CN104556312A - Method for preparing porous PbO2 electrode for deep sewage treatment - Google Patents
Method for preparing porous PbO2 electrode for deep sewage treatment Download PDFInfo
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- CN104556312A CN104556312A CN201410795738.1A CN201410795738A CN104556312A CN 104556312 A CN104556312 A CN 104556312A CN 201410795738 A CN201410795738 A CN 201410795738A CN 104556312 A CN104556312 A CN 104556312A
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Abstract
The invention provides a method for preparing a porous PbO2 electrode for deep sewage treatment. The method is characterized by comprising the following steps: adjusting the pH value of an electroplating liquid prepared from 0.45-0.90M/L of an aluminum salt, 4.0-24.0mM/L of sodium fluoride and 1.3-23.0mM/L of a cerium salt to be within 1.2-1.8, and performing electric deposition by taking a Ti/SnO2-Sb electrode as a substrate electrode and Ti as a negative electrode under the conditions that the gap between the two electrodes is 15-30mm and the current density is 100-200A/m<2>. According to the porous PbO2 electrode prepared by using the method, continuous distribution of a PbO2 layer can be effectively prevented because of the porous structure, the internal stress of the PbO2 layer is released, and the stability of the electrodes is improved.
Description
Technical field
The present invention relates to a kind of porous PbO for advanced treatment of wastewater
2the preparation method of electrode, particularly, to the porous PbO containing Perfluorocaprylic Acid organic industrial sewage advanced treatment
2the preparation method of electrode, belongs to technical field of electrochemistry.
Background introduction
Perfluorocaprylic Acid (PFOA, C
7f
15cOOH) as tensio-active agent, stain control agent, additive, fire foam, macromolecule emulsifier and agrochemical, it is produced and uses and exceedes ISUZU company.Perfluorocaprylic Acid is as one of perfluorochemical (PFCs) main home to return in the environment, its stable chemical property, volatile and it can not be made extensively to be present in natural water, settling, animal and human body by the characteristic that the ecosystem is degraded, ecotope and HUMAN HEALTH in serious threat.At present, global Perfluorocaprylic Acid pollutes and has caused showing great attention to of national governments and scientific circles to the impact of HUMAN HEALTH, in June, 2000 EPA (USEPA) starts the harm noticing that Perfluorocaprylic Acid is possible, proposition low-level Perfluorocaprylic Acid and salt thereof expose may 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 Chemicals Directory inventory in 2003, on December 30th, 2009, USEPA has issued first " chemical action plan ", the health caused the long-chain perfluorochemical comprising Perfluorocaprylic Acid and environmental problem are processed.In addition, European Union to combine and has issued " sell about restriction Perfluorooctane sulfonates and the finger that uses with " on December 27th, 2006 in European Parliament and council of ministers, suspect that Perfluorocaprylic Acid and salt thereof also exist the risk level being similar to Perfluorooctane sulfonates, and promise to undertake that 2010 by the discharge of Perfluorocaprylic Acid and the minimizing of content in the product 95% thereof, eliminates by 2015 completely by it.
So far, there is no the report adopting electrochemistry Perfluorocaprylic Acid in water to be carried out to efficient mineralization purification techniques.
Summary of the invention
The object of the present invention is to provide a kind of porous PbO for advanced treatment of wastewater
2the preparation method of electrode, in the electroplate liquid comprising 0.45 ~ 0.90M/L lead salt, 4.0 ~ 24.0mM/L Sodium Fluoride, 1.3 ~ 23.0mM/L cerium salt, and adjust ph to 1.2 ~ 1.8, with Ti/SnO
2-Sb electrode, as base electrode, take Ti as negative electrode, and spacing is 15 ~ 30mm between two electrodes, electropotential is 2.4V vs SCE, current density is 100 ~ 200A/m
2under carry out galvanic deposit.
Porous PbO of the present invention
2the preparation method of electrode, described lead salt is selected from the group be made up of lead nitrate, lead sulfate, plumbic acetate.
Porous PbO of the present invention
2the preparation method of electrode, described zirconates is selected from the group be made up of zirconium nitrate, zirconium sulfate, acetic acid zirconium, and relative with described lead salt.
Porous PbO of the present invention
2the preparation method of electrode, described electroplate liquid comprises 0.6M/L lead nitrate, 4.8mM/L Sodium Fluoride, 1.6mM/L cerous nitrate.
Porous PbO of the present invention
2the preparation method of electrode, described pH value is adjusted to 1.4.
Porous PbO of the present invention
2the preparation method of electrode, with Ti/SnO
2-Sb electrode is as base electrode, and take Ti as negative electrode, spacing is 20mm between two electrodes.
Porous PbO of the present invention
2the preparation method of electrode, described electropotential is 2.4V vsSCE, current density is 200A/m
2under carry out galvanic deposit.
Porous PbO of the present invention
2the preparation method of electrode, PbO
2the vesicular structure of electrode adopts hydrogen bubble template preparation, and the polarized potential controlling plate is 1.5V vs SCE.
Porous PbO of the present invention
2the preparation method of electrode, is characterized in that, the PbO prepared
2crystal diameter is less than 500nm.
The present invention also provides a kind of porous PbO prepared by described preparation method
2electrode.
Porous PbO of the present invention
2electrode, described porous PbO
2the pore diameter size of electrode is 20 μm ~ 60 μm.
Porous PbO of the present invention
2electrode, at 2A/cm
2, 1mol/L, the result of carrying out reinforcing life test under the condition of 50 DEG C be greater than 10000h, coating spending rate is less than 4mg (kAh)
-1.
The present invention further provides a kind of advanced treatment method for sewage water, use porous PbO of the present invention
2electrode carries out.
The invention has the advantages that: the porous PbO prepared by the present invention
2electrode, these pore structures effectively can stop PbO
2the continuous distribution of layer, release PbO
2the internal stress of layer, thus improves the stability of electrode; On the other hand, these pore structures also can increase roughness and the surface-area of electrode, are conducive to the catalytic performance improving electrode.By the porous PbO that the present invention prepares
2electrode, (can be not more than 200A/cm at high current density
2) under steady running, show good erosion resistance and the work-ing life of overlength when electrode works in an acidic solution.Further, the present invention, owing to adopting electrochemical oxidation process, has technical process simple, easy to operate, and reaction conditions is gentle, and treatment effect is good and reliable and stable, is easy to realize industrial applications.
Accompanying drawing explanation
Fig. 1 is that the porous of preparation receives brilliant Ti/SnO
2 -sn/Ce-PbO
2electrode surface pattern.
Embodiment
Below, by conjunction with the accompanying drawing in the embodiment of the present invention, be described in detail the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
It should be noted that, in this article, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.
The invention provides a kind of porous PbO for advanced treatment of wastewater
2the preparation method of electrode, in the electroplate liquid comprising 0.45 ~ 0.90M/L lead salt, 4.0 ~ 24.0mM/L Sodium Fluoride, 1.3 ~ 23.0mM/L cerium salt, and with acid for adjusting pH value to 1.2 ~ 1.8, with Ti/SnO
2-Sb electrode, as base electrode, take Ti as negative electrode, and spacing is 15 ~ 30mm between two electrodes, electropotential is 2.4V vs SCE, current density is 100 ~ 200A/m
2under carry out galvanic deposit.
Porous PbO of the present invention
2the preparation method of electrode, described electroplate liquid comprises 0.6M/L lead nitrate, 4.8mM/L Sodium Fluoride, 1.6mM/L cerous nitrate.
In the present invention, with Ti/SnO
2-Sb electrode as base electrode, at its surface deposition PbO
2electrode layer, in preparation process, Ti/SnO
2-Sb electrode layer can produce oxygen by brine electrolysis, and gas is piled up at polar board surface, and impact even stops PbO
2the same Ti/SnO of electrode layer
2the combination of-Sb electrode layer, causes electrode performance to decline and even prepares failure, and therefore those skilled in the art need the generation evading brine electrolysis side reaction by adding the means such as other materials, control electrode current potential.In the present invention, control bubble by regulating electropotential and produce speed, guiding gas is piled up in the site of polar board surface limited quantity, eliminates bubble to PbO
2electrode layer and Ti/SnO
2the impact that-Sb electrode layer combines, simultaneously at PbO
2electrode layer produces the aperture of specific dimensions, increases obtained porous PbO
2the specific surface area of electrode, namely this method is hydrogen bubble template.
Embodiment 1
Provided by the invention for the porous PbO containing Perfluorocaprylic Acid organic industrial sewage advanced treatment
2the preparation method of electrode, further comprising the steps of:
Ti substrate pretreated: be first that Ti matrix sand paper is polished, remove oxide on surface, then 1 ~ 2h in the sodium hydroxide solution of 100 DEG C 5% ~ 10% is immersed, to remove the greasy dirt on surface, taking-up distilled water cleans, 2 ~ 3h is etched afterwards, to obtain grey even curface in 100 DEG C of oxalic acid solutions of 10% ~ 15%;
The polymerization forerunner colloidal sol preparation of tin antimony: at 50 ~ 70 DEG C of temperature, a certain amount of citric acid is dissolved in (citric acid and ethylene glycol mol ratio are 1:4 ~ 6) in ethylene glycol, after dissolving completely, steady temperature 30 ~ 60min is 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 100 DEG C afterwards and constant temperature 1 ~ 3h, after naturally cooling, namely obtain the polymeric precursor colloidal sol of tin-antimony;
Ti/SnO
2prepared by-Sb electrode: adopt and draw formulation to overlay on Ti matrix by the polymeric precursor colloidal sol of the tin-antimony of preparation, in the baking oven of 120 ~ 160 DEG C, keep 10 ~ 20min to make colloidal sol transfer gel to afterwards, then roasting 10 ~ 30min in air atmosphere is proceeded in 450 ~ 550 DEG C of retort furnaces, front process is repeated again after taking out naturally cooling cleaning, drying, 20 ~ 40 times repeatedly, 1 ~ 3h during last roasting also anneals naturally, i.e. obtained Ti/SnO
2-Sb electrode;
Finally, in the electroplate liquid comprising 0.6M/L lead nitrate, 4.8mM/L Sodium Fluoride, 1.6mM/L cerous nitrate, and by nitric acid adjust ph to 1.4, with Ti/SnO
2-Sb electrode is as base electrode, and take Ti as negative electrode, two spacing between electrodes are 20mm, and electropotential is 2.4V vsSCE, and current density is 200A/m
2under carry out galvanic deposit.
The porous of preparation receives brilliant Ti/SnO
2 -sn/Ce-PbO
2electrode surface pattern as shown in Figure 1.Known electrode surface becomes vesicular, is conducive to pollutent and adsorbs at electrode surface; PbO
2granular size is hundreds of nanometer, for nanomorphic and surface compact, greatly increases reactive behavior point position.
By porous PbO prepared by the present embodiment
2electrode, at 2A/cm
2, 1mol/L, the result of carrying out reinforcing life test under the condition of 50 DEG C be greater than 10000h, coating spending rate is less than 4mg (kAh)
-1.Meanwhile, use the electrode obtained of the present invention to process containing the waste water of Perfluorocaprylic Acid, after 90min process, the clearance of Perfluorocaprylic Acid is greater than 92.8%, TOC and have dropped 92.6%.
Embodiment 2
The polymeric precursor colloidal sol preparation of Ti substrate pretreated, tin antimony and Ti/SnO
2the preparation of-Sb electrode is with embodiment 1.
In the electroplate liquid comprising 0.45M/L lead nitrate, 4.0mM/L Sodium Fluoride, 1.3mM/L cerous nitrate, and by nitric acid adjust ph to 1.2, with Ti/SnO
2-Sb electrode is as base electrode, and take Ti as negative electrode, two spacing between electrodes are 15mm, and electropotential is 1.5V vs SCE, and current density is 100A/m
2under carry out galvanic deposit.
By porous PbO prepared by the present embodiment
2electrode, at 2A/cm
2, 1mol/L, the result of carrying out reinforcing life test under the condition of 50 DEG C be greater than 10000h, coating spending rate is less than 4mg (kAh)
-1.Meanwhile, use the electrode obtained of the present invention to process containing the waste water of Perfluorocaprylic Acid, after 90min process, the clearance of Perfluorocaprylic Acid is greater than 92.8%, TOC and have dropped 92.6%.
Embodiment 3
The polymeric precursor colloidal sol preparation of Ti substrate pretreated, tin antimony and Ti/SnO
2the preparation of-Sb electrode is with embodiment 1.
In the electroplate liquid comprising 0.9M/L lead nitrate, 24.0mM/L Sodium Fluoride, 23mM/L cerous nitrate, and by nitre nitric acid adjust ph to 1.8, with Ti/SnO
2-Sb electrode is as base electrode, and take Ti as negative electrode, two spacing between electrodes are 15mm, and electropotential is 2.9V vsSCE, and current density is 100A/m
2under carry out galvanic deposit.
By porous PbO prepared by the present embodiment
2electrode, at 2A/cm
2, 1mol/L, the result of carrying out reinforcing life test under the condition of 50 DEG C be greater than 10000h, coating spending rate is less than 4mg (kAh)
-1.Meanwhile, use the electrode obtained of the present invention to process containing the waste water of Perfluorocaprylic Acid, after 90min process, pyridine clearance is greater than 91.2%, TOC and have dropped 92.6%.
Embodiment 4
In the electroplate liquid comprising 0.6M/L lead sulfate, 4.8mM/L Sodium Fluoride, 15mM/L cerous sulfate, and by sulfuric acid adjust ph to 1.4, with Ti/SnO
2-Sb electrode is as base electrode, and take Ti as negative electrode, two spacing between electrodes are 20mm, and electropotential is 2.4V vs SCE, and current density is 200A/m
2under carry out galvanic deposit.
By porous PbO prepared by the present embodiment
2electrode, at 2A/cm
2, 1mol/L, the result of carrying out reinforcing life test under the condition of 50 DEG C be greater than 10000h, coating spending rate is less than 4mg (kAh)
-1.Meanwhile, use the electrode obtained of the present invention to process containing the waste water of Perfluorocaprylic Acid, after 90min process, pyridine clearance is greater than 92.8%, TOC and have dropped 92.6%.
Embodiment 5
In the electroplate liquid comprising 0.6M/L plumbic acetate, 4.8mM/L Sodium Fluoride, 15mM/L cerous acetate, and by acetic acid adjust ph to 1.4, with Ti/SnO
2-Sb electrode is as base electrode, and take Ti as negative electrode, two spacing between electrodes are 20mm, and electropotential is 2.4V vs SCE, and current density is 200A/m
2under carry out galvanic deposit.
By porous PbO prepared by the present embodiment
2electrode, at 2A/cm
2, 1mol/L, the result of carrying out reinforcing life test under the condition of 50 DEG C be greater than 10000h, coating spending rate is less than 4mg (kAh)
-1.Meanwhile, use the electrode obtained of the present invention to process containing the waste water of Perfluorocaprylic Acid, after 90min process, pyridine clearance is greater than 91.6%, TOC and have dropped 92.6%.
To sum up, by porous PbO prepared by the present invention
2electrode, at 2A/cm
2, 1mol/L, the result of carrying out reinforcing life test under the condition of 50 DEG C be greater than 10000h, coating spending rate is less than 4mg (kAh)
-1.Meanwhile, the present invention, owing to adopting electrochemical oxidation process, has technical process simple, easy to operate, and reaction conditions is gentle, and treatment effect is good and reliable and stable, is easy to realize industrial applications.
The electrode obtained of the present invention is used to process PFOA simulated wastewater, after 90min process, PFOA clearance is greater than 99.0%, defluorinate rate is close to 90%, and be equivalent to existing 13.5 fluorine of 15 fluorine contained in PFOA molecule and be shed in solution, TOC have dropped 92.6% simultaneously.
By the porous PbO that the present invention prepares
2electrode, these pore structures effectively can stop PbO
2the continuous distribution of layer, release PbO
2the internal stress of layer, thus improves the stability of electrode; On the other hand, these pore structures also can increase roughness and the surface-area of electrode, are conducive to the catalytic performance improving electrode.By the porous PbO that the present invention prepares
2electrode, (can be not more than 200A/cm at high current density
2) under steady running, show good erosion resistance and the work-ing life of overlength when electrode works in an acidic solution.Therefore, by porous PbO prepared by the present invention
2electrode, for containing Perfluorocaprylic Acid organic industrial sewage advanced treatment.Further, the present invention, owing to adopting electrochemical oxidation process, has technical process simple, easy to operate, and reaction conditions is gentle, and treatment effect is good and reliable and stable, is easy to realize industrial applications.
The above-mentioned description to embodiment can understand and apply the invention for ease of those skilled in the art.Any those of ordinary skill in the art, in the technical scope that the present invention discloses, can make various amendment to the present embodiment easily, and principle described herein is applied to other example executes and need not through creative work.Therefore, the invention is not restricted to embodiment here, do not depart from scope make improve and amendment all should be encompassed within protection scope of the present invention.
Claims (12)
1. the porous PbO for advanced treatment of wastewater
2the preparation method of electrode, is characterized in that, in the electroplate liquid comprising 0.45 ~ 0.90M/L lead salt, 4.0 ~ 24.0mM/L Sodium Fluoride, 1.3 ~ 23.0mM/L cerium salt, and adjust ph to 1.2 ~ 1.8, with Ti/SnO
2-Sb electrode, as base electrode, take Ti as negative electrode, and spacing is 15 ~ 30mm between two electrodes, electropotential is 2.4V vs SCE, current density is 100 ~ 200A/m
2under carry out galvanic deposit.
2. porous PbO according to claim 1
2the preparation method of electrode, is characterized in that, described lead salt is selected from the group be made up of lead nitrate, lead sulfate, plumbic acetate.
3. porous PbO according to claim 2
2the preparation method of electrode, is characterized in that, described zirconates is selected from the group be made up of zirconium nitrate, zirconium sulfate, acetic acid zirconium, and relative with described lead salt.
4. porous PbO according to claim 1
2the preparation method of electrode, is characterized in that, described electroplate liquid comprises 0.6M/L lead nitrate, 4.8mM/L Sodium Fluoride, 1.6mM/L cerous nitrate.
5. porous PbO according to any one of claim 1 to 4
2the preparation method of electrode, is characterized in that, described pH value is adjusted to 1.4.
6. porous PbO according to any one of claim 1 to 4
2the preparation method of electrode, is characterized in that, with Ti/SnO
2-Sb electrode is as base electrode, and take Ti as negative electrode, spacing is 20mm between two electrodes.
7. porous PbO according to claim 1
2the preparation method of electrode, is characterized in that, described electropotential is 2.4V vs SCE, current density is 200A/m
2under carry out galvanic deposit.
8. the porous PbO according to any one of claim 1 ~ 7
2the preparation method of electrode, is characterized in that, PbO
2the vesicular structure of electrode adopts hydrogen bubble template preparation, and the polarized potential controlling plate is 1.5V vs SCE.
9. the porous PbO according to any one of claim 1 ~ 7
2the preparation method of electrode, is characterized in that, the PbO prepared
2crystal diameter is less than 500nm.
10. the porous PbO adopting the preparation method according to any one of claim 1 ~ 9 to prepare
2electrode.
11. porous PbO according to claim 10
2electrode, is characterized in that, described porous PbO
2the pore diameter size of electrode is 20 μm ~ 60 μm.
12. 1 kinds of advanced treatment method for sewage water, is characterized in that, use the porous PbO described in claim 10 or 11
2electrode carries out.
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| CN201410795738.1A CN104556312A (en) | 2014-12-18 | 2014-12-18 | Method for preparing porous PbO2 electrode for deep sewage treatment |
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|---|---|---|---|
| CN201410795738.1A CN104556312A (en) | 2014-12-18 | 2014-12-18 | Method for preparing porous PbO2 electrode for deep sewage treatment |
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| CN104556312A true CN104556312A (en) | 2015-04-29 |
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| CN113832501A (en) * | 2021-08-27 | 2021-12-24 | 昆明理工大学 | Al @ (TiB)2+Ti4O7)-PbO2+CeO2Composite anode plate and preparation method thereof |
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