CN103818986A - Photocatalytic electrode responding to visible lights and application thereof on chromium-containing wastewater treatment - Google Patents

Photocatalytic electrode responding to visible lights and application thereof on chromium-containing wastewater treatment Download PDF

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CN103818986A
CN103818986A CN201410052110.2A CN201410052110A CN103818986A CN 103818986 A CN103818986 A CN 103818986A CN 201410052110 A CN201410052110 A CN 201410052110A CN 103818986 A CN103818986 A CN 103818986A
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nts
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waste water
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CN103818986B (en
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余可儿
许剑佳
邹钢
郭丝丝
俞柯军
许媛媛
王齐
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Zhejiang Gongshang University
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Abstract

The invention discloses a photocatalytic electrode responding to visible lights and an application thereof on chromium-containing wastewater treatment. The preparation method of the photocatalytic electrode comprises the following steps: impregnating a TiO2-NTs electrode in a KI solution for 2 to 2.5 hours, taking out the TiO2-NTs electrode, impregnating the TiO2-NTs electrode in an AgNO3 solution with a pH value of 10.5 to 11.5 for 2 to 2.5 hours, washing the prepared electrode with deionized water, drying in the air, then soaking the electrode in a Bi(NO3)3 solution for 0.5 to 1 hour, taking out the electrode, drying in the air, and calcinating the electrode in a muffle furnace for 2 to 2.5 hours so as to obtain the Bi2O3/AgI/TiO2-NTs electrode. The application of the electrode on a chromium-containing wastewater treatment comprises the following steps: adding wastewater containing hexavalent chromium into a reactor taking the Bi2O3/AgI/TiO2-NTs electrode as the work electrode and Pt as the counter electrode, adjusting the reaction pH value by using an inorganic acid, stirring in the absence of light so as to ensure the absorption balance on the electrodes, applying a work voltage, and starting a light source to irradiate the system so as to carry out reactions. A photocatalytic electrode responding to visible lights is utilized, at the same time a certain amount of anode deflecting voltage is applied on the electrode so as to treat Cr(VI) through a photoelectric synergetic effect, and the treatment has the advantages of good treatment effect, rapid speed, and low cost.

Description

The application of a kind of visible light responsible photocatalytic electrode and processing waste water containing chrome thereof
Technical field
The present invention relates to high-level oxidation technology and water-treatment technology field, be specifically related to utilize a kind of visible light responsible photocatalytic electrode B i 2o 3/ AgI/TiO 2-NTs carries out the method for photoelectrocatalysis processing to chromate waste water.
Background technology
Heavy metal chromium Cr (VI) is the common pollution components in plating, process hides and dyeing waste water, has stronger teratogenecity and carinogenicity, is one of 129 kinds of generally acknowledged priority pollutants of USEPA, China's priority control object especially.At present, the thinking of administering for pollution of chromium is that solubility is good, easily migration, and it is little 100 times and be easy to the trivalent chromium Cr (III) of coordination precipitation that highly toxic sexavalent chrome Cr (VI) is reduced to toxicity.
Photoelectrocatalysis technology is as emerging advanced treatment of wastewater technology, with photocatalysis technology comparatively speaking, have the following advantages: played on the one hand the effect of support of the catalyst due to electrode, can effectively avoid like this separation of catalyzer, thereby improved the repeating utilization factor of catalyzer; On the other hand, light induced electron towards the direction motion to electrode, has reduced electron-hole pair recombination rate under the effect of additional anodic bias, has extended the life-span in hole, thereby has greatly improved the degradation efficiency of catalyzer to organic pollutant.
With titanium dioxide (TiO 2) be the photocatalyst of representative, can not only the most organic pollutant of oxidative degradation can also deoxidization, degradation heavy metal.But due to TiO 2be a kind of wide bandgap semiconductor, its energy gap is 3.2eV, only the UV-light in sunlight is responded, and solar energy utilization ratio is low.Therefore, be necessary TiO 2carry out doping vario-property, to promote its response to visible ray.In addition, than TiO 2nano particle, has the TiO of two-dirnentional structure 2nanotube has higher specific surface area and cell container, is more suitable for being applied to photoelectrocatalysis field.
Silver halide (AgX, X:Br, I) is widely used in filmstrip as the good sensitive materials of one, has very high light sensitivity in visible region, can produce light induced electron-hole pair the same as conductor photocatalysis under radiation of visible light.But, because being shown in light, AgX is easily decomposed into argent, be difficult to be used alone as photocatalyst.Bi 2o 3be another important narrow gap semiconductor (2.58eV), have visible light-responded preferably.But the recombination probability in the light induced electron producing after excited by visible light and hole is very high, Bi 2o 3visible light catalysis activity still can not meet the requirement of practical application, be further improved.
Summary of the invention
The invention provides the application of a kind of visible light responsible photocatalytic electrode and processing waste water containing chrome thereof, utilize a kind of visible light-responded photochemical catalyst electrode, additional certain anode deflecting voltage simultaneously, be used for chromium Cr (VI) to process by photoelectric-synergetic, treatment effect is good, speed is fast, and cost is low.
A kind of visible light responsible photocatalytic electrode, by the following method preparation:
By TiO 2-NTs electrode impregnated in KI solution 2～2.5 hours, impregnated in pH value again and be 10.5～11.5 AgNO after taking-up 3in solution 2～2.5 hours, by deionized water rinsing air-dry for the sample making, then be soaked in Bi (NO 3) 3in solution 0.5～1 hour, take out after air-dry and in retort furnace, calcine 2～2.5 hours, make Bi 2o 3/ AgI/TiO 2-NTs electrode.
The present invention is by Bi 2o 3, AgI, TiO 2-NTs three is combined together, with TiO 2-NTs is substrate, passes through Bi 2o 3with the modified synergic of AgI, under biased assisting, can maximize favourable factors and minimize unfavourable ones outside, significantly promote the utilization ratio of visible ray, suppress electron-hole compound, improve the stability of AgI, and then significantly promote photocatalysis performance.
The present invention utilizes Bi 2o 3/ AgI/TiO 2the performance that the visible light-responded and electronics of-NTs electrode transmits, Bi 2o 3act synergistically with AgI, photogenerated charge is more easily separated, be equipped with certain voltage inhibition light induced electron and hole to compound, sexavalent chrome Cr (VI) in water body is reduced to the trivalent chromium Cr (III) that toxicity is little 100 times, be easy to coordination precipitation by photoelectric-synergetic.
Described Bi 2o 3/ AgI/TiO 2-NTs electrode is the TiO that utilizes AgI nanometer particle-modified 2nanotube electrode material, and at AgI/TiO 2load Bi on-NTs electrode 2o 3, to TiO 2-NTs electrode has carried out the modification of diversity.
Described TiO 2-NTs electrode is prepared by the following method:
By after the sand papering of Ti sheet, then use successively acetone, dehydrated alcohol and deionized water ultrasonic cleaning 10min.After taking-up is dried, take the Ti sheet through polishing, ultrasonic cleaning as anode, Cu sheet is negative electrode, is containing NaF and Na 2sO 4the aqueous solution in, with constant voltage 20V anodic oxidation certain hour, by the deionized water rinsing, air-dry for sample making, obtain TiO 2-NTs electrode.In the aqueous solution, the content of NaF is 0.5%(mass ratio); The anodised time is 5h.
As preferably, KI and AgNO 3mol ratio be 1:1.
As preferably, the temperature of calcining is 100～500 ℃.More preferably 200～400 ℃, most preferably be 350 ℃.
KI solution and AgNO 3the preferred concentration of solution is 6 × 10 -3mol/L.
Bi (NO 3) 3solution preferred concentration is 1 × 10 -3mol/L～5 × 10 -2mol/L.
As preferably, AgNO 3with Bi (NO 3) 3mol ratio 0.12～6, more preferably 0.24～4, most preferably be 0.5.
Most preferably, described visible light responsible photocatalytic electrode, by the following method preparation:
By TiO 2-NTs electrode impregnated in KI solution 2 hours, impregnated in pH value again and be 11 AgNO after taking-up 3in solution 2 hours, by deionized water rinsing air-dry for the sample making, then be soaked in Bi (NO 3) 3in solution 0.5～1 hour, take out after air-dry and in retort furnace, calcine 2 hours, make Bi 2o 3/ AgI/TiO 2-NTs electrode; KI and AgNO 3mol ratio be 1:1; The temperature of calcining is for being 350 ℃; AgNO 3with Bi (NO 3) 3mol ratio be 0.5.。
The visible light responsible photocatalytic electrode B i being prepared by aforesaid method 2o 3reach best with the synergistic effect of AgI, the treatment effect during for the treatment of chromate waste water is better.
The present invention also provides a kind for the treatment of process of chromate waste water, comprises the steps:
Be equipped with as described in Bi 2o 3/ AgI/TiO 2-NTs electrode is that working electrode, Pt are to adding hexavalent chromium wastewater in the reactor of electrode, and regulates pH value in reaction, in the dark stirs to guarantee adsorption equilibrium on electrode, then adds operating voltage, opens light source and irradiates, and reacts.
As preferably, in described hexavalent chromium wastewater, also add EDTA, in the time of configuration hexavalent chromium wastewater, add.It is 0～1000umol/L that the interpolation of EDTA makes, and EDTA as the trapping agent in hole, within the specific limits, can make the efficiency of photoelectrocatalysis reduction reaction increase in reaction.
As preferably, described containing the chromic concentration 8 × 10 in hexavalent chromium wastewater -5mol/L.
The light source of described visible ray can be xenon lamp or natural light, and as preferably, described light source is the xenon lamp that utilizes spectral filter elimination λ <420nm part.
As preferably, the processing pH value of described waste water is 1～6, more preferably 2～5, be further preferably 2～3; Most preferably be 2.Regulate pH value mineral acid, such as hydrochloric acid etc.
As preferably, described operating voltage is 1～4V, more preferably 2.5V.
As preferably, described stirring is magnetic agitation.
As preferably, the working electrode of telling and be 1～1.5cm to the spacing between electrode, most preferably be 1cm.Electrolytic process is with Na 2sO 4as ionogen.
Core of the present invention is the photo catalytic reduction system of visible ray-catalysis electrode-additional anodic bias combination.Under the irradiation of visible ray, utilize Bi 2o 3/ AgI/TiO 2the good electronic transmission performance of-NTs electrode, further promoting electron-hole in conjunction with photoelectrocatalysis separates, additional anodic bias can effectively suppress the compound of light induced electron and hole simultaneously, has greatly improved the efficiency that sexavalent chrome Cr (VI) in water is reduced to hypotoxic trivalent chromium Cr (III).Above-mentioned each optimum condition combination under treatment effect better.
Bi used in this treatment process 2o 3/ AgI/TiO 2-NTs electrode performance is stable.Photoelectric-synergetic interaction energy is fast by pollutent reduction, and treatment effect is good, and catalyzer can be recycled in reaction process.Energy consumption is low, can directly utilize sun power, and reaction can be carried out at normal temperatures, saves running cost, and non-secondary pollution, has broad application prospects.
In prior art, make TiO 2the method that-NTs obtains visible light activity has a lot, with semi-conductor (CdS, the Fe of narrow band gap 2o 3, Cu 2o, Bi 2o 3, AgI etc.) compound be one of classical way.For example, have been reported independent Bi 2o 3or AgI modifies TiO 2after-NTs, all can obtain the lifting of visible light catalytic performance, its principle is the Bi of narrow band gap 2o 3or AgI has expanded TiO 2-NTs's is visible light-responded.Based on this, binary/poly modified in theory should be similar with the dosage effect that strengthens independent modifier to the expansion of visible absorption.But excessive narrow gap semiconductor is modified the raising that very easily causes photoproduction-electron-hole recombination rate, suppresses on the contrary photocatalytic activity.That is to say that binary/poly modified differing brings synergistic effect surely, in a lot of situations, there is on the contrary retroaction.But, in the present invention, find the Bi that continuous impregnating legal system is standby 2o 3with AgI binary modification TiO 2-NTs has beyond thought synergy: under the applying bias of 2V, use Bi 2o 3/ AgI/TiO 2hexavalent chromium removal rate constant (0.033min in the reactor of-NTs electrode -1) apparently higher than AgI/TiO 2-NTs (0.008min -1) and Bi 2o 3/ TiO 2-NTs (0.015min -1) removal rate constant sum when electrode.
Accompanying drawing explanation
Fig. 1 is AgI/TiO in the embodiment of the present invention 1 2-NTs, Bi 2o 3/ TiO 2-NTs and Bi 2o 3/ AgI/TiO 2the photoelectric current comparison diagram of-NTs.
Fig. 2 be in the embodiment of the present invention 2 after different temperature lower calcinations Bi 2o 3/ AgI/TiO 2-NTs electrode visible ray current density figure.
Fig. 3 be in the present embodiment 3 different external biasing voltages to Bi 2o 3/ AgI/TiO 2-NTs photoelectric catalysis degrading Cr (VI) affects figure.
Fig. 4 be in the present embodiment 4 different EDTA concentration to Bi 2o 3/ AgI/TiO 2-NTs photoelectric catalysis degrading Cr (VI) affects figure.
Fig. 5 be in the present embodiment 5 different solutions pH to Bi 2o 3/ AgI/TiO 2-NTs photoelectric catalysis degrading Cr (VI) affects figure.
Fig. 6 is Bi in photoelectrocatalysis reduction Cr (VI) process in the present embodiment 6 2o 3/ AgI/TiO 2the recycle efficiency diagram of-NTs electrode
Embodiment
Bi 2o 3/ AgI/TiO 2the making processes of-NTs electrode is as follows:
(1), by after the sand papering of Ti sheet, then use successively acetone, dehydrated alcohol and deionized water ultrasonic cleaning 10min.After taking-up is dried, take the Ti sheet through polishing, ultrasonic cleaning as anode, Cu sheet is negative electrode, is containing NaF and Na 2sO 4the aqueous solution in, with constant voltage 20V anodic oxidation certain hour, by the deionized water rinsing, air-dry for sample making, obtain TiO 2-NTs electrode.
(2) by TiO 2-NTs electrode impregnated in KI solution 2 hours, impregnated in pH value again and be 11 AgNO after taking-up 3in solution 2 hours, by deionized water rinsing air-dry for the sample making, then be soaked in Bi (NO 3) 3in solution 0.5 hour, take out after air-dry and in retort furnace, calcine 2 hours, make Bi 2o 3/ AgI/TiO 2-NTs electrode.
Bi 2o 3/ AgI/TiO 2the process of-NTs electrode processing waste water containing chrome is as follows:
Bi is being housed 2o 3/ AgI/TiO 2-NTs electrode is that working electrode, Pt are to adding hexavalent chromium wastewater in the reactor of electrode, and regulates pH value in reaction with mineral acid, in the dark stirs to guarantee adsorption equilibrium on electrode, then adds operating voltage, opens light source and irradiates, and reacts.
Embodiment 1
At AgI/TiO 2load Bi in the preparation process of-NTs 2o 3, by contrast AgI/TiO 2-NTs, Bi 2o 3/ TiO 2-NTs and Bi 2o 3/ AgI/TiO 2the hexavalent chromium removal rate constant of-NTs, investigates AgI and Bi 2o 3whether there is synergistic effect.
As can be seen from Figure 1, under the applying bias of 2V, use Bi 2o 3/ AgI/TiO 2hexavalent chromium removal rate constant in the reactor of-NTs electrode is apparently higher than AgI/TiO 2-NTs and Bi 2o 3/ TiO 2removal rate constant sum when-NTs electrode.Visible, for TiO 2the diversification modification of-NTs electrode can improve catalytic efficiency, Bi 2o 3obvious with the synergistic effect of AgI, photogenerated charge is more easily separated.
Embodiment 2
Research calcining temperature is processed Bi 2o 3/ AgI/TiO 2the impact of-NTs (λ ﹥ 420nm) photoelectric catalysis degrading Cr (VI) under visible ray is that 3, Cr (VI) concentration is 8 × 10 at pH -5under the reaction conditions of mol/L, while proceeding to 70min to reaction, measure being added with through the concentration of Cr (VI) in each reactor of the photocatalyst of 0 ℃, 100 ℃, 200 ℃, 350 ℃, 500 ℃ calcination processing respectively.
From Fig. 2, see and do not carry out calcination processing contrast, calcination processing has effectively improved Bi 2o 3/ AgI/TiO 2the PhotoelectrocatalytiPerformance Performance of-NTs, and in the time that maturing temperature is 350 ℃, Bi 2o 3/ AgI/TiO 2-NTs reaches maximum value to the clearance of Cr (VI), best results.
Embodiment 3
Research different bias voltages is to Bi 2o 3/ AgI/TiO 2the impact of-NTs-350 ℃ of (λ ﹥ 420nm) photoelectrocatalysis reduction Cr (VI) under visible ray is that 3, Cr (VI) concentration is 8 × 10 at pH -5under the reaction conditions of mol/L, the applying bias of each reactor is respectively 0.5V, 1V, 1.5V, 2V and 2.5V.In the time that proceeding to 70min, reaction respectively the concentration of Cr (VI) in each reactor is measured.
As can be known from Fig. 3, the concentration of Cr (VI) reduces along with the increase of applying bias, visible applying bias affects one of important factor of photoelectrocatalysis efficiency, and from reasonably inferring, within the specific limits, along with the increase of applying bias, Cr (VI) clearance is in rising trend.
Embodiment 4
Study different EDTA concentration to Bi 2o 3/ AgI/TiO 2the impact of-NTs-350 ℃ of (λ ﹥ 420nm) photoelectric catalysis degrading Cr (VI) under visible ray, is 3 o'clock at pH, additional deflecting voltage 2V, and Cr (VI) concentration is 8 × 10 -5under the reaction conditions of mol/L, in the processing waste water of each reactor, add EDTA, concentration is: 0umol/L, 100umol/L, 500umol/L and 1000umol/L, in the time that reaction proceeds to 40min, measure the concentration of Cr (VI) in each reactor respectively.
As can be known from Fig. 4, EDTA adds the photoelectric reduction speed of reaction that can effectively improve Cr (VI), and along with the increase of EDTA concentration, speed of reaction significantly increases.The trapping agent that act as hole of EDTA in reaction, visible, within the scope of finite concentration, the efficiency of described photoelectrocatalysis reduction Cr (VI) reaction increases with the increase of EDTA concentration.
Embodiment 5
PH is to Bi in research 2o 3/ AgI/TiO 2the impact of-NTs-350 ℃ of (λ ﹥ 420nm) photoelectric catalysis degrading Cr (VI) under visible ray, in Cr (VI) concentration 8 × 10 -5mol/L, under the reaction conditions of external biasing voltage 2V, the pH value 1,2,3,4,5,6 and 7 of each reactor.In the time that reaction proceeds to 70min, respectively the concentration of Cr (VI) in each reactor is measured.
As can be known from Fig. 5, in the time of pH=7, Cr (VI) does not degrade substantially, and along with the reduction of pH, the clearance of Cr (VI) raises gradually, and in the time of pH=2, it is maximum that Cr (VI) clearance reaches, now continuing increases pH value of solution, and the clearance of Cr (VI) reduces on the contrary.Visible, under acidic conditions, be conducive to the carrying out of Cr (VI) reduction reaction, and in the time of pH=2, it is best that Cr (VI) reduction reaction rate reaches.
Embodiment 6
Research Bi 2o 3/ AgI/TiO 2the service life cycle of-NTs-350 ℃, is 3 o'clock at pH, Cr (VI) concentration 8 × 10 -5mol/L, under the reaction conditions of external biasing voltage 2V, same Bi 2o 3/ AgI/TiO 2-NTs-350 ℃ of electrode recycles 6 times.In the time that every secondary response proceeds to 70min, respectively the concentration of Cr (VI) in each reactor is measured.
As can be seen from Figure 6, catalyst recirculation is used after 6 times, and the clearance of Cr (VI) drops to 87% from 91%, and the range of decrease is lower than 5%.Visible, Bi 2o 3/ AgI/TiO 2the service life cycle of-NTs-350 ℃ is good.

Claims (10)

1. a visible light responsible photocatalytic electrode, is characterized in that, by the following method preparation:
By TiO 2-NTs electrode impregnated in KI solution 2～2.5 hours, impregnated in pH value again and be 10.5～11.5 AgNO after taking-up 3in solution 2～2.5 hours, by deionized water rinsing air-dry for the sample making, then be soaked in Bi (NO 3) 3in solution 0.5～1 hour, take out after air-dry and in retort furnace, calcine 2～2.5 hours, make Bi 2o 3/ AgI/TiO 2-NTs electrode.
2. visible light responsible photocatalytic electrode according to claim 1, is characterized in that KI and AgNO 3mol ratio be 1:1.
3. visible light responsible photocatalytic electrode according to claim 1, is characterized in that AgNO 3with Bi (NO 3) 3mol ratio 0.12～6.
4. visible light responsible photocatalytic electrode according to claim 1, is characterized in that, the temperature of calcining is 100～500 ℃.
5. a treatment process for chromate waste water, is characterized in that, comprises the steps:
Bi is as claimed in claim 1 being housed 2o 3/ AgI/TiO 2-NTs electrode is that working electrode, Pt are to adding hexavalent chromium wastewater in the reactor of electrode, and regulates pH value in reaction, in the dark stirs to guarantee adsorption equilibrium on electrode, then adds operating voltage, opens light source and irradiates, and reacts.
6. the treatment process of chromate waste water according to claim 4, is characterized in that, described containing the chromic concentration 8 × 10 in hexavalent chromium wastewater -5mol/L.
7. the treatment process of chromate waste water according to claim 4, is characterized in that, described light source is the xenon lamp that utilizes spectral filter elimination λ <420nm part.
8. the treatment process of chromate waste water according to claim 4, is characterized in that, the processing pH value of waste water is 2～5.
9. the treatment process of chromate waste water according to claim 4, is characterized in that, described operating voltage is 1～4V.
10. the treatment process of chromate waste water according to claim 4, is characterized in that, described stirring is magnetic agitation.
CN201410052110.2A 2014-02-14 2014-02-14 Photocatalytic electrode responding to visible lights and application thereof on chromium-containing wastewater treatment Expired - Fee Related CN103818986B (en)

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