact, greatly increases reactive behavior point position.
Perfluorocaprylic Acid technical scheme in electrochemical oxidation mineralized water: preparation is containing the solution of 1.4g/L sodium perchlorate and 100mg/L Perfluorocaprylic Acid.Get 100mL and inject Fig. 2 electrolyzer, receive brilliant Ti/SnO with the porous of preparing
2-Sn/Ce-PbO
2electrode is anode, and taking Ti or 304 stainless steels as negative electrode, two electrode areas are 60cm
2.Adjusting polar plate spacing is 10mm, power-on to regulate electric current to keep outward current density be 10mA/cm
2, under room temperature, carrying out electrolysis treatment 90min, interval 15～30min adopts analysis.
Fig. 3 is that the present invention is to Perfluorocaprylic Acid degraded and mineralising effect and treatment time relation, after 90min processes, PFOA clearance is greater than 99.9% as shown in Figure 3, defluorinate rate approaches 90%, be equivalent to existing 13.5 fluorine of 15 fluorine contained in PFOA molecule and be shed in solution, TOC has declined 92.6% simultaneously.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.In the technical scope that any those of ordinary skill in the art disclose in the present invention, can make various amendments to the present embodiment easily, and application of principle described herein is executed and needn't be passed through creative work to other example.Therefore, the invention is not restricted to the embodiment here, do not depart from category of the present invention make improve and amendment all should be encompassed in protection scope of the present invention within.
Claims (1)
1. a porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2the preparation method of electrode, is characterized in that, comprises the following steps:
Ti substrate pretreated, with 200 order sand paper to the capable polishing of Ti matrix, remove oxide on surface, then immerse 1h in 8% the sodium hydroxide solution of 100 DEG C, to remove surperficial greasy dirt, after taking-up, clean with distilled water, etching 2.5h in 100 DEG C of oxalic acid solutions of 10% afterwards, to obtain grey even curface;
The polymerization forerunner colloidal sol preparation of tin antimony: at 60 DEG C of temperature, a certain amount of citric acid is dissolved in ethylene glycol, after dissolving completely, steady temperature 30min, with fully esterified, is then heated to 90 DEG C, adds SnCl
45H
2o and SbCl
3, fully stir until complete dissolving, be warming up to afterwards 100 DEG C and constant temperature 1～3h, after naturally cooling, obtain the polymeric precursor colloidal sol of tin-antimony, wherein ethylene glycol: citric acid: SnCl
45H
2o: SbCl
3mol ratio be 120: 30: 9: 1;
Ti/SnO
2-Sb electrode preparation: adopt and draw formulation that the polymeric precursor colloidal sol of the tin-antimony of preparation is overlayed on Ti matrix, in the baking oven of 140 DEG C, keep afterwards 15min to make colloidal sol transfer gel to, then proceed in 500 DEG C of retort furnaces roasting 15min in air atmosphere, after taking out naturally cooling cleaning, drying, repeat again front process, 20 times repeatedly, when last roasting, 2h annealing naturally, make Ti/SnO
2-Sb electrode;
Porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode preparation: the electrodeposit liquid of preparation 0.5mol/L lead nitrate, 0.001mol/L cerous nitrate and 0.5g/L Sodium Fluoride composition, and with nitre acid for adjusting pH value to 1.4, with Ti/SnO
2-Sb electrode, as base electrode, taking Ti as negative electrode, is 200A/m at electric current
2under carry out galvanic deposit 20min and prepare porous and receive brilliant Ti/SnO
2-Sn/Ce-PbO
2electrode.
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| CN201210172442.5A CN102701329B (en) | 2012-07-17 | 2012-07-17 | Preparation method of porous nanometer crystal electrodes and application of porous nanometer crystal electrodes |
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| CN201410279964.4A Expired - Fee Related CN104030403B (en) | 2012-07-17 | 2012-07-17 | Porous receives brilliant Ti/SnO 2-Sn/Ce-PbO 2the preparation method of electrode |
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| CN104556312A (en) * | 2014-12-18 | 2015-04-29 | 北京师范大学 | Method for preparing porous PbO2 electrode for deep sewage treatment |
| CN104591343A (en) * | 2014-12-18 | 2015-05-06 | 北京师范大学 | Method for preparing porous PbO2 electrode for advanced treatment of industrial organic wastewater |
| CN105954613A (en) * | 2016-04-29 | 2016-09-21 | 中国船舶重工集团公司第七二五研究所 | Titanium electrode acceleration life testing device |
| CN109772295A (en) * | 2019-03-11 | 2019-05-21 | 中南大学 | A kind of bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode, preparation method and application |
| CN112978869A (en) * | 2021-03-17 | 2021-06-18 | 东莞理工学院 | Efficient selective Ti/SnO2Preparation method and application of (E) -Sb-MI anode material |
| CN114933349A (en) * | 2022-05-16 | 2022-08-23 | 桂林电子科技大学 | Titanium-based metal oxide coating filtering membrane, preparation method and application thereof, coupling reactor and sewage treatment method |
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| CN103614712B (en) * | 2013-12-04 | 2016-05-18 | 淮南师范学院 | Sol-gel process is prepared Sb, Ce codope SnO2The method in intermediate layer |
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| CN106167290A (en) * | 2016-08-23 | 2016-11-30 | 杨梅 | A kind of rare earth Ce doping Ti/Sb SnO2the preparation method of electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010095764A (en) * | 2008-10-16 | 2010-04-30 | Japan Carlit Co Ltd:The | Electrode for electrolysis and method for producing the same |
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2012
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- 2012-07-17 CN CN201410279964.4A patent/CN104030403B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
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| 李晓乐: "掺杂Ti基二氧化铅电极的制备及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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| CN104556312A (en) * | 2014-12-18 | 2015-04-29 | 北京师范大学 | Method for preparing porous PbO2 electrode for deep sewage treatment |
| CN104591343A (en) * | 2014-12-18 | 2015-05-06 | 北京师范大学 | Method for preparing porous PbO2 electrode for advanced treatment of industrial organic wastewater |
| CN104591343B (en) * | 2014-12-18 | 2016-08-17 | 北京师范大学 | Porous PbO for organic industrial sewage advanced treating2the preparation method of electrode |
| CN105954613A (en) * | 2016-04-29 | 2016-09-21 | 中国船舶重工集团公司第七二五研究所 | Titanium electrode acceleration life testing device |
| CN109772295A (en) * | 2019-03-11 | 2019-05-21 | 中南大学 | A kind of bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode, preparation method and application |
| CN112978869A (en) * | 2021-03-17 | 2021-06-18 | 东莞理工学院 | Efficient selective Ti/SnO2Preparation method and application of (E) -Sb-MI anode material |
| CN114933349A (en) * | 2022-05-16 | 2022-08-23 | 桂林电子科技大学 | Titanium-based metal oxide coating filtering membrane, preparation method and application thereof, coupling reactor and sewage treatment method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102701329A (en) | 2012-10-03 |
| CN104030403B (en) | 2016-03-02 |
| CN102701329B (en) | 2014-08-06 |
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Granted publication date: 20160302 Termination date: 20210717 |