CN110228839A - A kind of efficient Atrazine photoelectrocatalysis reduction minimizing technology - Google Patents
A kind of efficient Atrazine photoelectrocatalysis reduction minimizing technology Download PDFInfo
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- CN110228839A CN110228839A CN201910542844.1A CN201910542844A CN110228839A CN 110228839 A CN110228839 A CN 110228839A CN 201910542844 A CN201910542844 A CN 201910542844A CN 110228839 A CN110228839 A CN 110228839A
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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
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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
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
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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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- 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
- C02F2101/305—Endocrine disruptive agents
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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
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4612—Controlling or monitoring
- C02F2201/46125—Electrical variables
- C02F2201/46135—Voltage
Abstract
The present invention relates to a kind of efficient Atrazine photoelectrocatalysis to restore minimizing technology, with PdQDs@TiO2NTs is to electrode as work cathode, Pt piece, and saturated calomel electrode is reference electrode, and building three-electrode system carries out photoelectrocatalysis reduction treatment to Atrazine solution, realizes and restores removal to the photoelectrocatalysis of Atrazine in solution.Compared with prior art, the efficient photoelectricity treater catalysis reduction and removing of Atrazine can be achieved in the present invention.
Description
Technical field
The invention belongs to photo-electrocatalytic technology fields, are related to a kind of efficient Atrazine photoelectrocatalysis reduction removal side
Method.
Background technique
Atrazine (the chloro- 4- ethamine -6- isopropylamine -1,3,5-triazines of 2-), is a kind of triazine derivative.It is to water
Middle biology has strong toxicity, has significant effect to the reproductive function of animal, is listed in incretion interferent.And Atrazine
Molecule contains heterocycle structure, and stability is strong, the residence time is long and is difficult biodegrade, and chlorine atom takes especially on triazine ring
In generation, further increases the fat-soluble of Atrazine molecule, inoxidizability and toxicity, and in water body, the continuous of Atrazine is tired out
Product, environmental problem occur and get worse therewith, thus the Atrazine in efficient removal water body is particularly necessary.
Photo-electrocatalytic technology inhibits light induced electron and sky compared with single photocatalysis technology, by applying certain bias
Compound, the raising photocatalytic activity in cave, and then improve the efficiency of photoelectrocatalysis removal pollutant.Currently, most of application
It concentrates on the hole generated using photo cathode surface and hydroxyl radical free radical realizes the photoelectrocatalysioxidization oxidization of pollutant, and for inciting somebody to action
Optoelectronic pole is as cathode, using the strong reducing property of light induced electron, to realize pollutant, and the light for the organic pollutant that especially (contains chlorine)
The application of electro-catalysis reduction removal is also fewer, less especially in terms of the removal of organic pollutant.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of efficient Aunars to draw
Saliva photoelectrocatalysis restores minimizing technology.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of efficient Atrazine photoelectrocatalysis reduction minimizing technology, with PdQDs@TiO2NTs is as work cathode, Pt
Piece is to electrode, and saturated calomel electrode is reference electrode, and building three-electrode system carries out photoelectrocatalysis also to Atrazine solution
Original place reason is realized and restores removal to the photoelectrocatalysis of Atrazine in solution.
Further, the PdQDs@TiO2NTs electrode is prepared by the following method:
(1) NH is weighed4F is dissolved in the mixed solution of water and ethylene glycol, is stirred evenly, and NH is obtained4F ethylene glycol solution is spare；
(2) take two blocks of Ti plates cleaned up of polishing respectively as anode and cathode, with NH4F ethylene glycol solution is as electricity
Liquid is solved, anodization three times is carried out, removes first secondly, first removing anode surface oxidation film every time before anodization；
(3) it by the electrode (i.e. anode) after anodization three times, cleans and dries up, then calcination processing is to get arriving
TiO2NTs electrode；
(4) weigh polyvinylpyrrolidone, palladium chloride and sodium iodide mixing be made into mixed aqueous solution after, be transferred to reaction kettle
In, by TiO2NTs electrode, which is placed in mixed aqueous solution, carries out hydro-thermal reaction, after the reaction was completed, takes out cooling, washing, drying, i.e.,
Obtain PdQDs@TiO2NTs electrode.
Further, in step (1), NH4The concrete composition of F ethylene glycol solution are as follows: with 1.7g NH4F meter, corresponding water
For 10mL, corresponding ethylene glycol is 500mL.
Further, in step (2), anodized condition is respectively as follows: anodized electricity for the first time three times
Pressure is 40-80V, time 2-4h；Second of anodized voltage is 20-40V, time 0.5-1.5h；Second of sun
The voltage of polarization process is 20-40V, time 0.5-1.5h.
Further, in step (2), the distance between cathode and anode are 1cm.
Further, in step (3), calcination condition specifically: under air atmosphere, room temperature keeps 5-15min, setting
Heating rate is 3-7 DEG C/min, and 2-4h, subsequent cooled to room temperature are calcined at 500-600 DEG C.Further, step
(4) in, in mixed aqueous solution, the mass ratio of polyvinylpyrrolidone, palladium chloride and sodium iodide is (600-1000): (6-12):
(200-400)。
Further, in step (4), the condition of hydro-thermal reaction are as follows: temperature is 100-300 DEG C, time 0.5-3h.
Further, in photoelectrocatalysis reduction treatment process, excitation light source uses optical power density for 150-250mW/cm2
Xenon lamp, with equipped with Atrazine solution degraded pond at a distance from be 20cm.
Further, PdQDs@TiO2The distance between NTs electrode and Pt piece are 1-2cm.
Further, in photoelectrocatalysis reduction treatment process, the bias of application is -1.5~-0.5V.
Further, when photoelectrocatalysis reduction treatment, degradation solution is the Atrazine solution of 2ppm, wherein comprising supporting electricity
The Na of Xie Zhiwei 0.1mol/L2SO4Solution.Take the initial Atrazine solution to be degraded of 40mL.
Further, when photoelectrocatalysis reduction treatment, before degrading, N is passed through into system with the flow velocity of 25L/min2
Half an hour, to exclude the interference of oxygen；Simultaneously under dark condition by electrode impregnate in the solution 30min to reach Ah to be degraded
The adsorption equilibrium of Te Lajin on the electrode.
Also to PdQDs@TiO in the present invention2Electrolyte composition in the preparation process of NTs electrode, anodization number,
Process conditions (voltage, anodising time etc.), calcine technology, hydro-thermal reaction technique etc. have carried out specific restriction.In TiO2NTs
In the preparation process of electrode, in a certain range, voltage is higher, electrolyte F-Concentration it is bigger, obtained pipe in preparation process
Diameter is also bigger, and shows relatively smooth smooth electrode surface pattern, but with the increase of anodising time, tube wall by
It gradually dissolves thinning.Multistep anodization can be in TiO2The surface NTs forms one layer of reticular structure, to improve the ratio table of catalyst
Area improves catalytic performance.In addition, in certain temperature range, with the increase of electrode calcination temperature, Anatase TiO2Knot
Brilliant degree is better, and Rutile Type TiO2It gradually increases, mixed crystal phase TiO2NTs electrode is conducive to the formation of homojunction, promotes photoproduction
The separation of carrier, thus there is better photoelectric catalytically active.In Hydrothermal Growth PdQDs, polyvinylpyrrolidone
Amount is excessive, and the hydro-thermal reaction time is too long, temperature is excessively high, PdQDs can be made to reunite, and causes particle excessive, to influence the biography of electronics
It is defeated；The amount of polyvinylpyrrolidone is very few, and the hydro-thermal time is too short, temperature is too low, and PdQDs deposition can be made very few, photoelectricity is caused to be urged
Changing reduction efficiency reduces.
In the present invention, using photoelectrocatalysis reduction technique as technical way, applied on the working electrode (s by adjusting
Cathode bias size, realize water body in low concentration high toxicity organic pollutant efficient removal.
Compared with prior art, the invention has the following advantages that
(1) present invention is prepared for PdQDs@TiO using three step anodizing of electrochemistry and simple hydro-thermal method2NTs light
Cathode, TiO2The tubular structure of NTs electrode surface can increase the specific surface area of catalyst, enhance pollutant in catalyst surface
Absorption, the upright nano tube structure under cavernous structure is conducive to the quick transmission of charge, improves photoelectrocatalysis efficiency；PdQDs
Modification, be conducive to enhancing and promote the separation in light induced electron and hole and the reduction of Atrazine, to effectively improve photoelectricity
The efficiency of catalysis reduction Atrazine.
(2) PdQDs@TiO used in the present invention2NTs photocathode preparation method is simple, and photoelectric catalytically active is high, chemistry
It has good stability, it is recyclable, it is not easy to secondary pollution to be caused, in energy such as the photoelectrocatalysis reduction and dechlorination of pollutant
Source and environmental area have potential application.
(3) by adjusting PdQDs@TiO in the present invention2The cathode potential applied on NTs electrode obtains optimal Aunar and draws
The photoelectric reduction removal efficiency of saliva.The result shows that the photoelectrocatalysis of Atrazine is also under the conditions of bias is -1.3V vs.SCE
Former efficiency, which reaches, is up to 99.5%, and dechlorination efficiency basically reaches 100%.
(4) chlorine atom in Atrazine molecule has strong electronegativity and electron-withdrawing ability, so as to cause heterocycle structure
Upper cloud density decline, thus it is difficult to happen oxidation reaction, and it is easy to happen reduction reaction.The present invention uses photoelectrocatalysis also
Former method removes Atrazine.For the molecular structure feature of Atrazine, compared to Traditional photovoltaic catalysed oxidation processes, light
The method of electro-catalysis reduction is more advantageous to the raising of Atrazine mineralization rate.
Detailed description of the invention
Fig. 1 is PdQDs@TiO2The scanning electron microscope (SEM) photograph (SEM) of NTs electrode；
Fig. 2 is PdQDs@TiO2The X-ray diffracting spectrum (XRD) of NTs electrode.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to
Following embodiments.
In following embodiment, unless otherwise instructed, then raw material used by showing or processing technique are this field
Conventional commercial product or Technology development.
Embodiment 1
PdQDs@TiO2The preparation of NTs electrode:
By 1.5 × 2.5cm2Ti plate to be polishing to its surface smooth and clean up, respectively in deionized water, acetone, second
Each ultrasound 15min in alcohol.Accurately weigh 1.7g NH4F is dissolved in the mixed solution of 10mL water and 500mL ethylene glycol.It will polish clear
Ti plate (1.5 × 2.5cm of wash clean2) and Pt piece be placed in parallel in the electrolyte that 40mL is prepared, electrode spacing 1cm.Entirely
Anodization system carries out in ice-water bath.Anodizing process is carried out by following procedure, first application constant voltage 60V, when anodization
Between be 3h, after first step anodization terminates, the oxidation film of electrode surface is removed by ultrasound；Electrode clean is completely laggard
Row second step anodization applies constant voltage 30V, anodising time 1h, and same ultrasound removes electricity after second step anodization
The oxidation film of pole surface；Third step anodization is carried out after cleaning drying, applies constant potential 30V, anodising time 30min.To
After three step anodization, the electrolyte of electrode surface and drying wash with distilled water.The electrode obtained is placed in tube furnace high
Temperature calcining, setting tube furnace temperature program it is as follows: under air atmosphere, room temperature keep 10min, setting heating rate be 5 DEG C/
Min calcines 3h, subsequent cooled to room temperature at 550 DEG C.
By 800mg polyvinylpyrrolidone (PVP), 9mg palladium chloride (PdCl2) and 300mg sodium iodide (NaI) be configured to
The aqueous solution of 13mL is transferred to after mixing in 23mL polytetrafluoroethylene (PTFE) stainless steel autoclave.The electrode of preparation is set
In mixed solution, hydro-thermal reaction 1.5h under conditions of 200 DEG C of constant temperature.After reaction kettle is cooled to room temperature, takes out electrode and use
Deionized water washs its surface repeatedly, dries up to get PdQDs@TiO is arrived2NTs electrode.Obtained PdQDs@TiO2NTs electrode
Pattern is shown in Figure 1, has been prepared by the above method and has arranged close, high-sequential 1-dimention nano pipe array, caliber
About 45nm, pipe thickness are about 23nm, and length of tube is about 0.58 μm.PdQDs is evenly distributed on tube wall, and size is about 4-
10nm.As shown in Fig. 2, prepared PdQDs@TiO2NTs electrode is anatase and rutile TiO2Duplex grain structure, and simple substance
Pd is successfully supported on electrode surface.
Embodiment 2
It is biased at PdQDs@TiO when -0.5V in addition2NTs electrode photo electrocatalysis restores for Atrazine
By Atrazine solution (concentration 2ppm, Na containing 0.1mol/L to be degraded2SO4Solution) it is placed in single layer quartz face
In the round degraded pond of light transmission, PdQDs@TiO2NTs electrode is to electrode as work cathode, Pt piece, and saturated calomel electrode is
Reference electrode (1.5 × 2.5cm of electrode effective area2), degradation solution volume is 40mL.PdQDs@TiO2Between NTs electrode and Pt piece
Distance be 20cm.Temperature of reaction system is set to maintain 25 DEG C using super constant temperature water tank.Before photoelectrocatalysis reduction starts,
First lead to 30min N in degradation solution2, to remove the O in solution2, and by PdQDs@TiO2NTs electrode is placed in Atrazine solution
Initial concentration C of the middle 30min to reach adsorption equilibrium, using concentration at this time as Atrazine0.Existed by adjusting potentiostat
PdQDs@TiO2Application -0.5V back bias voltage on NTs electrode (moors luxuriant and rich with fragrance Lay PLS-SXW300, optical power density is in xenon source
200mW/cm2) irradiation under, to Atrazine solution carry out photoelectrocatalysis reduction.Sampling interval is 30min, samples taken warp
0.22 μm of water phase syringe filter membrane filtration.With in solution during high performance liquid chromatography (HPLC) instrument measurement photoelectrocatalysis
The concentration of Atrazine changes with time trend.The result shows that when applying bias is -0.5V, the PEC removal of Atrazine
Rate is 24.1%, reaction rate constant 0.06h-1。
Embodiment 3
It is biased at PdQDs@TiO when -0.9V in addition2NTs electrode photo electrocatalysis will be wait drop for restoring Atrazine
Atrazine solution (the concentration 2ppm, Na containing 0.1mol/L of solution2SO4Solution) it is placed in the round degradation of single layer quartz face light transmission
Chi Zhong, PdQDs TiO2NTs electrode is as work cathode, and Pt piece is to electrode, and saturated calomel electrode is that (electrode has reference electrode
Imitate 1.5 × 2.5cm of area2), degradation solution volume is 40mL.PdQDs@TiO2The distance between NTs electrode and Pt piece are 20cm.Benefit
Temperature of reaction system is set to maintain 25 DEG C with super constant temperature water tank.Before photoelectrocatalysis reduction starts, first lead in degradation solution
30min N2, to remove the O in solution2, and by PdQDs@TiO2NTs electrode is placed in 30min in Atrazine solution and is inhaled with reaching
Attached balance, the initial concentration C using concentration at this time as Atrazine0.By adjusting potentiostat in PdQDs@TiO2NTs electricity
Extremely upper application -0.9V back bias voltage (moors luxuriant and rich with fragrance Lay PLS-SXW300, optical power density 200mW/cm in xenon source2) irradiation
Under, photoelectrocatalysis reduction is carried out to Atrazine solution.Sampling interval is 30min, and samples taken is through 0.22 μm of water phase pin type
Filtering membrane of filter filtering.With high performance liquid chromatography (HPLC) instrument measure the concentration of Atrazine in solution during photoelectrocatalysis with
The variation tendency of time.The result shows that the PEC removal rate of Atrazine is 83.9%, reaction when applying bias is -0.9V
Rate constant is 0.33h-1。
Embodiment 4
It is biased at PdQDs@TiO when -1.3V in addition2NTs electrode photo electrocatalysis restores for Atrazine
By Atrazine solution (concentration 2ppm, Na containing 0.1mol/L to be degraded2SO4Solution) it is placed in single layer quartz face
In the round degraded pond of light transmission, PdQDs@TiO2NTs electrode is to electrode as work cathode, Pt piece, and saturated calomel electrode is
Reference electrode (1.5 × 2.5cm of electrode effective area2), degradation solution volume is 40mL.PdQDs@TiO2Between NTs electrode and Pt piece
Distance be 20cm.Temperature of reaction system is set to maintain 25 DEG C using super constant temperature water tank.Before photoelectrocatalysis reduction starts,
First lead to 30min N in degradation solution2, to remove the O in solution2, and by PdQDs@TiO2NTs electrode is placed in Atrazine solution
Initial concentration C of the middle 30min to reach adsorption equilibrium, using concentration at this time as Atrazine0.Existed by adjusting potentiostat
PdQDs@TiO2Application -1.3V back bias voltage on NTs electrode (moors luxuriant and rich with fragrance Lay PLS-SXW300, optical power density is in xenon source
200mW/cm2) irradiation under, to Atrazine solution carry out photoelectrocatalysis reduction.Sampling interval is 30min, samples taken warp
0.22 μm of water phase syringe filter membrane filtration.With in solution during high performance liquid chromatography (HPLC) instrument measurement photoelectrocatalysis
The concentration of Atrazine changes with time trend.The result shows that when applying bias is -1.3V, the PEC removal of Atrazine
Rate is 99.5%, reaction rate constant 1.04h-1。
Embodiment 5
It is biased at PdQDs@TiO when -1.5V in addition2NTs electrode photo electrocatalysis restores for Atrazine
By Atrazine solution (concentration 2ppm, Na containing 0.1mol/L to be degraded2SO4Solution) it is placed in single layer quartz face
In the round degraded pond of light transmission, PdQDs@TiO2NTs electrode is to electrode as work cathode, Pt piece, and saturated calomel electrode is
Reference electrode (1.5 × 2.5cm of electrode effective area2), degradation solution volume is 40mL.PdQDs@TiO2Between NTs electrode and Pt piece
Distance be 20cm.Temperature of reaction system is set to maintain 25 DEG C using super constant temperature water tank.Before photoelectrocatalysis reduction starts,
First lead to 30min N in degradation solution2, to remove the O in solution2, and by PdQDs@TiO2NTs electrode is placed in Atrazine solution
Initial concentration C of the middle 30min to reach adsorption equilibrium, using concentration at this time as Atrazine0.Existed by adjusting potentiostat
PdQDs@TiO2Application -1.5V back bias voltage on NTs electrode (moors luxuriant and rich with fragrance Lay PLS-SXW300, optical power density is in xenon source
200mW/cm2) irradiation under, to Atrazine solution carry out photoelectrocatalysis reduction.Sampling interval is 30min, samples taken warp
0.22 μm of water phase syringe filter membrane filtration.With in solution during high performance liquid chromatography (HPLC) instrument measurement photoelectrocatalysis
The concentration of Atrazine changes with time trend.The result shows that when applying bias is -1.5V, the PEC removal of Atrazine
Rate is 93.4%, reaction rate constant 0.54h-1。
Embodiment 6
Compared with Example 1, the overwhelming majority is all identical, in addition in the present embodiment: anodized condition difference three times
Are as follows: anodized voltage is 40V, time 4h for the first time；Second anodized voltage is 20V, and the time is
1.5h；Second of anodized voltage is 20V, time 1.5h.
Embodiment 7
Compared with Example 1, the overwhelming majority is all identical, in addition in the present embodiment: anodized condition difference three times
Are as follows: anodized voltage is 80V, time 2h for the first time；Second anodized voltage is 40V, and the time is
0.5h；Second of anodized voltage is 40V, time 0.5h.
Embodiment 8
Compared with Example 1, the overwhelming majority is all identical, in addition in the present embodiment: calcination condition specifically: in air atmosphere
Under, room temperature keeps 5min, and setting heating rate is 3 DEG C/min, and 4h, subsequent cooled to room temperature are calcined at 500 DEG C.
Embodiment 9
Compared with Example 1, the overwhelming majority is all identical, in addition in the present embodiment: calcination condition specifically: in air atmosphere
Under, room temperature keeps 15min, and setting heating rate is 7 DEG C/min, and 2h, subsequent cooled to room temperature are calcined at 600 DEG C.
Embodiment 10
Compared with Example 1, the overwhelming majority is all identical, in addition in the present embodiment: polyvinylpyrrolidone, palladium chloride and iodine
The mass ratio for changing sodium is 600:6:200.
Embodiment 11
Compared with Example 1, the overwhelming majority is all identical, in addition in the present embodiment: polyvinylpyrrolidone, palladium chloride and iodine
The mass ratio for changing sodium is 1000:12:400.
Embodiment 12
Compared with Example 1, the overwhelming majority is all identical, in addition in the present embodiment: the condition of hydro-thermal reaction are as follows: temperature is
100 DEG C, time 3h.
Embodiment 13
Compared with Example 1, the overwhelming majority is all identical, in addition in the present embodiment: the condition of hydro-thermal reaction are as follows: temperature is
300 DEG C, time 0.5h.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of efficient Atrazine photoelectrocatalysis restores minimizing technology, which is characterized in that with PdQDs@TiO2NTs is as work
Make cathode, Pt piece is to electrode, and saturated calomel electrode is reference electrode, and building three-electrode system carries out light to Atrazine solution
Electro-catalysis reduction treatment is realized and restores removal to the photoelectrocatalysis of Atrazine in solution.
2. a kind of efficient Atrazine photoelectrocatalysis according to claim 1 restores minimizing technology, which is characterized in that institute
The PdQDs@TiO stated2NTs electrode is prepared by the following method:
(1) NH is weighed4F is dissolved in the mixed solution of water and ethylene glycol, is stirred evenly, and NH is obtained4F ethylene glycol solution is spare；
(2) take two blocks of Ti plates cleaned up of polishing respectively as anode and cathode, with NH4F ethylene glycol solution as electrolyte,
Anodization three times is carried out, removes first secondly, first removing anode surface oxidation film every time before anodization；
(3) electrode after anodization three times is cleaned and is dried up, then calcination processing to get arrive TiO2NTs electrode；
(4) weigh polyvinylpyrrolidone, palladium chloride and sodium iodide mixing be made into mixed aqueous solution after, be transferred in reaction kettle,
By TiO2NTs electrode, which is placed in mixed aqueous solution, carries out hydro-thermal reaction, after the reaction was completed, take out cooling, washing, it is dry to get
To PdQDs@TiO2NTs electrode.
3. a kind of efficient Atrazine photoelectrocatalysis according to claim 2 restores minimizing technology, which is characterized in that step
Suddenly in (1), NH4The concrete composition of F ethylene glycol solution are as follows: with 1.7g NH4F meter, corresponding water are 10mL, and corresponding ethylene glycol is
500mL。
4. a kind of efficient Atrazine photoelectrocatalysis according to claim 2 restores minimizing technology, which is characterized in that step
Suddenly in (2), it is 40-80V, time 2-4h that anodized condition, which is respectively as follows: anodized voltage for the first time, three times；
Second of anodized voltage is 20-40V, time 0.5-1.5h；Second of anodized voltage is 20-40V,
Time is 0.5-1.5h；
The distance between cathode and anode are 1cm.
5. a kind of efficient Atrazine photoelectrocatalysis according to claim 2 restores minimizing technology, which is characterized in that step
Suddenly in (3), calcination condition specifically: under air atmosphere, room temperature keeps 5-15min, and setting heating rate is 3-7 DEG C/min,
2-4h, subsequent cooled to room temperature are calcined at 500-600 DEG C.
6. a kind of efficient Atrazine photoelectrocatalysis according to claim 2 restores minimizing technology, which is characterized in that step
Suddenly in (4), in mixed aqueous solution, the mass ratio of polyvinylpyrrolidone, palladium chloride and sodium iodide is (600-1000): (6-
12): (200-400).
7. a kind of efficient Atrazine photoelectrocatalysis according to claim 2 restores minimizing technology, which is characterized in that step
Suddenly in (4), the condition of hydro-thermal reaction are as follows: temperature is 100-300 DEG C, time 0.5-3h.
8. a kind of efficient Atrazine photoelectrocatalysis according to claim 1 restores minimizing technology, which is characterized in that light
In electro-catalysis reduction treatment process, excitation light source uses optical power density for 150-250mW/cm2Xenon lamp, be equipped with Aunar
The distance for drawing the degraded pond of saliva solution is 20cm.
9. a kind of efficient Atrazine photoelectrocatalysis according to claim 1 restores minimizing technology, which is characterized in that
PdQDs@TiO2The distance between NTs electrode and Pt piece are 1-2cm.
10. a kind of efficient Atrazine photoelectrocatalysis according to claim 1 restores minimizing technology, which is characterized in that
In photoelectrocatalysis reduction treatment process, the bias of application is -1.5~-0.5V.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226284A (en) * | 2011-06-02 | 2011-10-26 | 厦门大学 | Method for performing photoelectrolysis of water and preparing hydrogen by using palladium quantum dot modified titanium dioxide nanotube array |
| CN102658130A (en) * | 2012-04-20 | 2012-09-12 | 大连理工大学 | Preparation method of Ru-Pd bimetal-supported TiO2 nanotube photocatalyst and application thereof |
| CN102744058A (en) * | 2012-03-20 | 2012-10-24 | 南京大学 | Pd/TiO2atCNT catalyst and preparation method thereof |
| CN104492431A (en) * | 2014-12-10 | 2015-04-08 | 青岛农业大学 | Preparation method of Au-Pd/TiO2 NBs photocatalyst |
| CN106219687A (en) * | 2016-08-15 | 2016-12-14 | 浙江大学 | A kind of method of pollutant in photoelectrocatalysis reduction treatment water body |
| CN106277229A (en) * | 2016-10-31 | 2017-01-04 | 淮南师范学院 | A kind of modified electrode electrocatalytic oxidation processes the method for toxic organic pollutant G-30027 |
-
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226284A (en) * | 2011-06-02 | 2011-10-26 | 厦门大学 | Method for performing photoelectrolysis of water and preparing hydrogen by using palladium quantum dot modified titanium dioxide nanotube array |
| CN102744058A (en) * | 2012-03-20 | 2012-10-24 | 南京大学 | Pd/TiO2atCNT catalyst and preparation method thereof |
| CN102658130A (en) * | 2012-04-20 | 2012-09-12 | 大连理工大学 | Preparation method of Ru-Pd bimetal-supported TiO2 nanotube photocatalyst and application thereof |
| CN104492431A (en) * | 2014-12-10 | 2015-04-08 | 青岛农业大学 | Preparation method of Au-Pd/TiO2 NBs photocatalyst |
| CN106219687A (en) * | 2016-08-15 | 2016-12-14 | 浙江大学 | A kind of method of pollutant in photoelectrocatalysis reduction treatment water body |
| CN106277229A (en) * | 2016-10-31 | 2017-01-04 | 淮南师范学院 | A kind of modified electrode electrocatalytic oxidation processes the method for toxic organic pollutant G-30027 |
Non-Patent Citations (2)
| Title |
|---|
| 徐蕾等著: "《负载型多酸光催化材料及应用》", 31 March 2015, 长春：东北师范大学出版社 * |
| 贾金平编著: "《活性炭纤维在环境与能源领域的新应用》", 30 November 2015, 上海：上海交通大学出版社 * |
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