CN101417831A - Novel ti-supported lead dioxide electric pole and preparation method thereof - Google Patents
Novel ti-supported lead dioxide electric pole and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a novel titanium substrate lead dioxide electrode and a preparation method thereof, which belong to the field of water treatment technology application. The titanium substrate lead dioxide electrode adopts titanium material as a carrier; after the titanium substrate undergoes acid etching, pyrolytic process is adopted to plate a tin-stibium oxide bottom layer; alkaline solution is then used for electroplating an alpha-PbO2 intermediate layer; acidic composite electroplating solution is used for preparing a fluorine-containing beta-PbO2 surface layer doped with an active metal (such as bismuth, nickel, lanthanum, cerium and erbium) and a particle with high absorption performance (such as powdered activated carbon and chitosan), thus obtaining a novel titanium substrate lead dioxide electrode. The titanium substrate lead dioxide electrode prepared by the method has low cost and long service life. Using the electrode as an anode and applying certain applied voltage can realize efficient removal and mineralization to the organic contaminants in the water. With simple operation and convenient management, the method is applicable to small-scale and dispersible wastewater and feed water treatment.
Description
Technical field
The present invention relates to a kind of novel ti-supported lead dioxide electric pole and preparation method thereof, and use it for organic pollutant in the efficient removal water, it specifically is the fluorine-containing ti-supported lead dioxide electric pole of a kind of high absorption property particle (as Powdered Activated Carbon or chitosan) and a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium) modification, under the situation of energising, the organic pollutant efficient oxidation in the water can be belonged to the Application Areas of water technology.
Background technology
PbO
2Satisfactory electrical conductivity with metalloid, titanium base PbO
2Electrode has the oxygen evolution potential height during electrolysis in the aqueous solution, oxidation capacity is strong, solidity to corrosion good, good conductivity, can be by characteristics such as big electric currents.This electrode is compared with platinum electrode, platinized electrode or other noble metal electrode with aspects such as prices at raw material sources, has outstanding advantage.In addition, this anode can also be processed into different shape, and the anode of exhausted or damage can heavily plate regeneration.Therefore, titanium base PbO
2Electrode successfully has been applied in many inorganic and aspects such as organic compound electrolysis production, environmental pollution control at present.At present, in use there is PbO in ti-supported lead dioxide electric pole
2Settled layer and matrix bond are not tight, PbO
2The settled layer internal stress such as greatly, easily peels off at problem.
In recent years, many researchists are devoted to PbO
2Electrode surface carries out chemically modified, promptly at PbO
2The active substance that mixes in the settled layer with further this electrode property that improves, effectively reduces internal stress, improves current efficiency, realizes the functional design of electrode.Leonardo etc. (Leonardo et al., Chemosphere, 2007,2035-2043.) catalytic activity and the stability in order to improve the lead dioxide electrode degradation of dye waste water has been studied Fe
3+, F-doped P bO
2Electrode performance, the result shows, doped F e
3+, F-PbO
2The TOC clearance reached more than 95% in 2 hours in the electrode pair water, than unadulterated PbO
2Electrode has improved about 13%.Manea etc. (Manea et al.Rev.Chim., 2005,56:266-271.) with Co
2+Be doped to PbO
2In the electrode, electrode stability obviously improves.
Organic pollutant more and more is subject to people's attention in the environmental pollution improvement field in recent years as a kind of environmental friendliness technology in the electrochemical oxidation water.How to prepare high-effect stabilized electrodes, improving current efficiency is a subject matter of this area research.For this reason, we propose reactive metal (as bismuth, nickel, lanthanum, cerium, erbium) and high absorption property particle (as Powdered Activated Carbon or chitosan) are entrained in PbO by co-deposition method
2In the settled layer, by improving the absorption property of electrode materials, improve electrochemical catalytic oxidation efficient on the one hand; Can effectively reduce PbO on the other hand
2The internal stress of settled layer improves electrode life.
Summary of the invention
The objective of the invention is: prepare the fluorine-containing ti-supported lead dioxide electric pole of a kind of doping high absorption property particle (as Powdered Activated Carbon or chitosan) and reactive metal (as bismuth, nickel, lanthanum, cerium, erbium), and utilize the organic pollutant in this electrode catalyst oxidizing water.The electrode that makes has advantages such as cost is low, activity is high, electrode life is long.
Purpose of the present invention is achieved through the following technical solutions:
A kind of novel ti-supported lead dioxide electric pole is a carrier with the titanium material, is followed successively by tin-antimony oxide bottom, α-PbO from the inside to the outside by the titanium matrix surface
2Fluorine-containing β-the PbO of middle layer, a kind of reactive metal that mixes (as bismuth, nickel, lanthanum, cerium, erbium) and a kind of high absorption property particle (as Powdered Activated Carbon, chitosan)
2Upper layer.
A kind of preparation method of novel ti-supported lead dioxide electric pole, earlier with after the titanium matrix acid etch, utilize tin tetrachloride and butter of antimony butanols mixing solutions coated titanium matrix surface, after drying naturally, descended dry 10-30 minute at 105-120 ℃, by this step, repetitive coatings and dry 2-4 time in 500-550 ℃ of following pyrolytic decomposition 2-4 hour, naturally cool to room temperature again, according to above step, repetitive coatings, drying and pyrolytic decomposition at least 2 times; Then with it as anode, galvanic deposit α-PbO in being dissolved with the sodium hydroxide electroplate liquid (A) of PbO
2Middle layer, depositing time are 0.5-1 hour, and depositing temperature is 20-50 ℃, and the anodic current density of galvanic deposit is 5-15mA/cm
2After floating thing is removed in washing, with it as anode, in the acid fluorine-containing lead solution (B) that is mixed with a kind of high absorption property particle (as Powdered Activated Carbon or chitosan) and a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium), galvanic deposit mix a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium) and a kind of fluorine-containing β-PbO with high absorption property particle (as Powdered Activated Carbon or chitosan)
2Upper layer, depositing time are 0.5-1 hour, and depositing temperature is 20-50 ℃, and the anodic current density of galvanic deposit is 5-15mA/cm
2
Tin tetrachloride among the described novel ti-supported lead dioxide electric pole preparation method and butter of antimony butanols mixing solutions consist of the SnCl of 440-520mmol/L
45H
2The SbCl of O, 90-170mmol/L
3, the 8-12 parts by volume the concentrated hydrochloric acid, the propyl carbinol of 35-45 parts by volume of 36-38wt%; Be dissolved with the PbO that consists of 0.10-0.12mol/L of PbO sodium hydroxide electroplate liquid (A), the sodium hydroxide of 120-150g/L; Be mixed with a kind of high absorption property particle (as Powdered Activated Carbon or chitosan) and a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium) acid fluorine-containing lead solution (B) consist of 0.4-0.6mol/L Pb (NO
3)
2, 0.08-0.12mol/L nitric acid, 0.005-0.04mol/L KF, the nitrate of 0.002-0.05mol/L reactive metal (as bismuth, nickel, lanthanum, cerium, erbium), 1-10g/L high absorption property particle (as Powdered Activated Carbon or chitosan).
A kind of method of removing organic pollutant in the water, fluorine-containing ti-supported lead dioxide electric pole with high absorption property particle (as Powdered Activated Carbon or chitosan) and a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium) modification is an anode, titanium plate, graphite inactive, conductive material are as negative electrode, under the situation of energising, the organic pollutant in the water is oxidized.Apply 3-15mA/cm between the anode and cathode
2Strength of current, the initial pH value of institute's treating water is 4-9.
Characteristics of the present invention are:
(1) prepared novel ti-supported lead dioxide electric pole is followed successively by tin-antimony oxide bottom, α-PbO from the inside to the outside
2Fluorine-containing β-the PbO of middle layer, a kind of reactive metal that mixes (as bismuth, nickel, lanthanum, cerium, erbium) and a kind of high absorption property particle (as Powdered Activated Carbon, chitosan)
2Upper layer.
(2) prepared novel ti-supported lead dioxide electric pole cost is low, in the oxidizing water organic pollutant active high, internal stress is little, electrode life is long.
(3) adopt organic pollutant in the prepared novel ti-supported lead dioxide electric pole oxidizing water, technology is simple, and is low to the operational management requirement, is applicable to that small-scale and decentralized waste water reach to water treatment.
Embodiment
Below with specific embodiment embodiment is described.
Example 1
A kind of novel ti-supported lead dioxide electric pole, the preparation method is as follows: with 15cm
2The titanium plate put into 10% oxalic acid solution, etching 2h under little situation of boiling utilizes the washed with de-ionized water surface after the taking-up; Utilize tin tetrachloride and butter of antimony butanols mixing solutions (485mmol/L SnCl
45H
2O, 130mmol/L SbCl
3, the concentrated hydrochloric acid of 10mL 36-38wt%, 40mL propyl carbinol) the coated titanium matrix surface, naturally after drying, drying is 15 minutes under 120 ℃, by this step, repetitive coatings and dry 2 times in 500 ℃ of following pyrolytic decompositions 2 hours, naturally cool to room temperature again, according to above step, repetitive coatings, drying and pyrolytic decomposition 4 times; Then with it as anode, the titanium plate is as negative electrode, is dissolved with galvanic deposit α-PbO in the electroplate liquid (A) of 0.11mol/LPbO and 140g/L sodium hydroxide at 100mL
2Middle layer, depositing time are 1 hour, and depositing temperature is 40 ℃, and the anodic current density of galvanic deposit is 10mA/cm
2After floating thing was removed in washing, as anode, the titanium plate was as negative electrode with it, was mixed with 5g/L chitosan and 0.004mol/L Erbium trinitrate, 0.5mol/L Pb (NO at 100mL
3)
2, 0.1mol/L nitric acid, 0.005mol/L KF electroplate liquid (B) in galvanic deposit β-PbO
2Upper layer, depositing time are 1 hour, and depositing temperature is 20 ℃, and the anodic current density of galvanic deposit is 10mA/cm
2, promptly get novel ti-supported lead dioxide electric pole.
Adopt this electrode as 2 in the anodic oxidation water, 4-two chlorophenols, negative electrode are the titanium plate, and annode area and cathode area are 15cm
2, interpole gap 15mm, received current intensity is 75mA.2,4-dichloro phenol solution starting point concentration is 90mg/L, and volume is 180mL, and initial pH is 5.3, and ionogen is a 0.02mol/L sodium sulfate, after 180min is carried out in reaction, and 2,4-two chlorophenol concentration are 2.2mg/L, clearance reaches 97.6%.
Example 2
Electrode preparation method such as example 1, different is electroplate liquid (B) is 100mL is mixed with 5g/L chitosan and 0.004mol/L Bismuth trinitrate, 0.5mol/L Pb (NO
3)
2, 0.1mol/L nitric acid, 0.02mol/L KF.
Adopt this electrode as 2 in the anodic oxidation water, 4-dichloro phenol method such as example 1, different is 2,4-dichloro phenol solution volume is 100mL, after 120min is carried out in reaction, 2,4-two chlorophenol concentration are 0.5mg/L, clearance reaches 99.4%.
Example 3
Electrode preparation method such as example 1, different is electroplate liquid (B) is 100mL is mixed with 5g/L Powdered Activated Carbon and 0.004mol/L lanthanum nitrate, 0.5mol/L Pb (NO3) 2,0.1mol/L nitric acid, 0.005mol/L KF.
Adopt this electrode as 2 in the anodic oxidation water, 4-dichloro phenol method such as example 1, different is 2,4-dichloro phenol solution volume is 100mL, after 120min is carried out in reaction, 2,4-two chlorophenol concentration are 0.4mg/L, clearance reaches 99.6%.
Claims (6)
1. a novel ti-supported lead dioxide electric pole is characterized in that, is carrier with the titanium material, is followed successively by tin-antimony oxide bottom, α-PbO from the inside to the outside by the titanium matrix surface
2Fluorine-containing β-the PbO of middle layer, a kind of reactive metal that mixes (as bismuth, nickel, lanthanum, cerium, erbium) and a kind of high absorption property particle (as Powdered Activated Carbon, chitosan)
2Upper layer.
2. the preparation method of the described novel ti-supported lead dioxide electric pole of claim 1, it is characterized in that,, utilize tin tetrachloride and butter of antimony butanols mixing solutions coated titanium matrix surface earlier with after the titanium matrix acid etch, naturally after drying, 105-120 ℃ dry 10-30 minute down, by this step, repetitive coatings and dry 2-4 time, again in 500-550 ℃ of following pyrolytic decomposition 2-4 hour, naturally cool to room temperature, according to above step, repetitive coatings, drying and pyrolytic decomposition at least 2 times; Then with it as anode, galvanic deposit α-PbO in being dissolved with the sodium hydroxide electroplate liquid (A) of PbO
2Middle layer, depositing time are 0.5-1 hour, and depositing temperature is 20-50 ℃, and the anodic current density of galvanic deposit is 5-15mA/cm
2After floating thing is removed in washing, with it as anode, in the acid fluorine-containing lead solution (B) that is mixed with a kind of high absorption property particle (as Powdered Activated Carbon or chitosan) and a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium), galvanic deposit mix a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium) and a kind of fluorine-containing β-PbO with high absorption property particle (as Powdered Activated Carbon or chitosan)
2Upper layer, depositing time are 0.5-1 hour, and depositing temperature is 20-50 ℃, and the anodic current density of galvanic deposit is 5-15mA/cm
2
3. according to the described preparation method of claim 2, it is characterized in that described tin tetrachloride and butter of antimony butanols mixing solutions consist of the SnCl of 440-520mmol/L
45H
2The SbCl of O, 90-170mmol/L
3, the 8-12 parts by volume the concentrated hydrochloric acid, the propyl carbinol of 35-45 parts by volume of 36-38wt%.
4. according to the described preparation method of claim 2, it is characterized in that, be dissolved with the PbO that consists of 0.10-0.12mol/L of the sodium hydroxide electroplate liquid (A) of PbO, the sodium hydroxide of 120-150g/L.
5. according to the described preparation method of claim 2, it is characterized in that, be mixed with a kind of high absorption property particle (as Powdered Activated Carbon or chitosan) and a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium) acid fluorine-containing lead solution (B) consist of 0.4-0.6mol/L Pb (NO
3)
2, 0.08-0.12mol/L nitric acid, 0.005-0.04mol/L KF, the nitrate of 0.002-0.05mol/L reactive metal (as bismuth, nickel, lanthanum, cerium, erbium), 1-10g/L high absorption property particle (as Powdered Activated Carbon or chitosan).
6. method of removing organic pollutant in the water, it is characterized in that, fluorine-containing ti-supported lead dioxide electric pole with high absorption property particle (as Powdered Activated Carbon or chitosan) and a kind of reactive metal (as bismuth, nickel, lanthanum, cerium, erbium) modification is an anode, titanium plate, graphite inactive, conductive material apply 3-15mA/cm as negative electrode between anode and cathode
2Strength of current, the initial pH value of institute's treating water is 4-9.
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