CN101966450A - High-efficiency composite photocatalyst and preparation method thereof - Google Patents
High-efficiency composite photocatalyst and preparation method thereof Download PDFInfo
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- CN101966450A CN101966450A CN2010102399535A CN201010239953A CN101966450A CN 101966450 A CN101966450 A CN 101966450A CN 2010102399535 A CN2010102399535 A CN 2010102399535A CN 201010239953 A CN201010239953 A CN 201010239953A CN 101966450 A CN101966450 A CN 101966450A
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Abstract
The invention belongs to the field of photocatalysis and relates to a high-efficiency composite photocatalyst and a preparation method thereof. The high-efficiency composite photocatalyst is synthesized by a hydrothermal method in one step, and is characterized in that: a semiconductor nano material is compounded by combining a zero-dimensional nano material (TiO2 nanoparticle) and a one-dimensional nano material (ZnO nanorod), heterogeneous interface junctions can be effectively increased in a mode of combining materials, effective separation of electron holes is promoted, the probability for exciton recombination is reduced, and the photoelectric conversion efficiency and photocatalytic activity of the photocatalysis are further improved. The preparation process is simple, the structure and components of a photocatalyst material can be effectively controlled, the photoelectric chemical properties of the semiconductor nano material are finally controlled, and the high-efficiency composite photocatalyst has significance for studying photocatalytic performance and application of the semiconductor nano material, and has potential application value.
Description
Technical field
The present invention relates to a kind of with TiO
2The preparation method of nano particle and the compound generation high efficiency photocatalyst of ZnO nanometer rods.
Background technology
At current photochemical catalyst research field, semiconductor nano material (as: titanium dioxide TiO
2With zinc oxide ZnO) owing to physicochemical properties, excellent catalytic activity, good stable and cheap cost, become the focus of research with size adjustable.Yet the photoresponse scope that how further to suppress right quick compound in the light induced electron/hole of these materials and improve these materials is that these materials move towards the problem that must solve in the market process all the time.In order to address these problems, the measure of usually taking comprises: the mode such as compound of the control pattern of semiconductor nano material and crystalline phase, doping, sensitization and multiple material.
In recent years, nano composite material (as: TiO
2/ SiO
2, TiO
2/ WO
3, TiO
2/ CdSe, TiO
2/ ZnO etc.), and become a kind of novel and efficient semiconductor photocatalyst material by extensive concern and research.Semiconductor nanometer composite material adopts dual mode to produce acquisition usually: physical mixed (nano particles of two or more crystalline phases) or chemical synthesis.Be compared to physical admixture, the nano composite material that the chemical synthesis mode makes forms spherical, banded or bar-shaped nucleocapsid structure (core/shell) usually, and combination is more tight and even between the various crystalline phase.It has been generally acknowledged that nano composite material is owing to have strong surface interaction between its composition, its character is not simply to be formed by stacking by its composition material, and should embody more excellent physicochemical properties; And the influence that electronic state changes between material interface in being subjected to recombination process of the physico-chemical property of nano composite material, also depend on the combination and the pattern of each composition material.
At present, people have attempted adopting various physics or chemical mode to prepare TiO
2/ ZnO nano composite material is with respect to simple TiO
2Nano material or ZnO nano material, these TiO
2The photoresponse scope of/ZnO nano composite material is wideer, and it is right more to separate the photoproduction electrons/effectively, is a kind of potential new and effective photochemical catalyst.In addition, studies show that for the ZnO nano particle, the One-Dimensional ZnO nano material is owing to have high-specific surface area and quantum confined effect, can more effectively suppress right compound in light induced electron/hole, improve photoelectric transformation efficiency.However, as far as we know, present TiO
2The research of/ZnO nano composite material mainly concentrates on TiO
2Compound between nano particle and ZnO nano particle is seldom relevant for TiO
2Nano particle/the preparation of One-Dimensional ZnO nanometer rods nano composite material and the research of performance thereof.Therefore, with TiO
2Nano particle and One-Dimensional ZnO nanometer rods can overcome usually at TiO on the one hand in conjunction with generating nano composite material
2The problem that is easy to reunite in nano particle and the ZnO nano particle recombination process, can also further more effectively suppress right compound in light induced electron/hole on the other hand, improve photoelectric transformation efficiency and photocatalytic activity, obtain a kind of high catalytic activity and novel photocatalysis agent with good stability.
Summary of the invention
The purpose of this invention is to provide a kind of new and effective composite photo-catalyst and preparation method thereof.
To achieve these goals, the invention provides a kind of composite photo-catalyst (TiO
2Nano particle/ZnO nanometer rods nano composite material) synthetic method.The present invention adopts the synthetic TiO that obtains of one step of hydro-thermal method
2/ ZnO composite photo-catalyst, entire reaction course is simple, the reaction condition gentleness, preparation cost is cheap.This composite photo-catalyst is by a large amount of TiO
2Nano particle (the about 20nm of size) coats One-Dimensional ZnO nanometer rods (the about 50nm of diameter, be about 1～2 μ m) be composited, this nanostructured can improve the specific area of photochemical catalyst and the transmittability of photogenerated charge effectively, thereby makes photochemical catalyst have high photoelectric transformation efficiency and photocatalysis performance.
The preparation method and the step of composite photo-catalyst of the present invention are as follows:
This composite catalyst is to adopt hydro-thermal method synthetic, with reactant presoma ZnCl
2And TiCl
4Under stirring condition, be dissolved in mixed solvent (10 milliliters ethanol and 10 ml waters mix), form precursor solution according to certain molar ratio; Then 10 milliliters of urea liquids (0.6M) are added drop-wise in the precursor solution under stirring condition, drip back continuation stirring and obtained transparent settled solution in about 15 minutes; Afterwards this settled solution is transferred in the teflon-lined stainless steel hydrothermal reaction kettle, and placed interior 180 degree of baking oven to react 16 hours down this reactor, reaction finishes and naturally cools to room temperature; Collect the reaction precipitation product by mode centrifugal and washing repeatedly, 450 degree calcinings 2 hours in Muffle furnace promptly obtain TiO behind the precipitated product oven drying after the calcining
2/ ZnO composite photo-catalyst.
The testing process of photochemical catalyst photocatalysis performance of the present invention is: if basal electrode adopts the F-SnO2 electro-conductive glass, 500mg self-control composite photo-catalyst is distributed to ethanol: in water (2: the 1) mixed solution, add equal-volume 40% polyoxyethylene aqueous solution, ultrasonic being uniformly dispersed is mixed with the pasty state slurries.With F-SnO
2Electro-conductive glass cuts into 1cm * 1.5cm, cleans with the special-purpose washing lotion of electro-conductive glass, and ethanol, each ultrasonic cleaning of acetone 3 minutes, nitrogen dries up, and uses plasma treatment 2 minutes.Adopt the blade coating mode with above-mentioned slurry blade coating at F-SnO
2Conductive glass surface was put into electrode in the Muffle furnace 450 ℃ of sintering 30 minutes then, promptly can be used for the photocatalytic activity test after the cooling; The template reagent of aqueous solution of methylene blue (10 μ M) as photocatalytic degradation adopted in photocatalytic activity test (as shown in Figure 2), photochemical catalyst electrode after the calcining is placed the quartz cell (3mL) that fills aqueous solution of methylene blue, and with high-pressure sodium lamp (power 100W) illumination (the about 35mW/cm of light intensity
2) carry out the photocatalytic degradation methylene blue solution; Afterwards, at set intervals the solution after the degraded is carried out the test of UV, visible light absorption curves, can reflect the photocatalytic activity (photocatalytic activity as shown in Figure 3) of photochemical catalyst thus.
Advantage of the present invention is to adopt zero-dimension nano material (TiO
2Nano particle) and the two mode of carrying out combination of monodimension nanometer material (ZnO nanometer rods) realize the compound of semiconductor nano material, utilize the mode of material combination can increase the heterogeneous node in interface effectively, promoted effective separation of electron hole, reduce the compound probability of exciton, and then increased the electricity conversion and the photocatalytic activity of photochemical catalyst; Simultaneously, preparation method provided by the invention can reduce the difficulty of semiconductor nanometer composite material preparation widely.
Description of drawings
Fig. 1 is a composite photo-catalyst pattern schematic diagram.
Fig. 2 is photocatalytic activity test structure schematic diagram figure.
Fig. 3 is photocatalytic activity test result (ordinate photocatalytic degradation speed is that the logarithm value by concentration ratio before and after the degradation product photocatalytic degradation reflects).
Among Fig. 1: 1. One-Dimensional ZnO nanometer rods; 2. zero dimension TiO
2Nano particle; 3.TiO
2Nano particle/ZnO nanometer rods composite photo-catalyst.
Among Fig. 2: 1. exciting light sources; 2. photocatalyst material layer; 3. photocatalytic degradation template reagent (can be methylene blue, rhodamine, formaldehyde, phenol, toluene), concentration is 10 μ M; 4. basal electrode; 5. quartz cell
Among Fig. 3: 1.TiO
2Nano particle photochemical catalyst (seeing embodiment 1); 2. One-Dimensional ZnO nano-rod photo-catalyst (seeing embodiment 2); 3. TiO
2/ ZnO composite photo-catalyst (seeing embodiment 3); 4. TiO
2/ ZnO composite photo-catalyst (seeing embodiment 4); 5. TiO
2/ ZnO composite photo-catalyst (seeing embodiment 5); 6. commercialization photochemical catalyst P25 (TiO
2Nano particle, German Degusa company produces)
The specific embodiment
Embodiment 1: with reactant presoma TiCl
4(1.14g) be dissolved in mixed solvent (10 milliliters ethanol and 10 ml waters mix) under stirring condition, forming concentration is 0.3M presoma TiCl
4Solution; Then 10 milliliters of urea liquids (0.6M) are added drop-wise in the precursor solution under stirring condition, drip back continuation stirring and obtained transparent settled solution in about 15 minutes; Afterwards this settled solution is transferred in the teflon-lined stainless steel hydrothermal reaction kettle, and placed interior 180 degree of baking oven to react 16 hours down this reactor, reaction finishes and naturally cools to room temperature; Collect the reaction precipitation product by mode centrifugal and washing repeatedly, 450 degree calcinings 2 hours in Muffle furnace promptly obtain TiO behind the precipitated product oven drying after the calcining
2The nano particle photochemical catalyst (is abbreviated as: TiO
2, as shown in Figure 1).As shown in Figure 3, simple TiO
2The photocatalytic activity of nano particle photochemical catalyst is the poorest.
Embodiment 2: with reactant presoma ZnCl
2(0.82g) be dissolved in mixed solvent (10 milliliters ethanol and 10 ml waters mix) under stirring condition, forming concentration is 0.3M presoma ZnCl
2Solution; Then 10 milliliters of urea liquids (0.6M) are added drop-wise in the precursor solution under stirring condition, drip back continuation stirring and obtained transparent settled solution in about 15 minutes; Afterwards this settled solution is transferred in the teflon-lined stainless steel hydrothermal reaction kettle, and placed interior 180 degree of baking oven to react 16 hours down this reactor, reaction finishes and naturally cools to room temperature; Collect the reaction precipitation product by mode centrifugal and washing repeatedly, 450 degree calcinings 2 hours in Muffle furnace behind the precipitated product oven drying, promptly obtain after the calcining ZnO nano-rod photo-catalyst (be abbreviated as: ZnO, as shown in Figure 1).As shown in Figure 3, the photocatalytic activity outline of simple ZnO nano-rod photo-catalyst is better than TiO
2The nano particle photochemical catalyst.
Embodiment 3: with reactant presoma ZnCl
2(0.27g) and TiCl
4(0.76g) under stirring condition, be dissolved in mixed solvent (10 milliliters ethanol and 10 ml waters mix), form presoma ZnCl according to certain molar ratio (1: 2)
2And TiCl
4Mixed solution; Then 10 milliliters of urea liquids (0.6M) are added drop-wise in the precursor solution under stirring condition, drip back continuation stirring and obtained transparent settled solution in about 15 minutes; Afterwards this settled solution is transferred in the teflon-lined stainless steel hydrothermal reaction kettle, and placed interior 180 degree of baking oven to react 16 hours down this reactor, reaction finishes and naturally cools to room temperature; Collect the reaction precipitation product by mode centrifugal and washing repeatedly, 450 degree calcinings 2 hours in Muffle furnace promptly obtain TiO behind the precipitated product oven drying after the calcining
2Nano particle/(the Zn/Ti mol ratio is 1: 2 to ZnO nanometer rods composite photo-catalyst, is abbreviated as: ZT12).As shown in Figure 3, this ZnO/TiO
2The photocatalytic activity of composite photo-catalyst will be significantly better than simple TiO
2Nano particle photochemical catalyst and simple ZnO nano-rod photo-catalyst.
Embodiment 4: with reactant presoma ZnCl
2(0.41g) and TiCl
4(0.57g) under stirring condition, be dissolved in mixed solvent (10 milliliters ethanol and 10 ml waters mix), form presoma ZnCl according to certain molar ratio (1: 1)
2And TiCl
4Mixed solution; Then 10 milliliters of urea liquids (0.6M) are added drop-wise in the precursor solution under stirring condition, drip back continuation stirring and obtained transparent settled solution in about 15 minutes; Afterwards this settled solution is transferred in the teflon-lined stainless steel hydrothermal reaction kettle, and placed interior 180 degree of baking oven to react 16 hours down this reactor, reaction finishes and naturally cools to room temperature; Collect the reaction precipitation product by mode centrifugal and washing repeatedly, 450 degree calcinings 2 hours in Muffle furnace promptly obtain TiO behind the precipitated product oven drying after the calcining
2Nano particle/(the Zn/Ti mol ratio is 1: 1 to ZnO nanometer rods composite photo-catalyst, is abbreviated as: ZT11).As shown in Figure 3, this ZnO/TiO
2The photocatalytic activity of composite photo-catalyst equally will be significantly better than simple TiO
2Nano particle photochemical catalyst and simple ZnO nano-rod photo-catalyst.
Embodiment 5: with reactant presoma ZnCl
2(0.55g) and TiCl
4(0.38g) under stirring condition, be dissolved in mixed solvent (10 milliliters ethanol and 10 ml waters mix), form presoma ZnCl according to certain molar ratio (2: 1)
2And TiCl
4Mixed solution; Then 10 milliliters of urea liquids (0.6M) are added drop-wise in the precursor solution under stirring condition, drip back continuation stirring and obtained transparent settled solution in about 15 minutes; Afterwards this settled solution is transferred in the teflon-lined stainless steel hydrothermal reaction kettle, and placed interior 180 degree of baking oven to react 16 hours down this reactor, reaction finishes and naturally cools to room temperature; Collect the reaction precipitation product by mode centrifugal and washing repeatedly, 450 degree calcinings 2 hours in Muffle furnace promptly obtain TiO behind the precipitated product oven drying after the calcining
2Nano particle/(the Zn/Ti mol ratio is 1: 1 to ZnO nanometer rods composite photo-catalyst, is abbreviated as: ZT21).As shown in Figure 3, this ZnO/TiO
2The photocatalytic activity of composite photo-catalyst is best, and photocatalytic activity has surpassed commercially produced product P25 (TiO in the market
2Nano particle, German Degusa company produces) photocatalytic activity.
Claims (9)
1. the preparation method of an efficient composite photo-catalyst is characterized in that: adopt one step of hydro-thermal method synthetic, composite photo-catalyst Zn/Ti mol ratio can be regulated according to reaction condition.
2. require the preparation method of described composite photo-catalyst as right 1, it is characterized in that: the ZnO presoma can be a zinc chloride, a kind of in the zinc sulfate; And TiO
2Presoma then can be a titanium tetrachloride, butyl titanate, a kind of in the tetraisopropyl titanate.
3. require the preparation method of described nano material electrode as right 1, it is characterized in that: solvent can adopt ethanol/water mixed solvent, water or alcohol solvent.
4. require the preparation method of described composite photo-catalyst as right 1, it is characterized in that: the composite photo-catalyst pattern can be regulated and control by setting different reaction temperatures and reaction time.
5. require the preparation method of described composite photo-catalyst as right 1, it is characterized in that: nano material can be a titanium dioxide, zinc oxide, tungstic acid, tin ash, one or more in the tri-iron tetroxide.
6. one kind prepares the preparation method that right 1 requires described photochemical catalyst electrode, it is characterized in that: nano material can adopt spin coating, blade coating or screen printing mode to be coated on the basal electrode surface.
7. one kind prepares the preparation method that right 1 requires described photochemical catalyst electrode, it is characterized in that: the basal electrode material can be fluoro tin ash (F-SnO
2) electro-conductive glass, indium tin oxide (ITO) electro-conductive glass, sheet metal (as: platinized platinum).
8. one kind requires the method for testing of described photochemical catalyst photocatalytic activity as right 1, it is characterized in that: the template reagent of photocatalytic degradation can be a kind of in methylene blue, rhodamine, formaldehyde, phenol, the toluene.
9. one kind requires the method for testing of described photochemical catalyst photocatalytic activity as right 1, it is characterized in that: composite photo-catalyst can be powder or require as right 6 as described in carry out photocatalytic degradation after being prepared into the photochemical catalyst electrode.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102284284A (en) * | 2011-06-03 | 2011-12-21 | 南昌航空大学 | Method for preparing molecularly imprinted TiO2/WO3 composite photocatalyst with visible light response through direct method |
| CN105289582A (en) * | 2015-10-30 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for zinc oxide nanometer rod supported manganese-oxide-base catalyst |
| CN105749897A (en) * | 2016-03-10 | 2016-07-13 | 中山大学 | Heterogenous photocatalyst with multichannel carrier separation function and preparation method and application of heterogenous photocatalyst with multichannel carrier separation function |
| CN107978458A (en) * | 2016-10-21 | 2018-05-01 | 江苏今道投资发展有限公司 | ZnO nanorod/TiO2The preparation method of nanoparticle composite film |
| CN109759042A (en) * | 2019-03-06 | 2019-05-17 | 北京化工大学 | A kind of photochemical catalyst and its application to the degradation of different gaseous-phase organic pollutant high efficiency photocatalysis |
| CN110026173A (en) * | 2019-04-28 | 2019-07-19 | 苏州科技大学 | Nano-ZnO/TiO2Composite photo-catalyst and its preparation method and application |
| CN110165003A (en) * | 2019-04-19 | 2019-08-23 | 广东工业大学 | Tungsten oxide and titanium oxide composite film of a kind of loaded mesoporous core-shell structure of tin oxide photonic crystal and its preparation method and application |
| CN111389428A (en) * | 2020-03-27 | 2020-07-10 | 中国海洋大学 | SiP2Quantum dot/photocatalytic material and preparation method thereof |
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| CN102284284A (en) * | 2011-06-03 | 2011-12-21 | 南昌航空大学 | Method for preparing molecularly imprinted TiO2/WO3 composite photocatalyst with visible light response through direct method |
| CN105289582A (en) * | 2015-10-30 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for zinc oxide nanometer rod supported manganese-oxide-base catalyst |
| CN105289582B (en) * | 2015-10-30 | 2017-11-10 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of zinc oxide nano rod supports the preparation method of oxidation manganese-based catalyst |
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| CN109759042A (en) * | 2019-03-06 | 2019-05-17 | 北京化工大学 | A kind of photochemical catalyst and its application to the degradation of different gaseous-phase organic pollutant high efficiency photocatalysis |
| CN110165003A (en) * | 2019-04-19 | 2019-08-23 | 广东工业大学 | Tungsten oxide and titanium oxide composite film of a kind of loaded mesoporous core-shell structure of tin oxide photonic crystal and its preparation method and application |
| CN110026173A (en) * | 2019-04-28 | 2019-07-19 | 苏州科技大学 | Nano-ZnO/TiO2Composite photo-catalyst and its preparation method and application |
| CN111389428A (en) * | 2020-03-27 | 2020-07-10 | 中国海洋大学 | SiP2Quantum dot/photocatalytic material and preparation method thereof |
| CN111389428B (en) * | 2020-03-27 | 2022-10-18 | 中国海洋大学 | SiP 2 Quantum dot/photocatalytic material and preparation method thereof |
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Application publication date: 20110209 |