CN102701329A - Preparation method of porous nanometer crystal electrodes and application of porous nanometer crystal electrodes - Google Patents
Preparation method of porous nanometer crystal electrodes and application of porous nanometer crystal electrodes Download PDFInfo
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- CN102701329A CN102701329A CN2012101724425A CN201210172442A CN102701329A CN 102701329 A CN102701329 A CN 102701329A CN 2012101724425 A CN2012101724425 A CN 2012101724425A CN 201210172442 A CN201210172442 A CN 201210172442A CN 102701329 A CN102701329 A CN 102701329A
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Abstract
The invention discloses a preparation method of porous nanometer crystal Ti/SnO2-Sn/Ce-PbO2 electrodes and a method for using the porous nanometer crystal Ti/SnO2-Sn/Ce-PbO2 electrodes for degrading and mineralizing perfluoro caprylic acid in water, and belongs to the technical field of electrochemistry. Waste water containing perfluoro caprylic acid is subjected to electrolytic oxidation treatment by using the porous nanometer crystal Ti/SnO2-Sn/Ce-PbO2 electrodes as anodes and Ti or 304 stainless steel as cathodes. The method is characterized in that the perfluoro caprylic acid can be efficiently mineralized under the mild condition. An electrochemical oxidation method is adopted, the technical flow process is simple, the operation is convenient, the reaction condition is mild, the treatment effect is good, in addition, stability and reliability are realized, and the industrial application is easy to realize. The adopted porous nanometer crystal Ti/SnO2-Sn/Ce-PbO2 electrodes have the advantages that the oxidation capacity is high, the service life is long, the processing is easy, the cost is low, and the like.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to a kind of porous and receive the method for Perfluorocaprylic Acid in preparation method and the efficient mineralized water of electrochemical oxidation of brilliant electrode.
Background technology
(PFOA, C7F15COOH) as tensio-active agent, stain control agent, additive, fire foam, macromolecule emulsifier and agrochemical, its production and use are above 50 years for Perfluorocaprylic Acid.Perfluorocaprylic Acid is as one of perfluorochemical (PFCs) main home to return in environment; Its stable chemical property, not volatile and can not it extensively is present in natural water, settling, animal and the human body by the characteristic of ecosystem degraded, ecotope and HUMAN HEALTH in serious threat.At present; Global Perfluorocaprylic Acid pollutes and health effects has been caused showing great attention to of national governments and scientific circles, and in June, 2000 EPA (USEPA) begins the harm of noticing that Perfluorocaprylic Acid is possible, proposes low-level Perfluorocaprylic Acid and salt thereof and exposes and possibly be harmful to HUMAN HEALTH; Perfluorocaprylic Acid can residue in the human body for a long time; Therefore according to " U.S.'s TSCA ", Perfluorocaprylic Acid was listed in forbidding chemical directoryof, on December 30th, 2009 in 2003; USEPA has issued first " chemical action plan ", and the health and the environmental problem that will cause the long-chain perfluorochemical that comprises Perfluorocaprylic Acid are handled.In addition; European Union on December 27th, 2006 unite in European Parliament and council of ministers and issued " about the restriction PFOS sell and the finger that uses with "; Suspect that also there are the risk level that is similar to PFOS in Perfluorocaprylic Acid and salt thereof; And promise to undertake 2010 with the discharging of Perfluorocaprylic Acid and the minimizing of the content in product 95% thereof, by 2015 it is eliminated fully.
At present; Existing relevant domestic patent to Perfluorocaprylic Acid degradation technique in the water body is put down in writing only 1; Number of patent application is 200510011126.X (Granted publication CN 100347137C); 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, still there is not employing electrochemistry is carried out efficient mineralising purification techniques to Perfluorocaprylic Acid in the water report.
Summary of the invention
The object of the invention is to prevent and treat the environmental pollution of Perfluorocaprylic Acid, to the deficiency of 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 objective of the invention is to realize like this, a kind of porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2The preparation method of electrode may further comprise the steps:
1. Ti substrate pretreated: at first be that the Ti matrix is polished with sand paper; Remove oxide on surface; Immerse 1～2h in 100 ℃ 5%～10% the sodium hydroxide solution then,, take out and clean with zero(ppm) water to remove the greasy dirt on surface; Etching 2～3h in 100 ℃ of oxalic acid solutions of 10%～15% afterwards is to obtain the grey even curface;
2. the polymerization forerunner colloidal sol of tin antimony preparation: under 50～70 ℃ of temperature; A certain amount of Hydrocerol A is dissolved in (Hydrocerol A and terepthaloyl moietie mol ratio are 1: 4～6) in the terepthaloyl moietie, and dissolving back steady temperature 30～60min is with abundant fatization fully; Be heated to 90 ℃ then, add SnCl
45H
2O and SbCl
3(Hydrocerol A and SnCl
45H
2The O mol ratio is 1: 0.05～0.1; SnCl
45H
2O and SbCl
3Mol ratio is 1: 0.1～0.2), fully stir until accomplishing dissolving, be warming up to 100 ℃ and constant temperature 1～3h afterwards, promptly obtain the polymeric precursor colloidal sol of stanniferous antimony behind the naturally cooling;
3. Ti/SnO
2-Sb electrode preparation: adopt and draw formulation that the polymeric precursor colloidal sol of the stanniferous antimony of preparation is overlayed on the Ti matrix; In 120～160 ℃ baking oven, keep 10～20min to make colloidal sol transfer gel to afterwards; Change in 450～550 ℃ of retort furnaces roasting 10～30min in air atmosphere then over to, repeat preceding process again, 20～40 times repeatedly after taking out the naturally cooling cleaning, drying; 1～3h and annealing naturally promptly make Ti/SnO during roasting for the last time
2-Sb electrode;
4. porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2Electrode preparation: at first prepare electrodeposit liquid, form 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 is negative electrode as base electrode with Ti, is 100～200A/m at electric current
2Under carry out galvanic deposit 10～30min and promptly prepare porous and receive brilliant Ti/SnO
2-Sn/Ce-PbO
2Electrode.
Perfluorocaprylic Acid technical scheme in the electrochemical oxidation mineralized water: with 1.0～2.0g/L sodium perchlorate is the solution that the supporting electrolyte preparation contains 5～1000mg/L Perfluorocaprylic Acid.Porous with preparation is received brilliant Ti/SnO
2-Sn/Ce-PbO
2Electrode is an anode, is that negative electrode at room temperature carries out the processing of electrochemical oxidation mineralising to containing Perfluorocaprylic Acid waste water with Ti or 304 stainless steels, and actuating current is 5～40mA/cm
2, polar plate spacing is 5～20mm.
Technical scheme by the invention described above provides can be found out, the method for the efficient mineralising of Perfluorocaprylic Acid in the water provided by the invention is owing to adopt electrochemical oxidation process; It is simple to have technical process, easy to operate, and reaction conditions is gentle; Treatment effect is good and reliable and stable, is easy to realize industrial applications.The porous that is adopted is received brilliant Ti/SnO
2-Sn/Ce-PbO
2Electrode has that oxidation capacity is strong, work-ing life is strong, be easy to advantages such as processing and cheapness.
Description of drawings
Fig. 1 receives brilliant Ti/SnO for porous
2-Sn/Ce-PbO
2The electrode 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 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
To combine accompanying drawing that the embodiment of the invention is done to describe in detail further below.
The method of Perfluorocaprylic Acid in the efficient mineralized water of a kind of electrochemical oxidation of the present invention, its preferable embodiment comprises step:
Porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2Electrode preparation:
1. at first with 200 order sand paper to the capable polishing of Ti matrix, immerse 1h in 100 ℃ 8% the sodium hydroxide solution then, take out with zero(ppm) water and clean, afterwards etching 2.5h in 100 ℃ of oxalic acid solutions of 10%;
2. under 60 ℃ of temperature, a certain amount of Hydrocerol A is dissolved in the terepthaloyl moietie, dissolving back steady temperature 30min is heated to 90 ℃ then fully, adds SnCl
45H
2O and SbCl
3, fully stir until accomplishing dissolving, be warming up to 100 ℃ and constant temperature 1～3h afterwards, promptly obtain the polymeric precursor colloidal sol of stanniferous antimony behind the naturally cooling, wherein terepthaloyl moietie: Hydrocerol A: SnCl
45H
2O: SbCl
3(mol ratio) is 120: 30: 9: 1;
3. adopt and draw formulation that the polymeric precursor colloidal sol of the stanniferous antimony of preparation is overlayed on the Ti matrix; In 140 ℃ baking oven, keep 15min to make colloidal sol transfer gel to afterwards; Change in 500 ℃ of retort furnaces roasting 15min in air atmosphere then over to, repeat preceding process again, 20 times repeatedly after taking out the naturally cooling cleaning, drying; 2h and annealing naturally promptly make Ti/SnO during roasting for the last time
2-Sb electrode;
4. prepare the electrodeposit liquid that 0.5mol/L lead nitrate, 0.001mol/L cerous nitrate and 0.5g/L Sodium Fluoride are formed, and with nitre acid for adjusting pH value to 1.4, with Ti/SnO
2-Sb electrode is negative electrode as base electrode with Ti, is 200A/m at electric current
2Under carry out galvanic deposit 20min and promptly 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
2The electrode surface pattern is as shown in Figure 1.Can know that from Fig. 1 electrode surface becomes vesicular, help pollutent and adsorb at electrode surface; PbO
2Particle size is hundreds of nanometers, is nanomorphic and surface compact, increases reactive behavior point position greatly.
Perfluorocaprylic Acid technical scheme in the electrochemical oxidation mineralized water: preparation contains 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 preparation
2-Sn/Ce-PbO
2Electrode is an anode, is negative electrode with Ti or 304 stainless steels, and two electrode areas are 60cm
2The adjusting polar plate spacing is 10mm, and power-on is also regulated electric current to keep outward current density be 10mA/cm
2, carrying out electrolysis treatment 90min under the room temperature, 15～30min adopts analysis at interval.
Fig. 3 degrades and mineralising effect and treatment time relation to Perfluorocaprylic Acid for the present invention; Can know that by Fig. 3 the PFOA clearance is greater than 99.9% after 90min handles; The defluorinate rate is near 90%; Existing 13.5 fluorine of 15 fluorine that are equivalent to contained in the PFOA molecule are shed in the solution, and TOC has descended 92.6% simultaneously.
Above-mentioned description to embodiment is can understand and use the present invention for ease of the those of ordinary skill of this technical field.Any those of ordinary skill in the art can make various modifications to present embodiment easily in the technical scope that the present invention discloses, and are applied to other instance to the principle in this explanation and execute and needn't pass through creative work.Therefore, the invention is not restricted to the embodiment here, do not break away from category of the present invention and make improving and revising and all should be encompassed within protection scope of the present invention.
Claims (2)
1. a porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2The preparation method of electrode is characterized in that, may further comprise the steps:
Ti substrate pretreated: at first be that the Ti matrix is polished with sand paper; Remove oxide on surface; Immerse 1～2h in 100 ℃ 5%～10% the sodium hydroxide solution then,, take out and clean with zero(ppm) water to remove the greasy dirt on surface; Etching 2～3h in 100 ℃ of oxalic acid solutions of 10%～15% afterwards is to obtain the grey even curface;
The polymerization forerunner colloidal sol preparation of tin antimony: under 50～70 ℃ of temperature; A certain amount of Hydrocerol A is dissolved in (Hydrocerol A and terepthaloyl moietie mol ratio are 1: 4～6) in the terepthaloyl moietie, and dissolving back steady temperature 30～60min is with abundant fatization fully; Be heated to 90 ℃ then, add SnCl
45H
2O and SbCl
3, Hydrocerol A and SnCl
45H
2The O mol ratio is 1: 0.05～0.1; SnCl
45H
2O and SbCl
3Mol ratio is 1: 0.1～0.2, fully stirs until accomplishing dissolving, is warming up to 100 ℃ and constant temperature 1～3h afterwards, promptly obtains the polymeric precursor colloidal sol of stanniferous antimony behind the naturally cooling;
Ti/SnO
2-Sb electrode preparation: adopt and draw formulation that the polymeric precursor colloidal sol of the stanniferous antimony of preparation is overlayed on the Ti matrix; In 120～160 ℃ baking oven, keep 10～20min to make colloidal sol transfer gel to afterwards; Change in 450～550 ℃ of retort furnaces roasting 10～30min in air atmosphere then over to, repeat preceding process again, 20～40 times repeatedly after taking out the naturally cooling cleaning, drying; 1～3h and annealing naturally promptly make Ti/SnO during roasting for the last time
2-Sb electrode;
Porous is received brilliant Ti/SnO
2-Sn/Ce-PbO
2Electrode preparation: at first prepare electrodeposit liquid, consist of 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 is negative electrode as base electrode with Ti, is 100～200A/m at electric current
2Under carry out galvanic deposit 10～30min and promptly prepare porous and receive brilliant Ti/SnO
2-Sn/Ce-PbO
2Electrode.
2. the method for Perfluorocaprylic Acid in the electrochemical oxidation degree of depth mineralized water is characterized in that, is supporting electrolyte with 1.0～2.0g/L sodium perchlorate, receives brilliant Ti/SnO with the porous of preparation in the claim 1
2-Sn/Ce-PbO
2Electrode is an anode, is that negative electrode at room temperature carries out the processing of electrochemical oxidation mineralising to containing Perfluorocaprylic Acid waste water with Ti or 304 stainless steels, and actuating current is 5～40mA/cm
2, the electrode pad spacing is 5～20mm.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210172442.5A CN102701329B (en) | 2012-07-17 | 2012-07-17 | Preparation method of porous nanometer crystal electrodes and application of porous nanometer crystal electrodes |
| CN201410279964.4A CN104030403B (en) | 2012-07-17 | 2012-07-17 | Porous receives brilliant Ti/SnO 2-Sn/Ce-PbO 2the preparation method of electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 Division 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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| CN102701329A true CN102701329A (en) | 2012-10-03 |
| CN102701329B CN102701329B (en) | 2014-08-06 |
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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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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103614712A (en) * | 2013-12-04 | 2014-03-05 | 淮南师范学院 | Method for preparing Sb and Ce co-doped SnO2 middle layer by sol-gel method |
| 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 |
| CN105600879A (en) * | 2015-12-28 | 2016-05-25 | 北京帝力伟业科技开发有限公司 | Electrocatalytic oxidation reaction device for treating toxic organic wastewater |
| CN106167290A (en) * | 2016-08-23 | 2016-11-30 | 杨梅 | A kind of rare earth Ce doping Ti/Sb SnO2the preparation method of electrode |
| CN106757248A (en) * | 2016-11-28 | 2017-05-31 | 深圳市橘井舒泉技术有限公司 | The preparation facilities and method of lead dioxide electrode |
| CN108675406A (en) * | 2018-05-16 | 2018-10-19 | 中大立信（北京）技术发展有限公司 | A kind of novel SnO2Electrode and its preparation method and application |
| CN110980890A (en) * | 2019-12-26 | 2020-04-10 | 西安泰金工业电化学技术有限公司 | Titanium-based lead dioxide electrode for degrading rhodamine B and preparation method and application thereof |
| 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 |
| CN115010222A (en) * | 2022-08-09 | 2022-09-06 | 广东工业大学 | Filtering type electrodeposition device, electrodeposition system and preparation method of DSA membrane electrode |
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| CN109772295B (en) * | 2019-03-11 | 2020-09-08 | 中南大学 | Bismuth tungstate modified antimony-doped tin dioxide composite photoelectric catalytic electrode, preparation method and application |
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- 2012-07-17 CN CN201410279964.4A patent/CN104030403B/en not_active Expired - Fee Related
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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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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103614712A (en) * | 2013-12-04 | 2014-03-05 | 淮南师范学院 | Method for preparing Sb and Ce co-doped SnO2 middle layer by sol-gel method |
| 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 |
| 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 |
| CN105600879A (en) * | 2015-12-28 | 2016-05-25 | 北京帝力伟业科技开发有限公司 | Electrocatalytic oxidation reaction device for treating toxic organic wastewater |
| CN106167290A (en) * | 2016-08-23 | 2016-11-30 | 杨梅 | A kind of rare earth Ce doping Ti/Sb SnO2the preparation method of electrode |
| CN106757248A (en) * | 2016-11-28 | 2017-05-31 | 深圳市橘井舒泉技术有限公司 | The preparation facilities and method of lead dioxide electrode |
| CN106757248B (en) * | 2016-11-28 | 2018-08-31 | 深圳市橘井舒泉技术有限公司 | The preparation facilities and method of lead dioxide electrode |
| CN108675406A (en) * | 2018-05-16 | 2018-10-19 | 中大立信（北京）技术发展有限公司 | A kind of novel SnO2Electrode and its preparation method and application |
| CN110980890A (en) * | 2019-12-26 | 2020-04-10 | 西安泰金工业电化学技术有限公司 | Titanium-based lead dioxide electrode for degrading rhodamine B and preparation method and application thereof |
| 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 |
| CN112978869B (en) * | 2021-03-17 | 2022-03-11 | 东莞理工学院 | Efficient selective Ti/SnO2Preparation method and application of (E) -Sb-MI anode material |
| CN115010222A (en) * | 2022-08-09 | 2022-09-06 | 广东工业大学 | Filtering type electrodeposition device, electrodeposition system and preparation method of DSA membrane electrode |
| CN115010222B (en) * | 2022-08-09 | 2022-11-15 | 广东工业大学 | Filtering type electrodeposition device, electrodeposition system and preparation method of DSA membrane electrode |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104030403B (en) | 2016-03-02 |
| CN104030403A (en) | 2014-09-10 |
| CN102701329B (en) | 2014-08-06 |
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