CN101913678B - Photoelectrocatalytic device and method for reducing heavy metal ions using same - Google Patents
Photoelectrocatalytic device and method for reducing heavy metal ions using same Download PDFInfo
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- CN101913678B CN101913678B CN 201010256763 CN201010256763A CN101913678B CN 101913678 B CN101913678 B CN 101913678B CN 201010256763 CN201010256763 CN 201010256763 CN 201010256763 A CN201010256763 A CN 201010256763A CN 101913678 B CN101913678 B CN 101913678B
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Abstract
The invention discloses a photoelectrocatalytic device and a method for reducing heavy metal ions using the same. The photoelectrocatalytic device comprises a power source, a TiO2 light anode, a counter electrode, a fluid vessel, a reaction solution, a magnetic stirring bar, a magnetic stirrer and a light source, wherein the light anode adopts a hyperactivity TiO2 nano tube which has a larger specific surface area and is more favor of electric conduction; and the counter electrode adopts acid-resistant metal sheets (nets) which can provide more reaction active sites and has a large surface area, such as titanium sheets (nets), platinum sheets (nets) and the like. When the light anode area is fixed, the larger the counter electrode area is within a certain range, the higher the activity ofthe photoelectrocatalytic system is. In the invention, the TiO2 nano tube anode with a large specific surface area, the photoelectrocatalytic technology and a cathode with a large surface area are combined so as to provide a method capable of efficiently degrading high toxicity wastewater polluted by heavy metals such as Cr (VI) and the like, thus having high practical value and application prospect and being easy for promotion and utilization.
Description
Technical field
The invention belongs to the environmental chemical engineering field, the method that is specifically related to a kind of photoelectrocatalysidevice device and utilizes this device photoelectrocatalysis reducing heavy metal ion.
Background technology
Photoelectrocatalysis has caused investigator's extensive concern in recent years as the compound technology of a kind of establishment semi-conductor photoproduction electron-hole pair.The photoelectrocatalysis technology mainly is to utilize the oxidation capacity of photohole at present, is widely used in the organic pollutant in the sewage oxidation treatment.Huijun Zhao etc. utilizes porous TiO
2The a series of organism of film photoelectric catalyzed degradation, for example, methyl alcohol, glucose, para-chlorophenol, phthalic acid etc., can realize permineralization (Huijun Zhao *, Dianlu Jiang, Shanqing Zhang, William Wen Photoelectrocatalytic oxidation of organic compounds at nanoporous TiO
2Electrodes in a thin-layer photoelectrochemical cell, Journal of Catalysis 250 (2007) 102-109).Chinese patent application number: 200610117583.1 disclose " method of catalyzing oxidation of organic compounds by ultraviolet ", and this patent is with nano-TiO
2Film is the light anode, and Ag/AgCl is reference electrode, and Pt is in the battery system to electrode, and adopting phosphoric concentration is that phosphoric acid salt or the phosphate buffered saline buffer of 0.1～2.8mol/l is ionogen, carries out the reaction of catalyzing oxidation of organic compounds by ultraviolet.And utilize the reducing power of light induced electron, it is considerably less that the photoelectrocatalysis technology is applied in the reducing waste water research of heavy metal ion.
Summary of the invention
The method that the purpose of this invention is to provide a kind of photoelectrocatalysidevice device and utilize this device photoelectrocatalysis reducing heavy metal ion.
Photoelectrocatalysidevice device provided by the present invention comprises power supply, TiO
2The light anode, to electrode, liquid container, reaction soln, magnetic stir bar, magnetic stirring apparatus and light source; Wherein, described TiO
2The light anode is TiO
2Nano-pipe array thin film light anode, described is acid metal sheet or acid metal net to electrode.
Described TiO
2TiO in the nano-pipe array thin film
2The length of nanotube can be 100nm～1 μ m, and internal diameter can be 20～200nm, and thickness of pipe can be 5～50nm.
Described electrode specifically be can be titanium sheet, titanium net, platinized platinum or platinum guaze.
Described TiO
2The light anode with the Area Ratio of electrode be can be 10-0.1: 1, be preferably 4-1: 1.
Described power supply is direct supply, and its voltage is 0.5-5V; Described light source can be ultraviolet lamp.
In electric light catalytic unit provided by the present invention, described light source is arranged on around the liquid container, and described liquid container is arranged on the magnetic stirring apparatus, and described reaction solution and magnetic stir bar are arranged in the liquid container, described TiO
2Light anode and electrode all is arranged in the reaction solution.
Used TiO among the present invention
2Nano-pipe array thin film light anode can prepare by the following method:
(1) the Ti sheet is cleaned in acetone, ethanol, deionized water for ultrasonic successively, then at mol ratio HF: HNO
3: H
2O=1: (2～5): polishing 30s processes in the mixing solutions of (5～20), and deionized water rinsing dries;
(2) be in the 0.3-0.5%HF solution in mass concentration, as anode, the Pt electrode is as negative electrode with the Ti sheet, and anodic oxidation 10-60min obtains TiO under the 15-30V voltage
2Nano-pipe array thin film;
(3) with TiO
2Nano-pipe array thin film deionized water ultrasonic cleaning is dried, and 350～550 ℃ of roasting 0.5～3h obtain TiO in the air atmosphere
2Nano-pipe array thin film light anode.
The method of photoelectrocatalysis reducing heavy metal ion provided by the present invention, that the solution that will contain heavy metal ion places photoelectrocatalysidevice device provided by the present invention, with organism as hole trapping agents, inorganic salt as ionogen, the solution that contains heavy metal ion is carried out the photoelectrocatalysis reduction reaction.
Described heavy metal ion can be selected from following at least a ion: Cr (VI), Hg (II), Pb (II) and Cu (II); The described pH value that contains the solution of heavy metal ion is 1-4, and the concentration of heavy metal ion is 0-2mmol/L, but does not comprise 0mmol/L.
Described hole trapping agents specifically can be citric acid, 4-chlorophenol, rhodamine B or methylene blue; In the reaction solution of described photoelectrocatalysis reduction reaction, the working concentration of citric acid, 4-chlorophenol is 0.01～5mmol/L, and the working concentration of rhodamine B, methylene blue is 0～0.1mmol/L.
Described ionogen specifically can be NaCl, Na
2SO
4Or NaClO
4, electrolytical working concentration described in the reaction solution of described photoelectrocatalysis reduction reaction is 0～1mol/L.
The present invention is with the TiO of high-specific surface area
2The negative electrode triplicity of nanotube anode, photoelectrocatalysis technology, high surface area proposes a kind of method of the contour toxic heavy metal pollutant effluents of Cr (VI) of can degrading efficiently.
The present invention takes above technical scheme, has the following advantages: 1, TiO
2The more general TiO of nano-pipe array thin film
2Film has higher specific surface area, and the conduction that its tubular structure is conducive to electronics shows higher activity.2, apply bias voltage and can with the transfer transport that produces on the light anode to negative electrode, promote the separation of electron-hole pair.3, because the heavy metal reduction reaction occurs in electrode, adopt large-arealy to electrode, for metal ion provides more adsorption site and reduction reaction avtive spot, greatly improved the degradation rate of heavy metals such as Cr (VI).4, the good stability of reaction unit of the present invention, it is still very high to reuse repeatedly activity.5, method proposed by the invention is simple, inexpensive, efficient, stable, can be applicable to the fast thoroughly processing of the heavy metal wastewater therebies such as high density Cr (VI), has very high practical value and application prospect, is easy to promote the use of.
Description of drawings
Fig. 1 is the structural representation of photoelectrocatalysidevice device of the present invention.
Fig. 2 is when adopting the inventive method and existing photocatalysis method degraded Cr (VI), the time dependent curve of Degradation and Transformation rate of Cr (VI).
When Fig. 3 is the photoelectric catalysis degrading Cr (VI) of different anodes and different cathode areas, the time dependent curve of Degradation and Transformation rate of Cr (VI).
Fig. 4 is for adopting apparatus of the present invention to the photoelectric catalysis degrading activity curve of different concns Cr (VI).
Embodiment
Below in conjunction with drawings and Examples the present invention is described in detail.
The present invention is with TiO
2Nanotube and the combination of photoelectrocatalysis technology, and adopt the conducts such as large-area Ti net or Pt net to the reduction of application of electrode in heavy metal ion such as Cr (VI).By apply bias voltage electronics is led large-area on the electrode, with the heavy metal ion generation reduction reaction that fully is adsorbed on electrode surface, reach abundant separate electronic-hole to, effectively utilize the effect of electronics and efficient degradation Cr (VI) ion.
As shown in Figure 1, photoelectric reacting device provided by the present invention is comprised of 9 parts: light source 1, quartzy liquid holding cup 2, TiO
2Light anode 3, to electrode 4, reaction soln 5, agitator 6, magnetic stir bar 7, power supply 8 and volt ohm-milliammeter 9.What light source 1 adopted is ultraviolet lamp, is arranged on around the quartzy liquid holding cup 2, and quartzy liquid holding cup 2 is arranged on the magnetic stirring apparatus 6, and electrolyte solution 5 and magneton all are arranged in the quartzy liquid holding cup 2, light anode 3 and electrode 4 all is arranged in the electrolyte solution 5.
Light anode 3 is TiO
2Nano-pipe array thin film light anode, wherein TiO
2The length of nanotube can be 100nm～1 μ m internal diameter and can be 20～200nm, and thickness of pipe can be 5～50nm.Electrode 4 be can be acid metal sheet (net), such as titanium sheet (net), platinized platinum (net) etc.Reaction soln 5 contains heavy metal ion such as Cr (VI) solution for certain pH, and concentration is 0～2mmol/L, and the pH value is 1～4; Wherein comprise organism as hole trapping agents and inorganic salt as ionogen.Described hole trapping agents is selected from any in citric acid, 4-chlorophenol, rhodamine B and the methylene blue.The working concentration of citric acid, 4-chlorophenol is 0.01～5mmol/L, and the working concentration of rhodamine B, methylene blue is 0～0.1mmol/L.Described ionogen is selected from NaCl, Na
2SO
4And NaClO
4In any, working concentration is 0～1mol/L.Magnetic stir bar+magnetic stirring apparatus 6 all can be purchased from market, and the two cooperates and is used for reaction soln is stirred, and guarantees that the reaction system strength of solution is even.Power supply 7 is a direct current power supply, and voltage range is 0.5～5V.Volt ohm-milliammeter 8 is for detection of the electric current in the reaction process.
The preparation method of the light anode 3 in the photoelectrocatalysidevice device provided by the present invention comprises the steps:
(1) the Ti sheet of market being buied is cut into a certain size rectangle, cleans in acetone, ethanol, deionized water for ultrasonic successively, then at mol ratio HF: HNO
3: H
2O=1: (2～5): polishing 30s processes in the mixing solutions of (5～20), and deionized water rinsing dries.
(2) in 0.3～0.5wt%HF solution, as anode, the Pt electrode is as negative electrode with the Ti sheet, and 15～30V anodic oxidation, 10～60min obtains TiO
2Nano-pipe array thin film.
(3) with the TiO that obtains
2Nanotube dries through the deionized water ultrasonic cleaning, and 450 ℃ of roasting 1h obtain certain thickness TiO in the air atmosphere
2Nano-pipe array thin film light anode.
The preparation method to electrode 4 in the photoelectrocatalysidevice device provided by the present invention is as follows: the Ti net that market is buied is cut into a certain size rectangle, cleans in acetone, ethanol, deionized water for ultrasonic successively, then at HF: HNO
3: H
2O=1: polishing 30s processes in 3: 16 mixing solutionss, and deionized water rinsing dries, and namely gets the Ti net to electrode.
Used photoelectrocatalysidevice device, as shown in Figure 1.This device adopts TiO
2Nano-pipe array thin film is the light anode, wherein, and TiO
2The length of nanotube is 248nm, and the Ti net is to electrode, light anode and be 1: 1 to the Area Ratio of electrode.The starting point concentration of Cr in the reaction system (VI) is 0.34mmol/L, reaction conditions: pH 2.5, citric acid 0.5mmol/L, NaCl 1mol/L, voltage 1.5V.Utilize ultraviolet-visible pectrophotometer to detect the concentration of Cr (VI).And take electrocatalytic method, photodissociation method and photocatalytic method degrade respectively Cr (VI) activity as the contrast, the degradation efficiency to Cr (VI) of photoelectrocatalysis method more of the present invention and above-mentioned three kinds of methods.
The results are shown in Figure 2.The Degradation and Transformation rate of each curve representation Cr (VI) curve over time among Fig. 2, X-coordinate represents the time, ordinate zou represents the degradation efficiency of Cr (VI).The a curve represents electrocatalysis, and the b curve represents photodissociation, and the c curve represents photochemical catalysis, and the d curve represents photoelectrocatalysis.In system of the present invention, adopt Cr (VI) nothing degraded under the electrocatalytic method 1.5V voltage, adopt photodissociation method illumination 2h rear section Cr (VI) that photodissociation occurs.Relatively c and d degradation rate are as can be known, apply bias voltage and can significantly accelerate the degraded of Cr (VI), its zeroth order reaction rate constant is light-catalysed 7.2 times, and the photoelectric-synergetic effect is remarkable, and 60min can degradable starting point concentration be the Cr (VI) of 0.34mmol/L.
Used photoelectrocatalysidevice device, as shown in Figure 1.This device adopts TiO
2Nano-pipe array thin film is the light anode, wherein, and TiO
2The length of nanotube is 248nm; The Ti net is to electrode, and the area of light anode is 60*52mm
2Reaction conditions is with embodiment 1.
Relatively the Ti net of different area the results are shown in Figure 3 to the impact of electrode pair photoelectric catalysis degrading Cr (VI) system.
As seen from Figure 3, with certain area (60*52mm
2) TiO
2Nano-pipe array thin film is during as the light anode, the light anode be that larger to electrode area, photoelectric catalytically active is higher in 4～1: 1 scope to the electrode area ratio, be 60*52mm in the Ti web area
2The time reach maximum.This is because large-area Ti net can provide enough avtive spot fully to be adsorbed on its surface for Cr (VI) to electrode, and further with light induced electron generation reduction reaction.And when fixing be 60*52mm to electrode area
2, be fine and close TiO with the light anode change
2During/ito thin film, its activity is but far below TiO
2Nano-pipe array thin film light anode.This shows, in photoelectrocatalysis reduction Cr (VI) system, adopt simultaneously the separation of excellent light induced electron and the TiO of conductive properties
2The Ti net of light anode and high surface area could be realized the efficient degradation of Cr (VI) to electrode.
Embodiment 3, comparison are with TiO
2Nano-pipe array thin film is light anode and with TiO
2Dense film is that the light anode is on the impact of photoelectric catalysis degrading Cr (VI) system
Used photoelectrocatalysidevice device, as shown in Figure 1.This device adopts TiO
2Nano-pipe array thin film is the light anode, wherein, and TiO
2The length of nanotube is 248nm; Or TiO
2Dense film is (with TiO
2/ ITO represents that the sol-gel method preparation obtains with crystal pulling method in the ITO substrate, thickness is 160nm) be the light anode, the Ti net is to electrode, is 60*52mm to electrode area
2Reaction conditions is with embodiment 1.
Compare TiO
2Nanotube and TiO
2The activity of dense film photoelectric catalysis degrading Cr (VI) the results are shown in Figure 3.
As seen from Figure 3, be 60*52mm when fixing electrode area
2The time, be fine and close TiO with the light anode change
2/ ito thin film, the activity of its degraded Cr (VI) is but far below TiO
2Nanotube array photo-anode.This shows, in photoelectrocatalysis reduction Cr (VI) system, adopt simultaneously the separation of excellent light induced electron and the TiO of conductive properties
2The Ti net of light anode and high surface area could be realized the efficient degradation of Cr (VI) to electrode.
Embodiment 4, utilize the Cr (VI) of photoelectrocatalysidevice device of the present invention degraded different concns
Used photoelectrocatalysidevice device, as shown in Figure 1.This device adopts TiO
2Nano-pipe array thin film is the light anode, wherein, and TiO
2The length of nanotube is 248nm; The Ti net is to electrode, and the area of light anode is 60*52mm
2, be 60*52mm to the area of electrode
2Reaction conditions is with embodiment 1.
Relatively the photoelectric catalysis degrading of different concns Cr (VI) is active, the results are shown in Figure 4.
As seen from Figure 4, increase the concentration of Cr (VI), its photoelectric catalysis degrading speed reduces.Because under the High Concentration Situation, there is certain restriction in the mass transfer of reduzate, in addition, and the TiO of load on the light anode
2Amount be certain, be difficult to satisfy the degraded of the Cr (VI) of high density.When reduction high concentrate Cr (VI) waste water, can suitably increase the area of light anode and photocathode, with the photoelectric catalysis degrading effect that obtains.In this case study, be 60*52mm at the light anode with to electrode area
2The time, the suitable starting point concentration of Cr (VI) is 0.19-0.58mmol/L.
Claims (8)
1. the method for a photoelectrocatalysis reducing heavy metal ion is that the solution that will contain heavy metal ion places photoelectrocatalysidevice device, with organism as hole trapping agents, inorganic salt as ionogen, the solution that contains heavy metal ion is carried out the photoelectrocatalysis reduction reaction;
Described photoelectrocatalysidevice device comprises power supply, TiO
2The light anode, to electrode, liquid container, reaction soln, magnetic stir bar, magnetic stirring apparatus and light source, it is characterized in that: described TiO
2The light anode is TiO
2Nano-pipe array thin film light anode, described is titanium sheet or titanium net to electrode; Described TiO
2The area of light anode be 4-1:1 to the Area Ratio of electrode.
2. method according to claim 1, it is characterized in that: described heavy metal ion is selected from following at least a ion: Cr (VI), Hg (II), Pb (II) and Cu (II); The described pH value that contains the solution of heavy metal ion is 1-4, and the concentration of heavy metal ion is 0-2mmol/L, but does not comprise 0mmol/L.
3. method according to claim 1 and 2, it is characterized in that: described hole trapping agents is citric acid, 4-chlorophenol, rhodamine B or methylene blue; In the reaction solution of described photoelectrocatalysis reduction reaction, the working concentration of citric acid and 4-chlorophenol is 0.01～5mmol/L, and the working concentration of rhodamine B and methylene blue is 0～0.1mmol/L, but does not comprise 0mmol/L.
4. method according to claim 1 and 2, it is characterized in that: described ionogen is NaCl, Na
2SO
4Or NaClO
4Electrolytical working concentration described in the reaction solution of described photoelectrocatalysis reduction reaction is 0～1mol/L, but does not comprise 0mol/L.
5. method according to claim 1 and 2 is characterized in that: in the described photoelectrocatalysidevice device, and described TiO
2TiO in the nano-pipe array thin film
2The length of nanotube is 100nm～1 μ m, and internal diameter is 20～200nm, and thickness of pipe is 5～50nm.
6. method according to claim 1 and 2 is characterized in that: described TiO
2Nano-pipe array thin film light anode prepares by the following method:
(1) the Ti sheet is cleaned at acetone, ethanol, deionized water for ultrasonic successively, then by HF, HNO
3And H
2Polishing 30s processes in the mixing solutions that O forms, and deionized water rinsing dries; Wherein, HF, HNO in the described mixing solutions
3And H
2The mol ratio of O is followed successively by 1:(2～5): (5～20);
(2) be in the 0.3-0.5%HF solution in mass concentration, as anode, the Pt electrode is as negative electrode with the Ti sheet, and anodic oxidation 10-60min obtains TiO under the 15-30V voltage
2Nano-pipe array thin film;
(3) with TiO
2Nano-pipe array thin film deionized water ultrasonic cleaning is dried, and 350～550 ℃ of roasting 0.5～3h obtain TiO in the air atmosphere
2Nano-pipe array thin film light anode.
7. method according to claim 1 and 2, it is characterized in that: described power supply is direct supply, its voltage is 0.5-5V; Described light source is ultraviolet lamp.
8. method according to claim 1 and 2, it is characterized in that: described light source is arranged on around the liquid container, and described liquid container is arranged on the magnetic stirring apparatus, and described reaction solution and magnetic stir bar are arranged in the liquid container, described TiO
2Light anode and electrode all is arranged in the reaction solution.
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| BR112014013372A2 (en) | 2011-12-02 | 2017-06-13 | Aquamost Inc | apparatus and method for treating aqueous solutions and contaminants therein |
| US8398828B1 (en) | 2012-01-06 | 2013-03-19 | AquaMost, Inc. | Apparatus and method for treating aqueous solutions and contaminants therein |
| US9045357B2 (en) | 2012-01-06 | 2015-06-02 | AquaMost, Inc. | System for reducing contaminants from a photoelectrocatalytic oxidization apparatus through polarity reversal and method of operation |
| CA2900722A1 (en) | 2013-02-11 | 2014-08-14 | AquaMost, Inc. | Apparatus and method for treating aqueous solutions and contaminants therein |
| CN103422138A (en) * | 2013-08-22 | 2013-12-04 | 浙江大学 | Method for preparing titanium dioxide nanometer tube |
| CN104069786B (en) * | 2014-06-23 | 2016-10-05 | 华南理工大学 | A kind of photoelectrocatalysis reaction unit and the method processing organic polluting water |
| CN105582906A (en) * | 2014-10-24 | 2016-05-18 | 广州贝特缪斯能源科技有限公司 | Visible-light photocatalytic material and preparation method therefor |
| CN104944511B (en) * | 2015-05-27 | 2017-12-08 | 北京大学 | The method and apparatus that a kind of photoelectrocatalysis removes heavy metal ions in wastewater |
| CN105214634B (en) * | 2015-10-28 | 2017-09-19 | 中国科学院合肥物质科学研究院 | Careless mesh screen of rutile type titanium oxide nanometer and its production and use |
| CN105776444A (en) * | 2016-04-25 | 2016-07-20 | 青岛理工大学 | Method for strengthening Cr (VI) electroreduction by using small-molecular organic acid |
| CN106894047B (en) * | 2017-03-10 | 2019-01-22 | 傅楚闽 | A kind of environmental protection recycling method of nickel in chemical nickel-plating ageing liquid |
| CN107941731A (en) * | 2017-12-05 | 2018-04-20 | 海南聚能科技创新研究院有限公司 | COD on-line detector in a kind of water quality |
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