CN105502589B - A kind of ti-supported lead dioxide electric pole for mixing the modification of chromium strontium titanates and preparation method thereof - Google Patents

A kind of ti-supported lead dioxide electric pole for mixing the modification of chromium strontium titanates and preparation method thereof Download PDF

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CN105502589B
CN105502589B CN201510863863.6A CN201510863863A CN105502589B CN 105502589 B CN105502589 B CN 105502589B CN 201510863863 A CN201510863863 A CN 201510863863A CN 105502589 B CN105502589 B CN 105502589B
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modification
coating
mixing
strontium titanates
srtio
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CN105502589A (en
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贺前锋
陈亚利
宋乐山
言海燕
姚咏歌
赵迪
阙雄杰
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HUNAN YONKER ENVIRONMENTAL PROTECTION RESEARCH INSTITUTE Co Ltd
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HUNAN YONKER ENVIRONMENTAL PROTECTION RESEARCH INSTITUTE Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • 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
    • C02F1/46109—Electrodes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/24—Chromium, molybdenum or tungsten
    • B01J23/26—Chromium
    • B01J35/39—
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • 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
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • C02F2001/46138—Electrodes comprising a substrate and a coating
    • C02F2001/46142—Catalytic coating
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

Abstract

The invention discloses a kind of ti-supported lead dioxide electric pole for mixing the modification of chromium strontium titanates and preparation method thereof, the electrode includes substrate and coating, the substrate is titanium substrate, coating is made up of the Lead oxide brown for mixing the modification of chromium strontium titanates, the content that chromium strontium titanates is mixed in coating is 5 12 wt%, the thickness of coating is 0.2 1 mm, and the Lead oxide brown is β PbO2.By Cr SrTiO3Modification, make β PbO obtained by electro-deposition2Crystal grain refinement, improves its electrocatalysis characteristic.Additionally, Cr SrTiO3The ti-supported lead dioxide electric pole of modification have it is visible light-responded, can cross under visible light action, by photoelectric-synergetic effect Organic substance is degraded, improve sun light utilization efficiency.

Description

A kind of ti-supported lead dioxide electric pole for mixing the modification of chromium strontium titanates and preparation method thereof
Technical field
The present invention relates to a kind of ti-supported lead dioxide electric pole for mixing the modification of chromium strontium titanates and preparation method thereof.
Background technology
Photocatalysis technology and electro-catalysis technology can be by the organic pollutant degradations in water as important advanced oxidation Compound for environmental sound even realizes permineralization, has therefore suffered from people and has more and more paid close attention to, and light anode is light The core of electro-catalytic oxidation technology research.
DSA electrodes, TiO2Modified β-PbO2Electrode etc. is used as anode material and is studied, and shows substantially Concerted catalysis effect.But above-mentioned adopted electrode does not have or at all no visible light-responded, and no visible light photocatalysis are lived Property, for photoelectric catalysis degrading organic pollution, the utilization rate of sunlight is low.
In order to make full use of sunlight, the photocatalysts with visible light catalysis activity numerous in recent years are developed, portion Divided catalyst shows higher photocatalysis degradation organic contaminant activity.But, the electrode material with visible light catalysis activity Research still compare the time, the electrode material with photocatalytic activity have it is very weak or do not possess visible light catalytic work Property.Therefore exploitation has the great application prospect of anode material of visible light catalysis activity.
The content of the invention
Present invention solves the technical problem that being, photoelectrocatalysiss anode of the prior art does not possess visible light-responded, or can See that photoresponse is not strong.
The technical scheme is that, there is provided a kind of ti-supported lead dioxide electric pole for mixing the modification of chromium strontium titanates, the electrode Including substrate and coating, the substrate is titanium substrate, and coating is made up of the Lead oxide brown for mixing the modification of chromium strontium titanates, and chromium is mixed in coating The content of strontium titanates is 5-12 wt%, and the thickness of coating is 0.2-1 mm, and the Lead oxide brown is β-PbO2。
Further, the content of the middle chromium for mixing chromium strontium titanates is 1-6wt%；Wherein wt% represents quality percentage Number.
Further, the plating is deposited in titanium substrate using electro-deposition；Pb in the deposition liquid of the electro-deposition2+It is dense Spend for 0.2-0.5M, the concentration for mixing chromium strontium titanate nanoparticles is 5-15g/L.
Further, the Cu in the deposition liquid of the electro-deposition also containing 0.005-0.015 M2+。
Further, in the electrodeposition process, electric current density is 20-60 mA/cm2, mixing speed is 300- 600rpm, temperature are 25-35 DEG C, electro-deposition 1-3h.
SrTiO3It is typical perofskite type oxide, with high-k, low-dielectric loss, and excellent ferrum The properties such as electricity, piezoelectricity, pyroelectricity, be prepare multilayer ceramic capacitor, Nonvolatile ferroelectric random access memory, pressure transducer, The critical function material of the various devices such as thermal resistor.The energy gap of strontium titanates is 3.2 eV, is after TiO2It is another kind of afterwards Most it is hopeful to realize the photocatalyst semi-conducting material of practical application.Also, SrTiO3Fermi level it is of a relatively high, have ratio TiO2Higher light potential.β-PbO2Because which has the advantages that strong good conductivity, corrosion resistance, low cost, oxygen evolution potential are high and normal For electro-catalysis anode.
The present invention has prepared Cr-SrTiO using the method being co-deposited3Titanio β-the PbO of modified by nano particles2Electrode, should Electrode can be acted on by photoelectric-synergetic and reduce the quick compound of carrier, to improve light-catalyzed reaction efficiency；And by Cr- SrTiO3It is fixed on electrode, solves the problems, such as that photocatalyst is reclaimed difficult；Meanwhile, by SrTiO3The doping of nano-particle, Raising β-PbO can be played2Electrode electro catalytic activity, crystal grain thinning, the effect for improving binding force of cladding material and rotproofness.
SrTiO3Calcium nutrition structure make it have extensive ionic replacement characteristic so that transition metal ionss can be utilized Doped and substituted Sr, forms appropriate donor level or acceptor level, the photosensitivity of quasiconductor is expanded in visible-range. The present invention is by carrying out Cr-SrTiO to common anode oxide electrode ti-supported lead dioxide electric pole3（Mix chromium strontium titanates）Modification, So that coating have it is visible light-responded.
The present invention is used and mixes chromium SrTiO3The ti-supported lead dioxide electric pole of modification under visible light, leads to as photo cathode Cross photoelectric-synergetic effect and can realize the efficient degradation to methyl orange.
The invention has the beneficial effects as follows, by Cr-SrTiO3Modification, make β-PbO2 crystal grain refinements obtained by electro-deposition, carry High its electrocatalysis characteristic.Additionally, Cr-SrTiO3The ti-supported lead dioxide electric pole of modification have it is visible light-responded, can cross visible Under light action, Organic substance is degraded by photoelectric-synergetic effect, improve sun light utilization efficiency.
Description of the drawings
Fig. 1 represents strontium titanates and the XRD compares figures for mixing chromium strontium titanates.
Fig. 2 represents the XRD figure of the Lead oxide brown for mixing the modification of chromium strontium titanates.
Fig. 3 represents comparison diagram of the various light anodes to methyl orange clearance.
Fig. 4 represents the catalytic performance under the lead dioxide electrode different condition for mixing the modification of chromium strontium titanates.
Fig. 5 represents the stability of the lead dioxide electrode catalysis for mixing the modification of chromium strontium titanates.
Specific embodiment
The flesh and blood of the present invention is further illustrated with example, but embodiment is not construed as limiting the invention.
Synthesis SrTiO3Nanoparticle powder：By 5 mL SrCl2·6H2O solution is under continuous agitation lentamente Add 8 mL Ti (OC3H7)4Aqueous isopropanol in, potassium hydroxide methanol solution, 1 mL for being subsequently added 10 mL, 2 M is oily Acid and the solution of 1 mL water；Resulting solution is reacted into 5 h at 200 DEG C using hydro-thermal method；After cooling, received by centrifugation The SrTiO that collection is generated3Nano-particle, respectively with distilled water and washing with acetone 3 times, is then dried to drying under 60 DEG C of vacuum, standby With.
Synthesis Cr-SrTiO3 nanoparticle powders：By Cr (NO3)3·9H2O and SrCl2·6H2O is by a certain percentage（1: 10）, take 5 mL solution and be slowly added into 8 mL Ti (OC under continuous agitation3H7)4Aqueous isopropanol in, subsequently plus Enter the solution of the potassium hydroxide methanol solution, 1 mL Oleic acid and 1 mL water of 10 mL, 2 M；Resulting solution is existed using hydro-thermal method 5 h are reacted at 200 DEG C；After cooling, the SrTiO for generating is collected by centrifugation3Nano-particle, respectively with distilled water and third Ketone is washed 3 times, is then dried to drying under 60 DEG C of vacuum, standby.
The SrTiO3 nanoparticle powders for obtaining and Cr-SrTiO3The XRD results of nanoparticle powder are as shown in figure 1, two The characteristic peak for planting material does not have significant difference, it can be seen that after Cr doping, SrTiO3Peak position there is certain deviation, say Bright Cr3+Part replaces SrTiO3In Sr2+。
Electro-deposition：Then the titanium substrate to cutting into 120 × 70 × 0.5 mm carries out pretreatment according to the following steps：By titanio After the elder generation of bottom, the sand papering light of 200 mesh of Jing and 600 mesh, is then soaked in 40% sodium hydroxide solution, is heated to 60 DEG C, Cleaning 2h, is soaked in 15% oxalic acid solution after washing is clean, is heated to micro-boiling, and 2 h of etching extremely form uniform fiber crops ash color table Face, is finally stored in 1% oxalic acid solution, standby.
Cr-SrTiO3Nano-particle modified titanio PbO2Electrode is prepared using the method for coelectrodeposition：Electrodeposit liquid formula It is as follows with process conditions：
Pb(NO3)2 0.4M
HNO3 0.1M
NaF 0.05 M
Cu(NO3)2 0.01 M
Cr-SrTiO310 g/L of nano-particle
30 DEG C of temperature
40 mA/cm of electric current density2
2 h of electrodeposition time
400 rpm of magnetic stirring speed
The coating that electro-deposition is obtained is in dusty blue, bright smooth.
Cr-SrTiO3Nano-particle modified titanio PbO2The XRD figure of electrode is as shown in Figure 2：XRD analysis result shows Jing Cross electro-deposition and obtain β-PbO2Coating, doped with Cr-SrTiO on the coating for obtaining3。
Under identical condition（Differ only in：By Cr-SrTiO3Nano-particle is replaced）TiO is prepared respectively2、SrTiO3 The ti-supported lead dioxide electric pole of modification, as a comparison.Respectively with TiO2/β-PbO2、SrTiO3/β-PbO2、Cr-SrTiO3/β- PbO2Three kinds of electrodes carry out photoelectrocatalysiss experiment under visible light as light anode, methyl orange of degrading.Methyl orange degradation experiment exists Volume be 100 mL single-cell for electrolyzation in carry out, negative electrode is stainless steel electrode.Electrolysis bath one side is furnished with quartz window, is reactant System introduces visible ray.Visible light source is the xenon lamp of 500 W.5 V of constant voltage is applied to system by D.C. regulated power supply.With pH it is 5 10 mg/L methyl orange solutions are used as degraded target.Acquired results Fig. 3.It can be seen that TiO2/β-PbO2、SrTiO3/β-PbO2 The effect of photoelectrocatalysiss methyl orange degradation is similar, reacts two hours, and the clearance of methyl orange is 72% or so；And Cr- SrTiO3/β-PbO2The degradation effect of electrode photo electrocatalysis methyl orange substantially increases, and reacts two hours, methyl orange clearance Up to 92.7%.
Select Cr-SrTiO3/β-PbO2As anode, pH be 5 10 mg/L methyl orange solutions as degraded target, pass through Contrast photocatalysis, electro-catalysis, photoelectric catalysis degrading effect, probe into Cr-SrTiO3/β-PbO2The photoelectric-synergetic effect played.It is real Testing is carried out in the single-cell for electrolyzation that volume is 100 mL, and negative electrode is stainless steel electrode.Electrolysis bath one side is furnished with quartz window, thinks Reaction system introduces visible ray.Visible light source is the xenon lamp of 500 W.5 V of constant voltage is applied to system by D.C. regulated power supply. As a result as shown in figure 4, from result, present invention gained Cr-SrTiO3/β-PbO2The independent photocatalysis performance of anode is not good, 2 h Methyl orange photocatalysis clearance be only 10% or so；Preferably, 2h methyl oranges clearance is up to 82.3% for electrode electrocatalysis characteristic；And Under the collective effect of both light, electricity, Cr-SrTiO3/β-PbO2Electrode shows good photoelectric-synergetic effect, to methyl The clearance of orange is up to 92.7% at two hours.
Additionally, being entered to the stability of the Cr-SrTiO3/ β-PbO2 light anodes obtained by the present invention by six circulation experiments Go test,（Experiment condition is consistent every time, and each group experiment is carried out continuously, and light anode is no longer lived again）As a result show, Cr- SrTiO3/β-PbO2Light anode is continuously used 720 minutes, and its clearance to methyl orange remains to maintain more than 90%, has Good stability.

Claims (5)

1. a kind of to mix the ti-supported lead dioxide electric pole that chromium strontium titanates is modified, the electrode includes substrate and coating, and its feature exists It is titanium substrate in, the substrate, coating is made up of the Lead oxide brown for mixing the modification of chromium strontium titanates, and the content of chromium strontium titanates is mixed in coating For 5-12 wt%, the thickness of coating is 0.2-1 mm, and the Lead oxide brown is β-PbO2。
2. electrode as claimed in claim 1, it is characterised in that the content of the middle chromium for mixing chromium strontium titanates is 1- 6wt%。
3. a kind of preparation method of electrode as claimed in claim 1 or 2, it is characterised in that the coating is sunk using electro-deposition Product is in titanium substrate；Pb in the deposition liquid of the electro-deposition2+Concentration is 0.2-0.5M, and the concentration for mixing chromium strontium titanate nanoparticles is 5-15g/L。
4. preparation method as claimed in claim 3, it is characterised in that also contain 0.005- in the deposition liquid of the electro-deposition The Cu of 0.015 M2+。
5. preparation method as claimed in claim 3, it is characterised in that in the electrodeposition process, electric current density is 20-60 mA/cm2, mixing speed is 300-600rpm, and temperature is 25-35 DEG C, electro-deposition 1-3h.
CN201510863863.6A 2015-12-01 2015-12-01 A kind of ti-supported lead dioxide electric pole for mixing the modification of chromium strontium titanates and preparation method thereof Active CN105502589B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417831A (en) * 2008-11-11 2009-04-29 北京师范大学 Novel ti-supported lead dioxide electric pole and preparation method thereof
CN102603037A (en) * 2012-04-01 2012-07-25 南京工业大学 Organic wastewater treatment film reactor utilizing sunlight-assisted electro-catalysis

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417831A (en) * 2008-11-11 2009-04-29 北京师范大学 Novel ti-supported lead dioxide electric pole and preparation method thereof
CN102603037A (en) * 2012-04-01 2012-07-25 南京工业大学 Organic wastewater treatment film reactor utilizing sunlight-assisted electro-catalysis

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
钛酸锶粉体功能材料的合成和应用研究进展;舒诗文等;<材料导报>;20120531;第26卷;89页左栏倒数第一段 *

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