CN102219279A - Visible light catalytic degradation method of organic pollutants based on TiO2/carbon aerogel electrode - Google Patents
Visible light catalytic degradation method of organic pollutants based on TiO2/carbon aerogel electrode Download PDFInfo
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- CN102219279A CN102219279A CN2011101097918A CN201110109791A CN102219279A CN 102219279 A CN102219279 A CN 102219279A CN 2011101097918 A CN2011101097918 A CN 2011101097918A CN 201110109791 A CN201110109791 A CN 201110109791A CN 102219279 A CN102219279 A CN 102219279A
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Abstract
The invention belongs to the technical field of water treatment, and relates to a visible light catalytic degradation method of organic pollutants based on a TiO2/carbon aerogel electrode. The method comprises the following steps of: connecting a TiO2/carbon aerogel electrode material with a platinum wire to obtain a working electrode, using a platinum sheet as a counter electrode, and using a saturated calomel electrode as a reference electrode; adjusting the pH value of pollutants to be treated, and continuously introducing oxygen or air to the bottom of the TiO2/carbon aerogel working electrode during entire reaction process; then sensitizing TiO2 particles on the surface of the TiO2/carbon aerogel electrode for some time at a certain temperature and a constant negative potential; and starting a visible light source for carrying out photocatalytic degradation on the organic pollutants. By the invention, the visible light photocatalytic degradation of the organic pollutants based on a TiO2 photocatalyst can be realized. The method has simple process operation and good treatment effect on wastewater containing pollutants, is a safe, efficient and energy-saving new technology, and has a great application value in the wastewater treatment field.
Description
Technical field
The invention belongs to water-treatment technology field, relate to a kind of method of visible light photocatalytic degradation of organic pollutants.
Background technology
TiO
2Photocatalysis technology because its stable in properties, nontoxic, catalytic activity is high, advantage such as inexpensive receives increasing concern in wastewater treatment and organic pollutant degradation field in recent years.Yet, traditional TiO
2The widespread use of photocatalysis technology is subjected to the limitation of himself character.Because TiO
2Energy gap be 3.2eV, so in theory only under the UV-irradiation of wavelength＜385nm, just can make TiO
2The transition of valence band electron production realize photochemical catalysis.And in the solar spectrum only there be about 5% this a part of UV-light, for the visible spectrum TiO that accounts for about 45%
2Then not response is very low to the utilization ratio of luminous energy.Therefore, how to make TiO
2Absorption spectrum improve it has become this field to solar energy utilization rate research focus to the visible region from the ultraviolet region red shift.
Present research work mainly is by changing TiO
2The energy gap of self is widened visibility region with its absorption spectrum.For example pass through TiO
2Carry out finishing or pass through nonmetal C, methods such as doping such as N etc., transition metal Au, Ag have realized TiO
2Visible light catalytic.Yet, by the TiO that these methods obtained
2Compare also than very low under the efficient of visible light catalytic and the UV-irradiation.In addition, because light-catalyzed reaction is at TiO
2Therefore carry out on the surface of photocatalyst, can expect the TiO with high specific surface area
2Catalyzer tends to show better photocatalytic activity.Yet the TiO that is adopted in studying at present
2The often relatively lower 2～200cm of the specific surface area of powder and loaded photocatalyst
2/ g, and much studies show that, through the TiO after transition metal and the nonmetal doping modification
2Specific surface area can further reduce, and is unfavorable for efficiently carrying out of light-catalyzed reaction.Therefore, when constantly research prepares the novel photocatalysis agent material with visible light catalytic catalytic activity of high-specific surface area by adulterated method, explore TiO
2Photocatalyst surface differential responses approach realizes that the catalytic novel method of efficient visible light is the striving direction of this area research always.
Summary of the invention
The objective of the invention is at the defective of prior art and a kind of TiO is provided
2The method of/carbon aerogels (CA) electrode visible light photocatalytic degradation of organic pollutants.
For achieving the above object, the technical solution used in the present invention is as follows:
Originally researched and proposed a kind of TiO of novelty
2/ carbon silica aerogel electrode is direct TiO under excess oxygen
2The method of visible light catalytic.Be different from the method that traditional method of passing through finishing or element doping realizes its visible light catalytic, will be without the TiO of any doping vario-property
2Load on the carbon aerogels with good electric chemical property and high-specific surface area, under certain oxygen enrichment and cathode potential condition, realized TiO
2The visible light electrocatalysis.And this method is further used for pollutent waste water is carried out degradation treatment, obtain good effect, have important significance for theories and potential using value.
A kind of TiO
2The method of/carbon silica aerogel electrode visible light photocatalytic degradation of organic pollutants, it is as follows to comprise step:
(1) with TiO
2/ carbon silica aerogel electrode material is connected with platinum filament as working electrode, and platinized platinum is a counter electrode, and saturated calomel electrode is reference electrode (SCE);
(2) the pH value of the pending pollutent of adjusting;
(3) then under certain temperature, the effect of constant negative potential, to TiO
2/ carbon silica aerogel electrode carries out pre-reaction;
(4) open light source and carry out the photocatalytic degradation experiment.
In the described step (1), TiO
2/ carbon aerogels working electrode is identical with the area of platinized platinum counter electrode, is respectively 5.5～23.5cm
2Described TiO
2/ carbon silica aerogel electrode material adopts the sol-gel dipping, takes out the preparation of back high-temperature calcination method.
In the described step (1), the three-electrode system that reference electrode, counter electrode and working electrode constitute provides required negative voltage, wherein TiO by electrochemical workstation
2Distance between/carbon aerogels working electrode and the platinized platinum counter electrode is 2～3cm.
The pH scope is controlled at 1.7～2 in the described step (2).
In the described step (3) potential range be-0.3～-1.0V.
Carry out in having the single chamber reaction tank of recirculated water overcoat described step (2)～(4), and the capacity of reaction solution is 100～500mL in the single chamber reaction tank; Circulating water temperature is 25～35 ℃; Or in described step (2)～(4), at TiO
2/ carbon silica aerogel electrode bottom continues aerating oxygen or air, and gas velocity is 200～1000mL/min.
Pre-reaction time is 10～30min in the described step (3).
Distance in the described step (4) between light source and the reaction tank outer wall is 2～3cm; The light source that is adopted is the visible light of wavelength l＞420nm.
The photodegradation time of described step (4) is 180～360min.
Described pollutent comprises, typical phenolic comp ' ds pollution, has high chroma or highly toxic heterocyclic dyestuff, preferred phenol, p-Nitroaniline, rhodamine 6G or methylene blue etc.
The visible light photocatalytic degradation of organic pollutants device comprises electrochemical workstation; TiO
2/ carbon silica aerogel electrode; The platinized platinum electrode; Reference electrode; Ventilating pit (contained gas steel cylinder or air aeration device and air flowmeter); Visible light source (l＞420nm); The magnetic agitation instrument; Single chamber reaction tank with recirculated water overcoat; Recirculated water is imported and exported.
Three-electrode system is adopted in experiment, provides the constant negative potential by electrochemical workstation.
The TiO that employing of the present invention is connected with platinum filament
2/ carbon aerogels working electrode material is at carbon aerogels area load TiO by sol-gel, high-temperature calcination method
2Nano particle, the characteristics of this material are: the carbon aerogels as base material is a kind of porous carbon materials with network-like structure, has characteristics such as specific surface area is big, good electrical conductivity, is a kind of block type electrode of excellent performance.Platinized platinum is as counter electrode, and what reference electrode adopted is saturated calomel electrode.
Described device, the feeding speed of oxygen or air can be controlled by gas meter, in order to keep the constant temperature of reaction, can be by the outer recirculated water control reaction temperature of reaction tank.
Use this method that organic pollutant wastewater is handled discovery: it can overcome TiO
2Photocatalyst does not have the shortcoming of catalytic effect at visible region, makes TiO
2/ carbon silica aerogel electrode has been issued to 90.3% clearance in the visible light effect, is TiO under the similarity condition
26.8 times of/ITO electrode.
Compared with prior art, the present invention has following advantage:
(1) with conventional Ti O
2Photocatalyst can only be used for the ultraviolet catalytic degradation of contaminant to be compared, and method provided by the present invention can allow TiO
2Particle produces katalysis at visible region, is used for the visible light photocatalytic degradation of organic pollutant.
(2) realize TiO with existing method by finishing or element doping
2Visible light catalytic use and to compare, the present invention adopts easy electrochemistry sensitization under excess oxygen to handle means, makes TiO
2Significant red shift appears in particle energy of absorption edge under the state of not doing any modification, shows visible light catalysis activity efficiently.This technological operation is easy, and is good to the treatment effect of pollutent waste water, is a kind of safe, efficient, energy-conservation new technology, has very big using value in field of waste water treatment.
Description of drawings
The TiO that Fig. 1 is connected with platinum filament for employing of the present invention
2/ carbon aerogels working electrode visible light photocatalytic degradation of organic pollutants setting drawing.
The TiO of Fig. 2 for being connected with platinum filament among the present invention
2/ carbon aerogels working electrode is ultraviolet-visible diffuse-reflectance figure before and after the electrochemistry sensibilized.
Embodiment
Further specify the present invention below by embodiment.
TiO
2/ carbon silica aerogel electrode visible light photocatalytic degradation of organic pollutants device comprises electrochemical workstation (1); TiO
2/ carbon silica aerogel electrode (2); Platinized platinum electrode (3); Reference electrode (4); Ventilating pit (5) (contained gas steel cylinder and gas meter); Visible light source (6) (l＞420nm); Magnetic agitation instrument (7); Single chamber reaction tank (8) with recirculated water overcoat; Recirculated water is imported and exported (9).
(1) produces a constant negative potential by electrochemical workstation and put on the TiO that is connected with platinum filament
2On/carbon aerogels the working electrode;
(2) and during the course aerating oxygen (or air) all the time in solution makes solution be in the oxygen enrichment state;
(3) TiO that is connected with platinum filament
2/ carbon aerogels working electrode is electrochemistry pre-reaction for some time in acidic solution;
(4) through after the pre-reaction of certain hour, open visible light source and be used for the visible light degradation of contaminant.
Embodiment 1: with rhodamine 6G pollutent waste water is example.
The starting point concentration of rhodamine 6G simulated wastewater is 50mg/L, and supporting electrolyte vitriolic concentration is 0.01mol/L, and the pH value of solution value is 1.7, and volume is 100mL.Degradation experiment carries out (Shanghai China in morning, China) on electrochemical workstation CHI760.
(1) adopts traditional three-electrode system.With TiO
2/ carbon silica aerogel electrode material is connected as working electrode with platinum filament, and platinized platinum is a counter electrode, and saturated calomel electrode is as reference electrode (SCE); The TiO that is connected with platinum filament
2The area of/carbon aerogels working electrode is 10.5cm
2, the distance between working electrode and the platinized platinum counter electrode is 3cm.
(2) at the TiO that is connected with platinum filament
2/ carbon silica aerogel electrode bottom, aerating oxygen, in whole experiment, near oxygen flow velocity with the 200mL/min solution bottom cathode feeds
(3) then under the negative potential of 25 ℃ and constant-0.9V, reaction continues 30min under the condition of not opening light source.
(4) open visible light source and carry out the photocatalytic degradation experiment.
Visible light source is the xenon lamp of λ＞420nm, and the spacing between light source and the working electrode is 3cm.
The clearance of rhodamine 6G has reached 90.3% in the 300min, is TiO under the similarity condition
26.8 times of/ITO electrode.
Embodiment 2: with p-Nitroaniline pollutent waste water is example.
The starting point concentration of p-Nitroaniline simulated wastewater is 150mg/L, and the concentration of supporting electrolyte sodium sulfate is 0.05mol/L, and with dilute sulphuric acid regulator solution pH=2, volume is 100mL.Degradation experiment carries out (Shanghai China in morning, China) on electrochemical workstation CHI760.
(1) adopts traditional three-electrode system.With TiO
2/ carbon silica aerogel electrode material is connected as working electrode with platinum filament, and platinized platinum is a counter electrode, and saturated calomel electrode is as reference electrode (SCE); The TiO that is connected with platinum filament
2The area of/carbon aerogels working electrode is 5.5cm
2, the distance between working electrode and the platinized platinum counter electrode is 2cm.
(2) at the TiO that is connected with platinum filament
2/ carbon silica aerogel electrode bottom, bubbling air, in whole experiment, near oxygen flow velocity with the 400mL/min solution bottom cathode feeds.
(3) then under the negative potential of 25 ℃ and constant-0.6V, reaction continues 30min under the condition of not opening light source.
(4) open visible light source and carry out the photocatalytic degradation experiment.
Visible light source is the xenon lamp of λ＞420nm, and the spacing between light source and the working electrode is 3cm.
The clearance of p-Nitroaniline has reached 98.2% in the 180min, is TiO under the similarity condition
21.23 times of/Graphite Electrodes.
Embodiment 3: being example to methylene blue pollutent waste water.
The starting point concentration of methylene blue simulated wastewater is 100mg/L, and supporting electrolyte vitriolic concentration is 0.01mol/L, and the pH value of solution value is 1.7, and volume is 100mL.Degradation experiment carries out (Shanghai China in morning, China) on electrochemical workstation CHI760.
(1) adopts traditional three-electrode system.With TiO
2/ carbon silica aerogel electrode material is connected as working electrode with platinum filament, and platinized platinum is a counter electrode, and saturated calomel electrode is as reference electrode (SCE); The TiO that is connected with platinum filament
2The area of/carbon aerogels working electrode is 7cm
2, the distance between working electrode and the platinized platinum counter electrode is 2cm.
(2) at the TiO that is connected with platinum filament
2/ carbon silica aerogel electrode bottom, aerating oxygen, in whole experiment, near oxygen flow velocity with the 300mL/min solution bottom cathode feeds.
(3) then under the negative potential of 30 ℃ and constant-1.0V, reaction continues 20min under the condition of not opening light source.
(4) open visible light source and carry out the photocatalytic degradation experiment.
Visible light source is the xenon lamp of λ＞420nm, and the spacing between light source and the working electrode is 3cm.
The clearance of methylene blue has reached 95% in the 360min, is TiO under the similarity condition
28 times of/ITO electrode.Embodiment 4: with phenol pollutent waste water is example.
The starting point concentration of phenol synthetic water is 100mg/L, and supporting electrolyte vitriolic concentration is 0.01mol/L, and the pH value of solution value is 1.7, and volume is 500mL.Degradation experiment carries out (Shanghai China in morning, China) on electrochemical workstation CHI760.
(1) adopts traditional three-electrode system.With TiO
2/ carbon silica aerogel electrode material is connected as working electrode with platinum filament, and platinized platinum is a counter electrode, and saturated calomel electrode is as reference electrode (SCE); The TiO that is connected with platinum filament
2The area of/carbon aerogels working electrode is 23.5cm
2, the distance between working electrode and the platinized platinum counter electrode is 3cm.
(2) at the TiO that is connected with platinum filament
2/ carbon silica aerogel electrode bottom, aerating oxygen, in whole experiment, near oxygen flow velocity with the 1000mL/min solution bottom cathode feeds.
(3) then under the negative potential of 35 ℃ and constant-0.3V, reaction continues 10min under the condition of not opening light source;
(4) open visible light source and carry out the photocatalytic degradation experiment.
Visible light source is the xenon lamp of λ＞420nm, and the spacing between light source and the working electrode is 2cm.
The clearance of phenol has reached 89% in the 360min, is TiO under the similarity condition
22.5 times of/ITO electrode.
In the equipment of practical application, along with increasing of wastewater treatment capacity, measures such as feeding amount that can be by regulating electrode area, electropotential and oxygen or air and photocatalytic degradation treatment time guarantee degradation effect.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. TiO
2The method of/carbon silica aerogel electrode visible light photocatalytic degradation of organic pollutants is characterized in that: it is as follows to comprise step:
(1) with TiO
2/ carbon silica aerogel electrode material is connected with platinum filament as working electrode, and platinized platinum is a counter electrode, and saturated calomel electrode is a reference electrode;
(2) the pH value of the pending pollutent of adjusting;
(3) then under certain temperature, the effect of constant negative potential, to TiO
2/ carbon silica aerogel electrode carries out pre-reaction;
(4) open light source and carry out the photocatalytic degradation experiment.
2. method according to claim 1 is characterized in that: in the described step (1), and TiO
2/ carbon aerogels working electrode is identical with the area of platinized platinum counter electrode, is respectively 5.5～23.5cm
2Described TiO
2/ carbon silica aerogel electrode material adopts the sol-gel dipping, takes out the preparation of back high-temperature calcination method.
3. method according to claim 1 is characterized in that: in the described step (1), the three-electrode system that reference electrode, counter electrode and working electrode constitute provides required negative voltage by electrochemical workstation; TiO wherein
2Distance between/carbon aerogels working electrode and the platinized platinum counter electrode is 2～3cm.
4. method according to claim 1 is characterized in that: the pH scope is controlled at 1.7～2 in the described step (2).
5. method according to claim 1 is characterized in that: in the described step (3) potential range be-0.3～-1.0V; Pre-reaction time is 10～30min.
6. method according to claim 1 is characterized in that: carry out in having the single chamber reaction tank of recirculated water overcoat described step (2)～(4), and the capacity of reaction solution is 100～500mL in the single chamber reaction tank; Circulating water temperature is 25～35 ℃; Or in described step (2)～(4), at TiO
2/ carbon silica aerogel electrode bottom continues aerating oxygen or air, and gas velocity is 200～1000mL/min.
7. method according to claim 1 is characterized in that: the distance in the described step (4) between light source and the reaction tank outer wall is 2～3cm; The light source that is adopted is the visible light of wavelength l＞420nm; Or the photodegradation time of described step (4) is 180～360min.
8. method according to claim 1 is characterized in that: the distance in the described step (4) between light source and the reaction tank outer wall is 2～3cm; The light source that is adopted is the visible light of wavelength l＞420nm; The photodegradative time of described step (4) is 180～360min.
9. method according to claim 1 is characterized in that: described pollutent comprises typical phenolic comp ' ds pollution, has high chroma or highly toxic heterocyclic dyestuff, preferred phenol, p-Nitroaniline, rhodamine 6G or methylene blue.
10. method according to claim 1 is characterized in that: this method is carried out in the visible light photocatalytic degradation of organic pollutants device, comprising electrochemical workstation (1); TiO
2/ carbon silica aerogel electrode (2); Platinized platinum electrode (3); Reference electrode (4); Ventilating pit (5); Visible light source (6); Magnetic agitation instrument (7); Single chamber reaction tank (8) with recirculated water overcoat; Recirculated water is imported and exported (9).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102671587A (en) * | 2012-05-31 | 2012-09-19 | 上海应用技术学院 | Titanium dioxide/carbon hybrid aerogel material and preparation method thereof |
| CN103964540A (en) * | 2013-01-31 | 2014-08-06 | 同济大学 | Application of small size {001} TiO2/carbon aerogel electrode |
| CN108940143A (en) * | 2018-09-29 | 2018-12-07 | 云南大学 | A kind of pigment is the preparation method and applications of the titanium silica aerogel of template |
| CN111018059A (en) * | 2019-11-26 | 2020-04-17 | 西安建筑科技大学 | Preparation method of carbon fiber inorganic polymer composite electrode |
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| CN1962477A (en) * | 2006-10-26 | 2007-05-16 | 上海交通大学 | Process for catalyzing oxidation of organic compounds by ultraviolet |
| CN101549895A (en) * | 2009-04-23 | 2009-10-07 | 同济大学 | Preparation method of carbon aerogel load titanium dioxide electrodes and application thereof |
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2011
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| CN1962477A (en) * | 2006-10-26 | 2007-05-16 | 上海交通大学 | Process for catalyzing oxidation of organic compounds by ultraviolet |
| CN101549895A (en) * | 2009-04-23 | 2009-10-07 | 同济大学 | Preparation method of carbon aerogel load titanium dioxide electrodes and application thereof |
Non-Patent Citations (1)
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|---|
| YUNING JIN,ECT: "Photocatalysis-enhanced electrosorption process for degradation of high-concentration dye wastewater on TiO2/carbon aerogel", 《CHEMICAL ENGINEERING JOURNAL》, vol. 168, no. 3, 18 February 2011 (2011-02-18), pages 1248 - 1255 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102671587A (en) * | 2012-05-31 | 2012-09-19 | 上海应用技术学院 | Titanium dioxide/carbon hybrid aerogel material and preparation method thereof |
| CN102671587B (en) * | 2012-05-31 | 2015-02-11 | 上海应用技术学院 | Titanium dioxide/carbon hybrid aerogel material and preparation method thereof |
| CN103964540A (en) * | 2013-01-31 | 2014-08-06 | 同济大学 | Application of small size {001} TiO2/carbon aerogel electrode |
| CN103964540B (en) * | 2013-01-31 | 2016-01-20 | 同济大学 | A kind of small size { 001}TiO 2the application of/carbon silica aerogel electrode |
| CN108940143A (en) * | 2018-09-29 | 2018-12-07 | 云南大学 | A kind of pigment is the preparation method and applications of the titanium silica aerogel of template |
| CN111018059A (en) * | 2019-11-26 | 2020-04-17 | 西安建筑科技大学 | Preparation method of carbon fiber inorganic polymer composite electrode |
| CN111018059B (en) * | 2019-11-26 | 2022-05-17 | 西安建筑科技大学 | Preparation method of carbon fiber inorganic polymer composite electrode |
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Application publication date: 20111019 |