CN101367035A - Preparation method for nano-titanium dioxide film photocatalyst - Google Patents
Preparation method for nano-titanium dioxide film photocatalyst Download PDFInfo
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Abstract
The invention relates to the technical field of photocatalyst, and discloses a method for preparing a nanometer titanium dioxide film photocatalyst through a sol gel method on the weak acid condition. The method comprises the following steps of: mixing and stirring the acetate solution of titanium acid dinbutyl phthalate and the alcohol solution of a non-ion type template agent to prepare titanium sol; and dipping and extracting a processed substrate, drying the substrate into a former body film, and calcining the former body film at a high temperature to obtain the nanometer titanium dioxide film photocatalyst. The method has a simple and easily controlled preparation process, the low cost of the preparation technology, little damage to equipment and environment, and no secondary pollution. The nanometer titanium dioxide film photocatalyst which is formed by compact and even nanometer level particles in ordered arrangement has the flat film and high photocatalysis efficiency. The nanometer titanium dioxide film photocatalyst can be repeatedly used with a certain practical application value.
Description
Technical field
The invention belongs to the technical field of photochemical catalyst, Prepared by Sol Gel Method nano titanium oxide (TiO under particularly a kind of mild acid conditions
2) preparation method of film photocatalyst.
Background technology
The photocatalysis technology that with the conductor oxidate is catalyst is one of focus of Environmental Studies over nearly 20 years.Utilizing aspects such as the method degraded water organic pollution of conductor photocatalysis oxidation and gaseous-phase organic pollutant all to carry out fruitful research, is a pollution control new technology that comes into one's own day by day in recent years.Titanium dioxide is stable owing to chemical property, anti-photoetch ability is strong, cost is low, nontoxic and photocatalytic activity advantages of higher has broad application prospects.The cost height that in environmental improvement, exists at the suspended phase photochemical catalyst, poor stability, difficultly reclaim and easily cause defective such as secondary pollution, preparation stable firmly and the immobilized titanium dioxide with high catalytic activity be that photocatalysis technology practicability is badly in need of the key issue that solves, also be late 1980s research focus so far.The preparation method of immobilized titanium dioxide is a lot, as sol-gel process, and metal organic chemistry vapour phase deposition process, cathode electrodeposition method, or directly powder titanium dioxide is fixed on the base material, wherein relatively typical case and sol-gel process effectively with heat/gluing method.
Sol-gel process is meant metal organic or inorganic compound through solution hydrolysis, colloidal sol, gel, curing, forms a kind of method of oxide or other solid again through Low Temperature Heat Treatment.In the preparation process of titanium dioxide, the too fast hydrolysis that suppresses organic or inorganic titanium source is an important step of preparation.Usually need to add the too fast hydrolysis that reagent such as acetylacetone,2,4-pentanedione or isopropyl alcohol suppress the titanium source in the building-up process, also need to use H simultaneously
2SO
4, HCl or HNO
3Deng strong acid as acid catalyst.But be to use strong acid catalyst to have two problems, the one, the formation speed of titanium gel is fast, wayward in the inorganic acid medium, and it is bigger to form product titanium dioxide particle diameter, causes the decline of photocatalyst activity; The 2nd, used strong acid has bigger pollution and corrosiveness to environment and experimental facilities.Therefore, conventional synthetic method is complicated, and organic reagent kind and amount used in the building-up process are all bigger, cause environmental pollution and unnecessary waste.In addition, there are defectives such as the crack that comes off easily in the titanium dioxide fixed film of conventional sol-gel process preparation.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the invention is to provide that the preparation load is firm under a kind of mild acid conditions, photocatalysis efficiency is high and the method for the nano-titanium dioxide film photocatalyst of applied range.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of nano-titanium dioxide film photocatalyst comprises the steps:
(1) 0.5～5.0g tetrabutyl titanate is dropwise joined in 5～100mL acetum, stir 1～24h, obtain the acetum of tetrabutyl titanate; The agent of 0.1～5.0g nonionic template is joined in 5～50mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join in the acetum of above-mentioned tetrabutyl titanate again, continue to stir 1～24h, obtain titanium colloidal sol, behind the ultrasonic dispersion 1～10min of titanium colloidal sol, ageing 12～48h obtains the titanium gel.
(2) matrix is cleaned up the back oven dry, immerse 0.1～30min in the above-mentioned titanium gel that makes, pulling film forming at 50～150 ℃ of oven dry 10～360min, obtains the precursor film.
(3) with the precursor film at 250～750 ℃ of high-temperature calcination 2～10h, can obtain nano-titanium dioxide film photocatalyst.
In order to realize the present invention better, in the step (1), described acetum is that by volume percentage is counted 5～80% acetum; Polyoxyethylene-poly-oxypropylene polyoxyethylene (P123) is selected in the agent of described nonionic template for use, also can select polyethylene glycol (PEG) or polyvinylpyrrolidone (PVP) etc. for use.In the step (2), described matrix comprises high temperature resistant materials such as tin indium oxide (ITO) coated glass, simple glass sheet, titanium plate, corrosion resistant plate, titanium net or nickel foam; The pull rate of described pulling film forming is 0.1～5mm/s.
The nano-titanium dioxide film photocatalyst that the present invention makes can be used in the actual treatment of waste water and waste gas.
The present invention compared with prior art has following advantage and beneficial effect:
The present invention reacts in the weakly acidic condition of gentleness according to the response characteristic of titanium alkoxide.Chelatropic reaction takes place in the affiliation that adds of acetic acid, acetate ion plays two ligand effects in the reaction, the polymer generation hydrolysis condensation reaction that generates forms three-dimensional space net structure, thereby play the effect that delays source hydrolysis of organic or inorganic titanium and polycondensation reaction, easy control of reaction conditions more helps the titanium gel and form structurally ordered titanium dioxide under the traction of template agent.Acetic acid has not only simultaneously also played the effect of acid catalyst as hydrolysis inhibitor in reaction, thereby has significantly reduced kind and the consumption for preparing required experiment reagent, and preparation technology meets requirements of green environmental protection.In addition, the photochemical catalyst efficient height that preparation technology of the present invention is simple, prepared, has certain actual application value at low price.The nano-titanium dioxide film photocatalyst of the present invention preparation is by fine and close, evenly and arrange orderly nano-scale particle and constitute, and film is smooth, photocatalysis efficiency height, but repeated multiple times utilization.Nano-titanium dioxide film photocatalyst of the present invention both can be used in degraded water organic pollution, and volatile organic contaminants such as airborne gas-phase benzene, toluene, formaldehyde and acetone also can be used for degrading.
Description of drawings
Fig. 1 is AFM (AFM) two dimension and the 3 d surface topography figure of the titanium dioxide film photocatalyst for preparing of the present invention.
Fig. 2 is AFM (AFM) the 3 d surface topography figure of the titanium dioxide film photocatalyst for preparing of the present invention.
Fig. 3 is that the film photocatalyst that the present invention prepares is schemed the photocatalytic degradation of water methyl orange is active.
Fig. 4 is that the film photocatalyst that the present invention prepares is schemed the photocatalytic degradation of vapor phase toluene is alive.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
(1) the 0.5g tetrabutyl titanate is dropwise joined 5mL by volume percentage count in 10% the acetum, continuous stirring 3h obtains the acetum of tetrabutyl titanate; 0.1g nonionic template agent (polyoxyethylene-poly-oxypropylene polyoxyethylene) is dissolved in the 5mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 1h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 5min, transfer to ageing 24h in the closed container, obtain the titanium gel.
(2) will cut out the ito coated glass that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 1min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 1mm/s at 120 ℃ of oven dry 10min, obtains the precursor film.
(3) precursor film program in Muffle furnace is warming up to 650 ℃ of high-temperature calcination 4h.Through XRD the structure of film is characterized, film is that the anatase titanium dioxide particle of 17.0nm constitutes by particle diameter, shows to have prepared nano-titanium dioxide film photocatalyst.
(1) the 2.0g tetrabutyl titanate is dropwise joined 10mL by volume percentage count in 50% the acetum, continuous stirring 8h obtains the acetum of tetrabutyl titanate; 0.3g nonionic template agent (polyoxyethylene-poly-oxypropylene polyoxyethylene) is dissolved in the 5mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 3h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 5min, transfer to ageing 48h in the closed container, obtain the titanium gel.
(2) will cut out the ito coated glass that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 5min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 4mm/s obtains the precursor film at 60 ℃ of oven dry 360min.
(3) precursor film program in Muffle furnace is warming up to 650 ℃ of high-temperature calcination 8h.Can obtain nano-titanium dioxide film photocatalyst.This film photocatalyst is that the anatase titanium dioxide particle of 18.2nm constitutes by particle diameter.
(1) the 5.0g tetrabutyl titanate is dropwise joined 100mL by volume percentage count in 10% the acetum, continuous stirring 6h obtains the acetum of tetrabutyl titanate; 0.3g nonionic template agent (polyethylene glycol) is dissolved in the 5mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 12h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 10min, transfer to ageing 1h in the closed container, obtain the titanium gel.
(2) will cut out the ito coated glass that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 10min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 4mm/s obtains the precursor film at 120 ℃ of oven dry 10min.
(3) precursor film program in Muffle furnace is warming up to 250 ℃ of high-temperature calcination 10h.Can obtain nano-titanium dioxide film photocatalyst.This film photocatalyst is that the anatase titanium dioxide particle of 14.4nm constitutes by particle diameter.
(1) the 1.5g tetrabutyl titanate is dropwise joined 50mL by volume percentage count in 5% the acetum, continuous stirring 3h obtains the acetum of tetrabutyl titanate; 2.0g nonionic template agent (polyoxyethylene-poly-oxypropylene polyoxyethylene) is dissolved in the 20mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 24h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 1min, transfer to ageing 24h in the closed container, obtain the titanium gel.
(2) will cut out the ito coated glass that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 1min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 1mm/s obtains the precursor film at 80 ℃ of oven dry 240min.
(3) precursor film program in Muffle furnace is warming up to 450 ℃ of high-temperature calcination 6h.Can obtain nano-titanium dioxide film photocatalyst.This film photocatalyst is that the anatase titanium dioxide particle of 15.9nm constitutes by particle diameter.
(1) the 3.0g tetrabutyl titanate is dropwise joined 80mL by volume percentage count in 40% the acetum, continuous stirring 1h obtains the acetum of tetrabutyl titanate; 5.0g nonionic template agent (polyoxyethylene-poly-oxypropylene polyoxyethylene) is dissolved in the 30mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 1h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 5min, transfer to ageing 12h in the closed container, obtain the titanium gel.
(2) will cut out the ito coated glass that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 30min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 0.1mm/s obtains the precursor film at 150 ℃ of oven dry 100min.
(3) precursor film program in Muffle furnace is warming up to 350 ℃ of high-temperature calcination 9h.Can obtain nano-titanium dioxide film photocatalyst.This film photocatalyst is that the anatase titanium dioxide particle of 15.1nm constitutes by particle diameter.
(1) the 2.0g tetrabutyl titanate is dropwise joined 30mL by volume percentage count in 80% the acetum, continuous stirring 12h obtains the acetum of tetrabutyl titanate; 2.0g nonionic template agent (polyoxyethylene-poly-oxypropylene polyoxyethylene) is dissolved in the 10mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 2h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 5min, transfer to ageing 24h in the closed container, obtain the titanium gel.
(2) will cut out the ito coated glass that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 10min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 4mm/s obtains the precursor film at 120 ℃ of oven dry 10min.
(3) precursor film program in Muffle furnace is warming up to 750 ℃ of high-temperature calcination 2h.Can obtain nano-titanium dioxide film photocatalyst.This film photocatalyst is that the anatase titanium dioxide particle of 19.6nm constitutes by particle diameter.
Embodiment 7
(1) the 1.0g tetrabutyl titanate is dropwise joined 50mL by volume percentage count in 60% the acetum, continuous stirring 3h obtains the acetum of tetrabutyl titanate; 2.0g nonionic template agent (polyoxyethylene-poly-oxypropylene polyoxyethylene) is dissolved in the 50mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 12h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 5min, transfer to ageing 1h in the closed container, obtain the titanium gel.
(2) will cut out the simple glass that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 3min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 2mm/s obtains the precursor film at 50 ℃ of oven dry 360min.
(3) precursor film program in Muffle furnace is warming up to 250 ℃ of high-temperature calcination 10h.Can obtain nano-titanium dioxide film photocatalyst.This film photocatalyst is that the anatase titanium dioxide particle of 14.1nm constitutes by particle diameter.
(1) the 4.0g tetrabutyl titanate is dropwise joined 100mL by volume percentage count in 40% the acetum, continuous stirring 8h obtains the acetum of tetrabutyl titanate; 2.0g nonionic template agent (polyoxyethylene-poly-oxypropylene polyoxyethylene) is dissolved in the 40mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 12h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 5min, transfer to ageing 12h in the closed container, obtain the titanium gel.
(2) will cut out the titanium plate that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 8min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 0.5mm/s obtains the precursor film at 100 ℃ of oven dry 120min.
(3) precursor film program in Muffle furnace is warming up to 550 ℃ of high-temperature calcination 5h.Can obtain nano-titanium dioxide film photocatalyst.This film photocatalyst is that the anatase titanium dioxide particle of 16.7nm constitutes by particle diameter.
(1) the 1.0g tetrabutyl titanate is dropwise joined 10mL by volume percentage count in 20% the acetum, continuous stirring 8h obtains the acetum of tetrabutyl titanate; 2.0g nonionic template agent (polyvinylpyrrolidone) is dissolved in the 40mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join again and continue to stir 6h in the acetum of above-mentioned tetrabutyl titanate, obtain titanium colloidal sol, behind the ultrasonic dispersion of titanium colloidal sol 5min, transfer to ageing 24h in the closed container, obtain the titanium gel.
(2) will cut out the corrosion resistant plate that is of a size of 12 * 5.7cm in advance and clean up the back oven dry, and immerse 5min in the above-mentioned titanium gel that makes, the pull rate dipping pulling film forming with 5mm/s obtains the precursor film at 120 ℃ of oven dry 10min.
(3) precursor film program in Muffle furnace is warming up to 750 ℃ of high-temperature calcination 2h.Can obtain nano-titanium dioxide film photocatalyst.This film photocatalyst is that the anatase titanium dioxide particle of 19.1nm constitutes by particle diameter.
Comparing embodiment
Nano-titanium dioxide film photocatalyst characterizes
Fig. 1 and Fig. 2 (nano-titanium dioxide film photocatalyst of embodiment 1 preparation) are respectively the two and three dimensions shape appearance figure that AFM is taken.Can see the TiO that draws the nano-titanium dioxide film photocatalyst surface by figure
2Average grain diameter is about 18.0nm, and the mean roughness of film (Ra) only is 3.65nm, and maximum height difference (Rmax) is 15.92nm.As seen from the figure, the nano-titanium dioxide film photocatalyst of the present invention's preparation is to be made of the fine spherical grains nano particle, complete in crystal formation, and the surfacing densification, roughness is little.
In order to screen the photocatalytic activity of nano-titanium dioxide film photocatalyst better, examined or check the actual light catalytic degradation effect of preparation film.At first be target contaminant with the methyl orange solution, device is the quartz reaction groove of a volume 100mL, is equipped with air pump and plays the effect that aeration is held concurrently and mixed, and aeration rate is 0.15m
3/ h.With 125W high-pressure sodium lamp (GGZ300, the inferior bright lighting apparatus in Shanghai Co., Ltd, E
Max=365nm) as light source, the quartz reaction slot pitch is from light source 20cm place, and a solar panel is equipped with in the light source back.With the titanium dioxide film photocatalyst for preparing under the different condition, identical (12 * 5.7cm) the film photocatalyst of a slice load area is used in every group reaction.Methyl orange initial concentration 10mL/L, volume 90mL, after the adsorption-desorption balance, light-catalyzed reaction 60min.The adsorbance of methyl orange solution on film is very little, the 15min adsorption equilibrium.As shown in Figure 3, light-catalyzed reaction 60min, the film photocatalyst that embodiment 1～9 (1# represents the film photocatalyst of embodiment 1 preparation, and 2# represent the film photocatalyst of embodiment 2 preparations, and the like) prepares is 78.6～98.9% to the photocatalytic degradation rate of methyl orange.
In a volume is the gas-solid phase photo catalysis reactor of 5L, the photocatalytic degradation activity of film photocatalyst in gas phase of the present invention's preparation investigated simultaneously.Every group with two TiO
2(12 * 5.7cm) is photochemical catalyst to/ITO, and dry air is the organic matter carrier, mixes by fan, inject 5uL toluene and 200uL distilled water when reaction, wait after the full volatilization in reactor, 180min reaches the adsorption-desorption balance, toluene initial concentration 0.6mg/L, relative humidity 45%.With 125W (365nm) high-pressure sodium lamp is light source, and light-catalyzed reaction 60min photodissociation rate is 13.4%.As shown in Figure 4, (1# represents the film photocatalyst of embodiment 1 preparation to embodiment 1～9,2# represents the film photocatalyst of embodiment 2 preparation, and the like) film photocatalyst of preparation is 50～100% to the photocatalytic degradation rate scope of vapor phase toluene, reaches as high as 100%.
Film photocatalyst according to photocatalytic degradation description of test the present invention of liquid phase methyl orange and vapor phase toluene preparation all has treatment effect preferably to water and vapor phase contaminants.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spiritual essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. the preparation method of a nano-titanium dioxide film photocatalyst is characterized in that comprising the steps:
(1) 0.5～5g tetrabutyl titanate is dropwise joined in 5～100mL acetum, stir 1～24h, obtain the acetum of tetrabutyl titanate; The agent of 0.1～5.0g nonionic template is joined in 5～50mL absolute ethyl alcohol, be stirred to dissolving, obtain the ethanolic solution of nonionic template agent, dropwise join in the acetum of above-mentioned tetrabutyl titanate again, continue to stir 1～24h, obtain titanium colloidal sol, behind the ultrasonic dispersion 1～10min of titanium colloidal sol, ageing 12～48h obtains the titanium gel;
(2) matrix is cleaned up the back oven dry, immerse 0.1～30min in the above-mentioned titanium gel that makes, pulling film forming obtains the precursor film at 50～150 ℃ of oven dry 10～360min;
(3) with the precursor film at 250～750 ℃ of high-temperature calcination 2～10h, can obtain nano-titanium dioxide film photocatalyst.
2. the preparation method of a kind of nano-titanium dioxide film photocatalyst according to claim 1, it is characterized in that: in the step (1), described acetum is that by volume percentage is counted 5～80% acetum.
3. the preparation method of a kind of nano-titanium dioxide film photocatalyst according to claim 1, it is characterized in that: in the step (1), the agent of described nonionic template is polyoxyethylene-poly-oxypropylene polyoxyethylene, polyethylene glycol or polyvinylpyrrolidone.
4. the preparation method of a kind of nano-titanium dioxide film photocatalyst according to claim 1, it is characterized in that: in the step (2), described matrix is indium oxide coating glass, simple glass sheet, titanium plate, corrosion resistant plate, titanium net or nickel foam.
5. the preparation method of a kind of nano-titanium dioxide film photocatalyst according to claim 1, it is characterized in that: in the step (2), the pull rate of described pulling film forming is 0.1～5mm/s.
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| CN118502046A (en) * | 2024-07-16 | 2024-08-16 | 江苏亨通光电股份有限公司 | Bending insensitive butterfly cable and preparation method thereof |
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