CN105198033A - Method for accelerating photodegradation of citric acid pickling wastewater from power plant boiler - Google Patents

Method for accelerating photodegradation of citric acid pickling wastewater from power plant boiler Download PDF

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CN105198033A
CN105198033A CN201510646654.6A CN201510646654A CN105198033A CN 105198033 A CN105198033 A CN 105198033A CN 201510646654 A CN201510646654 A CN 201510646654A CN 105198033 A CN105198033 A CN 105198033A
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citric acid
power plant
boiler
tio
photodegradation
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CN105198033B (en
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王罗春
熊金磊
李亭
王军建
朱世杰
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Shanghai University of Electric Power
University of Shanghai for Science and Technology
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Shanghai University of Electric Power
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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Abstract

The invention relates to a method for accelerating the photodegradation of citric acid pickling wastewater from a power plant boiler. The method comprises the steps of preparing a TiO2 nanotube array by using an anodic oxidation method; then, preparing a WO3-TiO2 modified TiO2 nanotube array photocatalyst by using a chemical bath deposition method; next, adding citric acid pickling wastewater from the power plant boiler, placing the WO3-TiO2 modified TiO2 nanotube array photocatalyst and a Pt sheet into wastewater, and connecting by using a conducting wire; and carrying out light treatment on the wastewater by virtue of visible light instead of applying external voltage to accelerate the photodegradation of citric acid pickling wastewater from the power plant boiler. Compared with the prior art, the method has the advantages that the problem that photoelectrons are compounded with holes is effectively solved, and the photocatalytic activity of the photocatalyst to the citric acid pickling wastewater from the power plant boiler is greatly improved.

Description

A kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed
Technical field
The present invention relates to photochemical catalysis field, especially relate to a kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed.
Background technology
Energy and environment are the important topics of the relation mankind survival and development always, and the demand of fast development to electric power of industry also increases severely day by day, and the present supply of electric power of China is still based on thermoelectricity.As the integral part of thermal power generation, boiler of power plant every 3 ~ 4 years needs clean once, to improve working efficiency and the work-ing life of boiler.Citric acid is a kind of organic acid soluble in water, because the advantages such as its corrodibility is little, toxicity is little, easy preservation transport are usually for the matting of boiler of power plant.The boiler of power plant citric acid wastewater produced often has extremely strong acidity, COD crbe worth mg/L up to ten thousand.At present, chemical oxidization method, burning method, biochemical process and reverse osmosis is had to the treatment process of this kind of waste water.In these treatment processs, each method is less to be used alone, generally all with other treatment process conbined usage.
Photocatalytic oxidation is a kind of high-level oxidation technology that development in recent years is got up, and is the transmission of a series of photo-generated carriers produced under light illumination by photocatalyst and produces the HO with strong oxidizing property and be oxidized organic pollutant.The advantages such as the method has green, efficient, contaminant degradation is thorough, non-secondary pollution, cause the great interest of people in the application of field of Environment Protection.Its subject matter is in light-catalyzed reaction process, the compound in meeting light induced electron and hole, thus reduces its oxidation capacity.
Chinese patent CN103130368A discloses a kind for the treatment of process of rapid degradation of power plant citric acid cleaning boiler waste water, comprises the following steps: in power plant citric acid cleaning boiler waste water, add the gac that absorption is saturated; The pH value regulating power plant citric acid cleaning boiler waste water is 3.00 ~ 3.10; Under the power plant citric acid cleaning boiler waste water regulating pH value is placed in solar irradiation, and stir with the rotating speed of 200 ~ 300r/min; In power plant citric acid cleaning boiler waste water, dropwise slowly add the hydrogen peroxide of 30wt%; Measure the pH value of power plant citric acid cleaning boiler waste water every 1h and be adjusted to 3.60 ~ 3.80; The C0D of power plant citric acid cleaning boiler waste water crafter illumination 4 ~ 8h, decline 45 ~ 55%, power plant citric acid cleaning boiler waste water obtains fast degradation.This patent processes waste water by dripping hydrogen peroxide in waste water.But the method dropwise need add hydrogen peroxide, complex operation, and method does not have novelty.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and a kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed is provided.
Object of the present invention can be achieved through the following technical solutions:
Accelerate a method for boiler of power plant citric acid wastewater photodegradation speed, utilize anonizing to prepare TiO 2nano-tube array photocatalyst, and then utilize chemical bath deposition method to prepare WO 3-TiO 2modification TiO 2nano-tube array photocatalyst, then adds boiler of power plant citric acid wastewater, by WO 3-TiO 2modification TiO 2nano-tube array photocatalyst is placed in waste water with Pt sheet and is connected by wire, not impressed voltage, utilizes visible ray to carry out photo-irradiation treatment to waste water, accelerates boiler of power plant citric acid wastewater photodegradation speed.
When utilizing visible ray to carry out photo-irradiation treatment to waste water, light source is PLSSXE300C, light application time 60 ~ 180min, and strength of current is 11.0 ~ 20.0A, and intensity of illumination is 0.75 ~ 1.40 × 10 3w/m 2.
Preferably, light application time is 120min, and strength of current is 17.0A, and intensity of illumination is 1.18 × 10 3w/m 2.
When utilizing visible ray to carry out photo-irradiation treatment to waste water, also in electrolytic solution, add the sodium sulfate that concentration is 0.2M, the light source now adopted is PLSSXE300C, light application time 60 ~ 180min, and strength of current is 11.0 ~ 20.0A, and intensity of illumination is 0.75 ~ 1.40 × 10 3w/m 2.
Preferably, light application time is 120min, and strength of current is 17.0A, and intensity of illumination is 1.18 × 10 3w/m 2.
Compared with prior art, the mechanism that the present invention utilizes novel photocatalysis system to accelerate boiler of power plant citric acid wastewater photodegradation speed is: TiO 2there is good photocatalytic activity, TiO 2skin there is special electronic structure, its energy band structure is normally made up of a low energy valence band being full of electronics and an empty high energy valence band.Region between these two energy bands is called forbidden band, and when having the rayed being greater than this band-gap energy, the electrons in valence band transits on conduction band, thus forms hole/electron pair, the h produced +tiO will be adsorbed on 2the OH of particle surface -and H 2o molecular oxygen changes into OH.OH is strong oxidizer, can be oxidized boiler of power plant citric acid wastewater.But in light-catalyzed reaction process, the Complex Problem in light induced electron and hole have impact on its oxidation capacity to a great extent.
At WO 3-TiO 2in compound system, TiO 2be a kind of n-type semiconductor, forbidden band can be 3.2eV, the light induced electron (e produced when being excited -) density be far longer than hole (h +) density, photo-generated carrier is mainly e -; WO 3be a kind of p-type semiconductor, forbidden band can be 2.8eV, the hole (h produced when being excited +) density is much larger than light induced electron (e -) density, photo-generated carrier is mainly h +.WO 3valence band (VB) and conduction band (VB) position be all positioned at TiO 2position of energy band on, when compound system is subject to excitation light irradiation, due to the capacity volume variance of residing energy level, WO 3h in valence band +to TiO 2valence band migration; Meanwhile, TiO 2the transition of electron produced is to TiO 2the backward WO of conduction band 3conduction band on move.This electrons that compound system is produced is to (e -/ h +) be effectively separated.And the TiO of tubular type pattern 2there is larger specific surface area and stronger adsorptive power; The hollow tubular structure of its uniqueness can provide passage for the transmission of light induced electron, also can reduce the recombination probability of photo-generate electron-hole to a certain extent, improve catalytic activity.
WO 3-TiO 2modification TiO 2after nano-tube array is connected with Pt sheet, due to the existence of system built-in potential difference, light induced electron is driven to migrate to Pt sheet from light anode by external circuit, effectively overcome the Complex Problem in light induced electron and hole, the photocatalytic activity of photocatalyst to boiler of power plant citric acid wastewater is greatly improved.
By adding metabisulfite solution, insert WO 3-TiO 2modification TiO 2nano-tube array and Pt sheet, and connect WO with wire 3-TiO 2modification TiO 2nano-tube array photocatalyst and Pt sheet, and in conjunction with visible ray, light application time, intensity that the application adopts, wastewater degradation speed can be increased substantially.
Accompanying drawing explanation
Fig. 1 be in embodiment 2 visible ray to the spectrogram of wastewater treatment;
Fig. 2 be in embodiment 3 visible ray to the spectrogram of wastewater treatment.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Utilize the inventive method in the example accelerating boiler of power plant citric acid wastewater photodegradation speed.
Citric acid cleaning wastewater from power plant boiler used be simulation Cleaning Wastewater composition, according to every premium on currency add 21g citric acid, 16.1g iron nitrate ratio formulated voluntarily.Waste water after filtration and with ammoniacal liquor, pH is adjusted to 3, is 16500mg/L through National Standard Method wastewater measurement COD value.DeR is carried out in homemade square quartzy glass sock layer reactor, and reactor useful volume is 30mL.Logical tap water in each reaction process, makes reaction system keep homo(io)thermism, the interference of external light source to reaction system and paper using plate resistance is broken.Simulated visible light is utilized to irradiate 120min.
Direct photolysis, only with simulated visible light to reaction system illumination; During photocatalytic degradation, in reaction system, add WO 3-TiO 2modification TiO 2nano-tube array photocatalyst; During the degraded of novel photocatalysis device system, add platinized platinum and with wire by platinized platinum and WO 3-TiO 2modification TiO 2nano-tube array photocatalyst connects.
The first step: direct photolysis, only with simulated visible light to reaction system illumination.
Second step: photocatalytic degradation, adds the WO of preparation in reaction system 3-TiO 2modification TiO 2nano-tube array photocatalyst, with simulated visible light to reaction system illumination.
3rd step: novel photocatalysis system is degraded.Add platinized platinum and with wire by platinized platinum and WO 3-TiO 2modification TiO 2nano-tube array photocatalyst connects, and adds 0.2M sodium sulfate, with simulated visible light to reaction system illumination in simulation Cleaning Wastewater.
4th step: measure COD respectively and calculate clearance.
The citric acid cleaning wastewater from power plant boiler of direct photolysis to high density has certain degradation effect, and after reaction 120min, COD clearance is 9%.Photocatalytic degradation system, owing to adding the photocatalyst of highlight catalytic active, COD clearance obviously increases to 31%.Novel photocatalysis system, shows the highest COD clearance 46%.
Embodiment 2
Accelerate a method for boiler of power plant citric acid wastewater photodegradation speed, adopt following steps:
(1) anonizing is utilized to prepare TiO 2nano-tube array: titanium sheet is cut out the rectangle into 20mm × 45mm, is placed in acetone, ethanol, deionized water for ultrasonic cleaning after 10min removes surperficial grease, air drying successively.Afterwards, the titanium sheet of drying (is consisted of V in polishing fluid hF: V hNO3: V h2O=1:4:5) middle chemical rightenning 5s, after deionized water rinsing, air-dry stand-by in air.With cleaned titanium sheet be anode, platinum for negative electrode is in magnetic agitation condition anodic oxygen, electrolytic solution consists of containing 0.5w%NH 4the ethylene glycol solution of F, 1w%1MKOH; Oxidation voltage adopts step anodic oxidation voltage: employing high pressure 60V, low pressure 10V continue 1min alternating oxidation, and total oxidization time is 60min.The good titanium sheet of anodic oxidation is with after a large amount of deionized water rinsing, air-dry, is placed in resistance furnace and rises to furnace cooling after 450 DEG C of insulation 1h with the temperature rise rate of 5 DEG C/min;
(2) chemical bath deposition method is utilized to prepare WO 3-TiO 2modification TiO 2nano-tube array:
(2-1) by TiCl 4dropwise add (TiCl in deionized water 4be 1.1:10 with the volume ratio of deionized water), carry out in ice-water bath in whole process and vigorous stirring, obtain water white TiCl 4solution 1.;
(2-2) 0.3965gWCl is taken 6powder is dissolved in 10mL dehydrated alcohol, obtains 0.1MWCl 6storing solution, dilution is afterwards 0.01MWCl 6use liquid 2..Because of WCl 6very easily with the moisture in air and oxygen reaction, all dissolvings and dilution operation are all carried out in ml headspace bottle and syringe, and now solution colour is yellow;
(2-3) by obtained TiO 2nanometer pipe array electrode is placed in beaker, adds WCl 6use liquid 2., constantly rocking beaker, to add volume ratio be the ethanol of 1:1 and the mixed solution of water, until solution colour becomes mazarine from yellow through colourless, adds TiCl afterwards 41. solution, rock beaker and make it mix; The volume that each solution is taken is as table 1.
TiO prepared by table 1 2-WO 3modification TiO 2each solution amount of taking during nanotube
(2-4) beaker is sealed, be placed in thermostat water bath, be warming up to 70 DEG C of insulations to take out after one hour, now solution is oyster white, with after washes of absolute alcohol electrode surface in nitrogen atmosphere dry 30min, afterwards in resistance furnace with the temperature rise rate of 5 DEG C/min rise to 450 DEG C insulation one hour after furnace cooling.Obtain WO 3-TiO 2modification TiO 2nano-tube array photocatalyst.
(3) boiler of power plant citric acid wastewater is added, by WO 3-TiO 2modification TiO 2nano-tube array photocatalyst is placed in waste water with Pt sheet and is connected by wire, and when utilizing visible ray to carry out photo-irradiation treatment to waste water, light source is PLSSXE300C, light application time 120min, and strength of current is 17.0A, and intensity of illumination is 1.18 × 10 3w/m 2, spectrogram when regulating be 5ms integral time as shown in Figure 1, by measuring COD content wherein, can find that the method can accelerate boiler of power plant citric acid wastewater photodegradation speed.
Embodiment 3
A kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed, the first two step is identical with embodiment 2, difference is, when step (3) utilizes visible ray to carry out photo-irradiation treatment to waste water, also add the sodium sulfate that concentration is 0.2M wherein, the light source of employing is PLSSXE300C, light application time 120min, strength of current is 17.0A, and intensity of illumination is 1.18 × 10 3w/m 2, spectrogram when regulating be 5ms integral time as shown in Figure 2, by measuring COD content wherein, can find that the method can accelerate boiler of power plant citric acid wastewater photodegradation speed.
Embodiment 4
Accelerate a method for boiler of power plant citric acid wastewater photodegradation speed, utilize anonizing to prepare TiO 2nano-tube array photocatalyst, recycling chemical bath deposition method prepares WO 3-TiO 2modification TiO 2nano-tube array photocatalyst, then adds boiler of power plant citric acid wastewater, by WO 3-TiO 2modification TiO 2nano-tube array photocatalyst is placed in waste water with Pt sheet and is connected by wire, not impressed voltage, utilizes visible ray to carry out photo-irradiation treatment to waste water, and light source is PLSSXE300C, light application time 60min, and strength of current is 20.0A, and intensity of illumination is 1.40 × 10 3w/m 2.Measure COD content wherein, accelerate boiler of power plant citric acid wastewater photodegradation speed.
Embodiment 5
Accelerate a method for boiler of power plant citric acid wastewater photodegradation speed, utilize anonizing to prepare TiO 2nano-tube array photocatalyst, recycling chemical bath deposition method prepares WO 3-TiO 2modification TiO 2nano-tube array photocatalyst, then adds boiler of power plant citric acid wastewater, by WO 3-TiO 2modification TiO 2nano-tube array photocatalyst is placed in waste water with Pt sheet and is connected by wire, not impressed voltage, utilizes visible ray to carry out photo-irradiation treatment to waste water, and light source is PLSSXE300C, light application time 180min, and strength of current is 11.0A, and intensity of illumination is 0.75 × 10 3w/m 2.Measure COD content wherein, accelerate boiler of power plant citric acid wastewater photodegradation speed.
Embodiment 6
Accelerate a method for boiler of power plant citric acid wastewater photodegradation speed, its method is identical with embodiment 5, and difference is, when utilizing visible ray to carry out photo-irradiation treatment to waste water, also in electrolytic solution, adds the sodium sulfate that concentration is 0.2M.

Claims (6)

1. accelerate a method for boiler of power plant citric acid wastewater photodegradation speed, utilize anonizing to prepare TiO 2nano-tube array, and then utilize chemical bath deposition method to prepare WO 3-TiO 2modification TiO 2nano-tube array photocatalyst, is characterized in that,
Add boiler of power plant citric acid wastewater, by WO 3-TiO 2modification TiO 2nano-tube array photocatalyst is placed in waste water with Pt sheet and is connected by wire, does not need impressed voltage, utilizes visible ray to carry out photo-irradiation treatment to waste water, accelerates boiler of power plant citric acid wastewater photodegradation speed.
2. a kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed according to claim 1, it is characterized in that, when utilizing visible ray to carry out photo-irradiation treatment to waste water, light source is PLSSXE300C, light application time 60 ~ 180min, strength of current is 11.0 ~ 20.0A, and intensity of illumination is 0.75 ~ 1.40 × 10 3w/m 2.
3. a kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed according to claim 2, is characterized in that, the preferred 120min of light application time, the preferred 17.0A of strength of current, intensity of illumination preferably 1.18 × 10 3w/m 2.
4. a kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed according to claim 1, is characterized in that, when utilizing visible ray to carry out photo-irradiation treatment to waste water, also in electrolytic solution, adds the sodium sulfate that concentration is 0.2M.
5. a kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed according to claim 4, it is characterized in that, when utilizing visible ray to carry out photo-irradiation treatment to waste water, light source is PLSSXE300C, light application time 60 ~ 180min, strength of current is 11.0 ~ 20.0A, and intensity of illumination is 0.75 ~ 1.40 × 10 3w/m 2.
6. a kind of method accelerating boiler of power plant citric acid wastewater photodegradation speed according to claim 5, is characterized in that, the preferred 120min of light application time, the preferred 17.0A of strength of current, intensity of illumination preferably 1.18 × 10 3w/m 2.
CN201510646654.6A 2015-10-08 2015-10-08 A kind of method for accelerating boiler of power plant citric acid wastewater light degradation speed Active CN105198033B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110342618A (en) * 2019-06-17 2019-10-18 浙江大学 The device and method of processing pickle liquor and electroplating sludge is cooperateed with using electrodialytic technique

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1995494A (en) * 2006-12-13 2007-07-11 天津大学 Anode oxidation method for preparing one-dimensional titanium dioxide array film
JP2013063442A (en) * 2013-01-18 2013-04-11 Shin-Etsu Chemical Co Ltd Dispersion liquid of photocatalyst particle and method of producing the same
CN103320839A (en) * 2013-05-28 2013-09-25 青岛农业大学 Preparation method of titanium dioxide nano-tube-array photo-electrode used for removing organic pollutant

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1995494A (en) * 2006-12-13 2007-07-11 天津大学 Anode oxidation method for preparing one-dimensional titanium dioxide array film
JP2013063442A (en) * 2013-01-18 2013-04-11 Shin-Etsu Chemical Co Ltd Dispersion liquid of photocatalyst particle and method of producing the same
CN103320839A (en) * 2013-05-28 2013-09-25 青岛农业大学 Preparation method of titanium dioxide nano-tube-array photo-electrode used for removing organic pollutant

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110342618A (en) * 2019-06-17 2019-10-18 浙江大学 The device and method of processing pickle liquor and electroplating sludge is cooperateed with using electrodialytic technique
CN110342618B (en) * 2019-06-17 2024-01-23 浙江大学 Device and method for cooperatively treating pickling waste liquid and electroplating sludge by utilizing electrodialysis technology

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