CN106219687A - A kind of method of pollutant in photoelectrocatalysis reduction treatment water body - Google Patents
A kind of method of pollutant in photoelectrocatalysis reduction treatment water body Download PDFInfo
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- CN106219687A CN106219687A CN201610670845.0A CN201610670845A CN106219687A CN 106219687 A CN106219687 A CN 106219687A CN 201610670845 A CN201610670845 A CN 201610670845A CN 106219687 A CN106219687 A CN 106219687A
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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
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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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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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
- C02F2001/46133—Electrodes characterised by the material
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Abstract
The invention discloses a kind of method of pollutant in photoelectrocatalysis reduction treatment water body, aqueous solution containing at least one pollutant is placed in photo electrocatalysis reactor by the present invention, use titanium dioxide nanotube array electrode as photocathode, under the conditions of ultraviolet source irradiation, aqueous solution is carried out photoelectrocatalysis reduction reaction.Pollutant in water body are reduced with the purpose reaching efficient degradation pollutant by the light induced electron that the present invention utilizes photocathode to produce under ultraviolet excitation；Present invention process suitably actual application, and simple to operate.
Description
Technical field
The invention belongs to water treatment field, particularly relate to a kind of utilize the side of pollutant in photoelectrocatalysis reduction treatment water body
Method.
Background technology
Along with modernizing industrial, agriculture etc. fast development, water pollutes increasingly severe, and available water resource is increasingly
Few.Traditional biology, chemical treatment method process means as conventional environmental contaminants, there is obvious technological deficiency, as
Operating environment is required height, and treatment effeciency is low, is easily generated secondary pollution etc..To this end, for different water bodys, as breeding wastewater,
Domestic water, subsoil water, industrial organic waste water etc., the method for wastewater treatment setting up economical and efficient is particularly important.
Photo-electrocatalytic technology is as a kind of replacement scheme of conventional processing technique, it is possible to achieve to a lot of traditional biological, change
Learn a skill the efficient degradation of reluctant pollutant.Applying the widest photo-electrocatalytic technology at present is photoelectrocatalysioxidization oxidization
Technology, this technology utilize the strong oxidizing property in hydroxyl radical free radical that photoelectric action produces and hole by dysoxidizable pollutant oxidation,
Reach the purpose of Non-toxic.
But, remove the research of pollutant in water body currently with photoelectrocatalysis reduction the most less.Aoxidized by water body
The impact of antibacterial etc., in water body, the pollutant load of high-valence state is the highest, is at this moment accomplished by efficient reduction technique and realizes
The degraded of pollutant.Photoelectrocatalysis reduction is to apply a back bias voltage on photocathode, and light induced electron is transferred to electrode surface.
Light induced electron has the strongest reducing power, and some pollutant in water can be by accepting the light induced electron on electrode surface and quilt
Reduction；Particularly with some organic reduction, can avoid producing the intermediate that toxicity is more higher than parent, and reduzate also may be used
Reclaim the reaction raw materials as some synthetic reaction to be used.Such as nitrite and bromate, the reduction in photocathode side is such as
Following formula (1)-(4).
TiO2/Ti+hν→ecb -+hνb + (1)
NO2 -+8H++6ecb -→NH4 ++2H2O (2)
NO2 -+4H++3ecb -→1/2N2+2H2O (3)
BrO3 -+3H2O+6ecb -→Br-+6OH- (4)
The patent of invention of " method utilizing the pollutant of photoelectrocatalysioxidization oxidization removing aqueous solution " of T P Barry application
(application number 201180068282.3) proposes photoelectrocatalysioxidization oxidization method to organism, organic chemicals, non-nitrogen inorganic chemical etc.
Removal, but its TiO used2Electrode is light anode, mainly reaches the purpose to pollutant removal by oxidation reaction.With
The titanium dioxide nanotube electrode that this method uses has difference substantially as photocathode, the reduction that this method is occurred
Reaction is in photocathode side.Patent of invention (the application of " a kind of method for the treatment of industrial waste water by means of photoelectrocatalysis " of clear application in Liu
Numbers 201010157248.0) propose to use TiO2Nano-pipe array thin film removes industrial wastewater as photocathode or photo cathode
Organic substance or heavy metal ion, but its described bias is positive bias, completely different with the back bias voltage that this method is used.Health
In the alizarin research using photoelectrocatalysis reduction perchlorate, its described principle is also by TiO2Nanometer pipe array electrode is as photoelectricity
Anode, light induced electron is transferred to negative electrode generation reduction reaction (Kang Qian .TiO2The modification of nanotube and electricity thereof help photo catalytic reduction high
The research [D] of chlorate. Harbin Institute of Technology, 2013).Up to the present, employing TiO is found no2Nano-tube array electricity
Pole or the TiO containing adulterant2Nanometer pipe array electrode is cloudy at photoelectricity as the reduction reaction of photocathode and degradation of contaminant
The correlation technique report that side, pole occurs.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of photoelectrocatalysis reduction treatment water body pollutes
The method of thing.
It is an object of the invention to be achieved through the following technical solutions, a kind of photoelectrocatalysis reduction treatment water body pollutes
The method of thing, adds the aqueous solution containing pollutant in photo electrocatalysis reactor, uses titanium dioxide nanotube array electrode
As photocathode, reaction electrode system is two electrodes or three electrodes, and photocathode is in ultraviolet source or radiation of visible light condition
Under, produce pollutant in Pair production aqueous solution and carry out photoelectrocatalysis reduction.
Further: described pollutant be nitrite, nitrate, perchlorate, bromate, 2,2 ', 4,4 ', 6-pentabromo-
Biphenyl Ether, 2,2 ', 4,4 '-tetrabromo Biphenyl Ether, 4-chlorophenol, 2,4,5-trichlorine (bromine) phenol, o-bromophenol, 2,4 dichloro benzene
In phenol, onitrophenol, paranitrophenol, metanitrophenol, 2,4-dinitrophenol,DNP, 2,4,6-trinitrophenol at least one
Kind.
Further: described titanium dioxide nanotube array electrode uses anodizing process Ti electrode surface and pass through
Muffle furnace the high temperature anneal obtains, and anodic oxidation voltage scope is 15V～100V, and annealing region is 350 DEG C～650
DEG C, titania nanotube crystal formation is Detitanium-ore-type, rutile-type or the two mixing crystal formation.
Further: the adulterant of described titanium dioxide nanotube array electrode is Ag, Pt, Ni, Au, Fe, Ru, Rh, Pd,
One or more in Ir, Co, Mg, Cr, Cu, Bi, N, P, C, adulterant and titanium dioxide mass ratio are 0.1%～10%.
Further: described two electrodes are by the titanium dioxide nanotube array electrode as photocathode with as to electrode
Platinum electrode, graphite electrode, any one electrode composition in Ti electrode, described three electrodes in addition to including above-mentioned two electrode systems,
Also include reference electrode.
Further: described two electrodes are connected with regulated power supply, described three electrodes and electrochemistry potentiostat or electrochemistry
Work station is connected, and the voltage range being applied on photocathode is-10.0V～-0.1V.
Further: in described ultraviolet source is placed in solution or outside solution, be distributed in around photocathode, ultraviolet wavelength model
Enclose is 200～400nm.
Further: photo electrocatalysis reactor is single chamber reactor or two-compartment reactor, single chamber reactor is static streaming
Reactor or circulation flow reactor；Two-compartment reactor comprises cathode chamber and anode chamber, with PEM or salt between two Room
Bridge is connected.
Further: during reaction, in single-chamber photoelectric catalytic reactor or the photocathode room of dual chamber is passed through N2Or Ar, with
Remove the dissolved oxygen in reacting solution.
The invention has the beneficial effects as follows:
1, by photoelectrocatalysis, substantial amounts of light induced electron is produced, by efficient for pollutant in water body deoxidization, degradation.
2, the existing big specific surface area of titanium dioxide nano-pipe array thin film used, has again consolidate good with Titanium base
Qualitative, difficult drop-off, good stability.
3, floor space of the present invention is little, and operating procedure is simple, and environment does not produce secondary pollution.
4, for some organic reduction, minimum valence state reduzate can be directly generated, can avoid producing toxicity than mother
The intermediate that body is higher.
Accompanying drawing explanation
Fig. 1 is the result figure of static streaming single chamber reactor photoelectrocatalysis reduction nitrite solution；
Fig. 2 is the result figure of circulation streaming single chamber reactor photoelectrocatalysis reduction nitrite solution；
Fig. 3 is the result figure of two-compartment reactor photoelectrocatalysis reduction bromate solution.
Detailed description of the invention
The present invention provides a kind of method of pollutant in photoelectrocatalysis reduction treatment water body, adds in photo electrocatalysis reactor
Entering the aqueous solution containing pollutant, use titanium dioxide nanotube array electrode as photocathode, photocathode is at ultraviolet light
Under the conditions of source is irradiated, produce pollutant in Pair production aqueous solution and carry out photoelectrocatalysis reduction.
Described pollutant be nitrite, nitrate, perchlorate, bromate, 2,2 ', 4,4 ', 6-pentabromo-Biphenyl Ether, 2,
2 ', 4,4 '-tetrabromo Biphenyl Ether, 4-chlorophenol, 2,4,5-trichlorine (bromine) phenol, o-bromophenol, 2,4 dichloro phenol, ortho-nitrophenyl
At least one in phenol, paranitrophenol, metanitrophenol, 2,4-dinitrophenol,DNP, 2,4,6-trinitrophenol.
Described titanium dioxide nanotube array electrode uses anodizing to process Ti electrode surface and through Muffle furnace height
Temperature annealing obtains, and oxidation voltage range is 15V～100V, and annealing region is 350 DEG C～650 DEG C, and titanium dioxide is received
Mitron crystal formation is Detitanium-ore-type, rutile-type or the two mixing crystal formation.The adulterant of described titanium dioxide nanotube array electrode
For one or more in Ag, Pt, Ni, Au, Fe, Ru, Rh, Pd, Ir, Co, Mg, Cr, Cu, Bi, N, P, C, adulterant and dioxy
Changing titanium mass ratio is 0.1%～10%.
Described two electrodes by as photocathode titanium dioxide nanotube array electrode and as to the platinum electrode of electrode,
Any one electrode composition in graphite electrode, Ti electrode, described three electrodes, in addition to including above-mentioned two electrodes, also include reference electricity
Pole.Described two electrodes are connected with regulated power supply, and described three electrodes are connected with electrochemistry potentiostat or electrochemical workstation, apply
Voltage range on photocathode is-10.0V～-0.1V.
Described ultraviolet source is placed in solution or outside solution, is distributed in around photocathode, UV wavelength range be 200～
400nm.Photo electrocatalysis reactor is single chamber reactor or two-compartment reactor, and single chamber reactor is static flow reactor or circulation
Flow reactor；Two-compartment reactor comprises cathode chamber and anode chamber, is connected with PEM or salt bridge between two Room.Reaction
Time, in single-chamber photoelectric catalytic reactor or the photocathode room of dual chamber is passed through N2Or Ar, molten with remove in reacting solution
Oxygen.
Being described further the present invention below by example, certainly, the present invention is not limited only to following embodiment.
Embodiment 1:
By titanium sheet (purity 99.6%) successively through mechanical grinding, chemical polishing, acetone, ethanol, deionized water are the most ultrasonic
Washing 10min；Electrochemical oxidation, condition is: platinum electrode is negative electrode, and the solution containing ammonium fluoride 0.15mol/L glycerol 10% is
Electrolyte, voltage 30.5V, oxidization time 50h；Muffle furnace heat treatment, condition is: 450 DEG C, 30min.Prepare by the method
Titanium dioxide nanotube array electrode as working electrode process initial concentration be the nitrite solution of 5mg/L, platinum electrode
For to electrode, Ag/AgCl electrode is reference electrode, uses two-compartment reactor, connects, always with salt bridge between cathode chamber and anode chamber
Volume 100mL, electrolyte is the NaCl of 0.4g/L, applies voltage-0.2V, and uviol lamp power is 80W, after reaction 60min, nitrous
Hydrochlorate degradation rate is 86%, as shown in a curve in Fig. 1.
Embodiment 2:
The titanium dioxide nanotube array electrode using example 1 to prepare processes above-mentioned initial concentration as working electrode
Nitrite solution, on above-mentioned conditioned basic, is passed through N in reactor2, after reaction 6min, as shown in b curve in Fig. 1, sub-
Nitrate removal rate reaches 100%, and the product of 93% is N2, the nitrite of only 7% is reduced to ammonia nitrogen.
Embodiment 3:
By titanium sheet (purity 99.9%) successively through sand papering, chemical polishing, the supersound washing respectively of ethanol, deionized water
10min；Anodizing condition is: graphite is negative electrode, and the solution containing 0.2wt%HF is electrolyte, voltage 20V, oxidization time
30min, 25 DEG C；Muffle furnace heat treatment condition is: 500 DEG C, 1h.Using the titanium dioxide nanotube array electrode for preparing as work
Make the nitrite solution (in terms of N) that Electrode treatment initial concentration is 5mg/L, use single chamber to circulate reactor, reative cell
Liquor capacity is 2L, and mixing chamber liquor capacity is 1L, and electrolyte is the NaCl of 0.4g/L, and applying voltage is-0.2V, uviol lamp merit
Rate is 125W, reacts 90min, and nitrite clearance is 47%, as in figure 2 it is shown, nitrous in photoelectric catalysis degrading circulating water body
Hydrochlorate also has good effect, represents preferable application prospect on circulating water cultivation water body processes.
Embodiment 4:
The titanium dioxide that the titanium dioxide nanotube array electrode using example 4 to prepare will prepare as photocathode
Nanometer pipe array electrode processes as photocathode and is dissolved in the bromate solution that initial concentration is 25mg/L, uses dual chamber reaction
Device, separates with perfluorinated sulfonic acid ion exchange membrane between cathode chamber and anode chamber, and electrolyte is the NaCl solution of 0.4g/L, applies electricity
Pressure-0.2V, uviol lamp power is 500W, and after reaction 75min, bromate concentration reduces by 70%.It addition, photoelectrocatalysis deoxidization, degradation
Bromate effect compares with photodissociation, photocatalysis effect, as it is shown on figure 3, photoelectric catalysis degrading bromate has good
Effect, and degradation effect is apparently higher than direct photocatalysis and electro-catalysis.
Above-described embodiment be used for illustrate the present invention rather than limit the invention, the present invention spirit and
In scope of the claims, any modifications and changes that the present invention is made, both fall within protection scope of the present invention.
Claims (9)
1. the method for pollutant in a photoelectrocatalysis reduction treatment water body, it is characterised in that: add in photo electrocatalysis reactor
Entering the aqueous solution containing pollutant, use titanium dioxide nanotube array electrode as photocathode, reaction electrode system is two
Electrode or three electrodes, photocathode, under ultraviolet source or radiation of visible light, produces pollutant in Pair production aqueous solution and enters
Row photoelectrocatalysis reduction.
The method of pollutant in a kind of photoelectrocatalysis reduction treatment water body the most according to claim 1, it is characterised in that: institute
State pollutant be nitrite, nitrate, perchlorate, bromate, 2,2 ', 4,4 ', 6-pentabromo-Biphenyl Ether, 2,2 ', 4,4 '-four
Bromo biphenyl ether, 4-chlorophenol, 2,4,5-trichlorine (bromine) phenol, o-bromophenol, 2,4 dichloro phenol, onitrophenol, to nitro
At least one in phenol, metanitrophenol, 2,4-dinitrophenol,DNP, 2,4,6-trinitrophenol etc..
The method of pollutant in a kind of photoelectrocatalysis reduction treatment water body the most according to claim 1, it is characterised in that: institute
Stating titanium dioxide nanotube array electrode uses anodizing to process Ti electrode surface and through Muffle furnace the high temperature anneal
Obtaining, anodic oxidation voltage scope is about 15V～100V, and annealing region is about 350 DEG C～650 DEG C, nano titania
Pipe crystal formation is Detitanium-ore-type, rutile-type or the two mixing crystal formation.
The method of pollutant in a kind of photoelectrocatalysis reduction treatment water body the most according to claim 3, it is characterised in that: institute
The adulterant stating titanium dioxide nanotube array electrode is Ag, Pt, Ni, Au, Fe, Ru, Rh, Pd, Ir, Co, Mg, Cr, Cu, Bi,
One or more in N, P, C, adulterant and titanium dioxide mass ratio are about 0.1%～10%.
The method of pollutant in a kind of photoelectrocatalysis reduction treatment water body the most according to claim 1, it is characterised in that: institute
State two electrodes by as photocathode titanium dioxide nanotube array electrode and as to the platinum electrode of electrode, graphite electrode,
Any one electrode composition in Ti electrode, described three electrodes, in addition to including above-mentioned two electrodes, also include reference electrode.
The method of pollutant in a kind of photoelectrocatalysis reduction treatment water body the most according to claim 5, it is characterised in that: institute
Stating two electrodes to be connected with regulated power supply, described three electrodes are connected with electrochemistry potentiostat or electrochemical workstation, are applied to light
Voltage range on electricity negative electrode is-10.0V～-0.1V.
The method of pollutant in a kind of photoelectrocatalysis reduction treatment water body the most according to claim 1, it is characterised in that: institute
Stating in ultraviolet source is placed in solution or outside solution, be distributed in around photocathode, UV wavelength range is 200～400nm.
The method of pollutant in a kind of photoelectrocatalysis reduction treatment water body the most according to claim 1, it is characterised in that: light
Electric catalysis reactor is single chamber reactor or two-compartment reactor, and single chamber reactor is static flow reactor or circulation streaming reaction
Device, two-compartment reactor comprises cathode chamber and anode chamber, is connected with PEM or salt bridge between two Room.
The method of pollutant in a kind of photoelectrocatalysis reduction treatment water body the most according to claim 8, it is characterised in that: anti-
At once, it is passed through N in photoelectrocatalysis single chamber reactor or in the cathode chamber of dual chamber2Or Ar, molten with remove in reacting solution
Oxygen.
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Cited By (22)
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| CN107138111A (en) * | 2017-05-23 | 2017-09-08 | 郑州轻工业学院 | A kind of carbon dioxide catalytic reduction reaction device |
| CN108275811A (en) * | 2018-01-10 | 2018-07-13 | 东北石油大学 | A method of passing through the hot THM coupling degradation of organic waste water of optical-electronic-using solar energy |
| CN108445054A (en) * | 2018-03-07 | 2018-08-24 | 武汉理工大学 | Nano tube array of titanium dioxide BOD sensors and its preparation method and application |
| CN108793342A (en) * | 2018-07-03 | 2018-11-13 | 青岛理工大学 | Preparation method of high-dispersion cobalt-titanium composite nano electrode for reducing nitrate nitrogen in water |
| CN109867333A (en) * | 2019-04-01 | 2019-06-11 | 中国科学院生态环境研究中心 | The method with uranium in recycle-water is efficiently removed using titanium-based titanium dioxide nanotube array electrode |
| CN109942076A (en) * | 2019-04-01 | 2019-06-28 | 中国科学院生态环境研究中心 | Utilize the method for uranium in microbiological fuel cell removal-recycle-water and synchronous electrogenesis |
| CN109939674A (en) * | 2019-04-25 | 2019-06-28 | 重庆工商大学 | A kind of Pd/TiO with Schottky hetero-junctions2Elctro-catalyst and its preparation and application |
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| CN107138111B (en) * | 2017-05-23 | 2019-02-22 | 郑州轻工业学院 | A kind of carbon dioxide catalytic reduction reaction device |
| CN107138111A (en) * | 2017-05-23 | 2017-09-08 | 郑州轻工业学院 | A kind of carbon dioxide catalytic reduction reaction device |
| CN108275811A (en) * | 2018-01-10 | 2018-07-13 | 东北石油大学 | A method of passing through the hot THM coupling degradation of organic waste water of optical-electronic-using solar energy |
| CN108275811B (en) * | 2018-01-10 | 2021-02-09 | 东北石油大学 | Method for degrading organic wastewater by solar energy through photo-electric-thermal three-field coupling |
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| CN109867333A (en) * | 2019-04-01 | 2019-06-11 | 中国科学院生态环境研究中心 | The method with uranium in recycle-water is efficiently removed using titanium-based titanium dioxide nanotube array electrode |
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