CN103657628A - Preparation method of SnO2-TiO2 composite nano photocatalyst - Google Patents
Preparation method of SnO2-TiO2 composite nano photocatalyst Download PDFInfo
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Abstract
A preparation method of a SnO2-TiO2 composite nano photocatalyst comprises operation steps as follows: (1), mixing tetrabutyl titanate, absolute ethyl alcohol and glacial acetic acid, adding dilute nitric acid to regulate pH, stirring and adding water; (2) adding a SnCl4*5H2O solution into the mixed solution in a molar ratio of titanium to tin to be 3:1, stirring, and aging for 22-26 h; (3) placing the aged material into an autoclave for treatment for 22-25 h at the temperature of 175-185 DEG C, and cooling the material in the autoclave to the room temperature; and (4) performing centrifugal separation on a product, then drying the product at 95-110 DEG C and roasting the product for 2-6 h to obtain a finished product. The SnO2-TiO2 composite nano photocatalyst prepared with the method has higher purity and activity, good dispersibility, high thermostability and good repeatability; the method does not require addition of a surfactant and the like, so that the cost is lower, and the production cost is reduced greatly; and meanwhile, the production time is shortened to 2-3 d, and further, the operation is simple and safe.
Description
Technical field
The invention belongs to nano material and photocatalysis technology field, relate to a kind of SnO
2-TiO
2the preparation method of composite Nano photochemical catalyst.
Background technology
TiO
2being commonly called as titanium dioxide, is a kind of semi-conducting material of N-shaped, and energy gap is 3.2eV.Because it has high-specific surface area, inexpensive nontoxic, photoelectric properties are strong, and therefore catalytic activity advantages of higher becomes the current photochemical catalyst that has application potential most.But, TiO
2inherent physical characteristic determine that it is very low to solar energy utilization ratio, electron-hole recombination rate is high, causes photocatalytic activity greatly to reduce.Therefore, by TiO
2carry out modification its wavelength exciting is expanded to visible ray from ultraviolet ray, the electron-hole that slows down compound, increases photocatalysis efficiency, has become scientist's research emphasis.At present, in order to realize this goal, adopt multiple different technologies to TiO
2carry out modification or doping, to improve its photocatalytic activity.As at TiO
2metal surface containing transition metal, nonmetal, surface deposition noble metal, surface sensitization processing and semiconductor are compound etc.Semiconductor is compound is mainly to utilize two kinds of semiconductors that bandwidth is different but close compound, so not only can make photo-generated carrier transport between different energy level carriers, and extended life-span of carrier, avoided to a great extent the compound of carrier, improve the separation rate of carrier, thereby improved the photocatalytic activity of system.
SnO
2also be a kind of typical N-shaped semiconductor, its energy gap 3.5～3.6eV, stable chemical nature, its energy level and semiconductor TiO
2match, and SnO
2with TiO
2conduction level between difference cause SnO
2and TiO
2after compound, light induced electron is from TiO
2shift and at SnO on surface
2upper enrichment, the corresponding TiO that reduced
2the density of surface electronic, light induced electron can be effectively separated with hole, also just reduced the right recombination probability in light induced electron-hole, can greatly improve TiO
2photocatalytic activity, for this reason we wish by research nano-TiO
2with SnO
2the composite forming effectively reduces right compound in light induced electron-hole, thereby improves quantum yield, widens ultraviolet-visible absorption spectroscopy simultaneously, reaches the object that improves photocatalytic activity.
Nano-photocatalyst is the jinx of pollutant, its mechanism of action is: it is right that nano-photocatalyst is excited to generate " electron-hole " under the irradiation of special wavelength light, after this " electron-hole " has an effect to the water with around, oxygen, there is extremely strong oxidation-reducing power, the pollutant such as formaldehyde, benzene in air directly can be resolved into harmless tasteless material.Under illumination, if the energy of photon is greater than semiconductor energy gap, the electronics (e in its valence band
-) will be excited on conduction band, in valence band, produce hole (h simultaneously
+).Photohole has very strong oxidability, and light induced electron has very strong reducing power, and they can move to the diverse location of semiconductor surface, with the pollutant generation redox reaction of adsorption.
At present, make SnO
2and TiO
2compound technological means has a variety of, coprecipitation wherein, sol-gal process, hydro-thermal method are all very typical conventional methods, the preparation of many nano materials is all to be prepared or prepared by the method for prolonging Shen or combining of these methods by these methods, therefore, they play a very important role in the preparation of solid catalysis agent material and research.
Sol-gel process is that the slaine of some facile hydrolysis is made to colloidal sol through chemical reactions such as hydrolysis and polycondensations, then colloidal sol is converted into gel, then by roasting, obtains the method for nano-powder.The method synthesis temperature is low, and process is easy to control; Technique is simply beneficial to batch production, and the powder making has the chemical composition uniformity of height, high-purity property, ultra-fine property etc.
The hot method of sol-solvent is directly to transfer to and in autoclave, carry out solvent thermal reaction forming colloidal sol before gel in sol-gal process.
The precipitation method are a kind of methods of preparing solid catalyst of classics and extensive use, nearly all solid catalyst has at least a part to be prepared by the precipitation method, coprecipitation is the method that two or more required components of catalyst are precipitated under the effect of precipitating reagent simultaneously, be characterized in once can obtaining several components simultaneously, and the distribution of each component is more even, if can form solid solution between each component, better to the absorbability of light so.
Co-precipitation-hydro-thermal method is that the component that forms precipitation is directly transferred to and in autoclave, carried out hydro-thermal reaction.
Hydro-thermal method is in sealed reactor, using the aqueous solution as reaction medium, heating reaction vessel, create reaction under high pressure environment, at normal temperatures and pressures, in solution, be difficult for oxidized material or be difficult for synthetic material, by system being placed in to get off a kind of material preparation method of carrying out of accelerated reaction of the high-temperature and high-pressure conditions of sealing.The technology and equipment of hydro-thermal method is simple, is easy to control, and without high temperature sintering, processes, and product is directly crystalline state.
Existing bibliographical information is prepared SnO by these methods
2-TiO
2composite Nano photochemical catalyst, but the catalyst activity that these methods prepare is not high, makes reaction effect bad; When separately with the precipitation method or hydro-thermal method Kaolinite Preparation of Catalyst, the presoma using is titanium tetrachloride, during the decomposes of titanium tetrachloride reaction violent, there is a large amount of dense smoke, make course of reaction more dangerous; Prior art is prepared SnO
2-TiO
2during composite catalyst, need to add the materials such as surfactant, cause production cost higher, meanwhile, general 4～5d consuming time in this catalyst process of preparation, the time is oversize.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, invent a kind of SnO of preparation
2-TiO
2the method of composite Nano photochemical catalyst, makes obtained catalyst have high activity, high stability; Meanwhile, the inventive method reaction time is short, catalyst is reproducible; Further, the present invention has reduced production cost, makes simple to operate, safety.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of SnO
2-TiO
2the preparation method of composite Nano photochemical catalyst, comprises following operating procedure:
(1) butyl titanate, absolute ethyl alcohol, glacial acetic acid are mixed, then adding rare nitre acid for adjusting pH value is 2～4, stirs 10～20min, adds water and stirs, standing;
(An Tai ︰ tin mol ratio, to be 3 ︰ 1 add SnCl to solution after mixing in step (1) to 2)
45H
2o solution, stirs, then ageing 22～26h;
(3) material after ageing in step (2) is put into autoclave and keep 175～185 ℃ of constant temperature to process 22～25h, then make material in autoclave be cooled to room temperature;
(4) by products therefrom centrifugation in step (3), at 95～110 ℃, dry, then roasting 2～6h at 500～600 ℃, obtains product.
A kind of SnO
2-TiO
2the preparation method of composite Nano photochemical catalyst, its more detailed step is as follows:
(1) butyl titanate, absolute ethyl alcohol, glacial acetic acid are mixed, under continuous stirring state, dropwise adding rare nitre acid for adjusting pH value is 2～4, stirs 10～20min, adds water and then continues to stir, standing;
(An Tai ︰ tin mol ratio, to be 3 ︰ 1 add SnCl to solution after mixing in step (1) to 2)
45H
2o solution, stirs, then ageing 22～26h;
(3) material after ageing in step (2) is put into autoclave and keep 175～185 ℃ of constant temperature to process 22～25h, then make material in autoclave be cooled to room temperature;
(4) by products therefrom centrifugation after ageing 22～25h in step (3), at 95～110 ℃, dry, then roasting 2～6h at 500～600 ℃, obtains product.
The volume ratio of the butyl titanate preferably, adding in step (1), absolute ethyl alcohol, glacial acetic acid, rare nitric acid, water is 3～5 ︰ 14～21 ︰ 1 ︰ 1～3 ︰ 1～3.
The volume ratio of the butyl titanate preferably, adding in step (1), absolute ethyl alcohol, glacial acetic acid, rare nitric acid, water is 4 ︰ 17 ︰ 1 ︰ 2 ︰ 2.
Preferably, the rare nitric acid described in step (1) is that nitric acid and water volume ratio are the diluted nitric acid aqueous solution of 1 ︰ 10.
Preferably, described water is deionized water or distilled water.
Preferably, SnCl used in step (2)
45H
2the molar concentration of O solution is 1.4mol/L.
Preferably, in step (1), adding water mixing time is 10min, and time of repose is 30min.
Preferably, after drying in step (4), after product is pulverized, then carry out roasting at 95～110 ℃.
The present invention is the SnO preparing under sol-gel process and solvent-thermal method compound action
2-TiO
2composite Nano photochemical catalyst, makes the degree of polymerization between colloidal sol good, and prepared catalyst purity, activity are higher, good dispersion, and heat endurance is strong, reproducible; Further the present invention does not need to add in addition the activating substances such as surfactant, makes cost lower, has reduced greatly production cost; Production time shortens to 2～3d simultaneously, and simple to operate, safety; Gentleness comparatively when the presoma that further the inventive method is used react for butyl titanate, makes in production process danger lower, is of value to expansion suitability for industrialized production.
Accompanying drawing explanation
Accompanying drawing 1 is 5 kinds of SnO prepared by distinct methods
2-TiO
2composite Nano photochemical catalyst XRD collection of illustrative plates.
Accompanying drawing 2 is the SnO of sol-solvent hot preparation
2-TiO
2the scanning electron microscope diagram sheet of composite Nano photochemical catalyst.
Accompanying drawing 3 is 5 kinds of SnO prepared by distinct methods
2-TiO
2the photocatalytic degradation design sketch of composite Nano photochemical catalyst.
The specific embodiment
Referring to the specific embodiment, further describe the present invention, to make those skilled in the art can implement according to this with reference to description word, protection domain of the present invention is not limited by embodiments of the present invention.In an embodiment, experiment component is three groups to carry out, and is respectively embodiment 1, embodiment 2, embodiment 3; Contrast test is divided into two groups, is respectively embodiment 4, embodiment 5.Wherein s-g represents sol-gel process, and s-hyth is the hot method of sol-solvent (being two kinds of compound methods of sol-gel process and solvent-thermal method), and cop is coprecipitation, and cop-hyth is co-precipitation-hydro-thermal method, and hyth is hydro-thermal method.
Embodiment 1
6ml tetra-n-butyl titanate, 25ml absolute ethyl alcohol, 1.5ml glacial acetic acid are mixed, under constantly stirring, dropwise add the rare nitric acid (of 3ml Xiao Suan ︰ water=1 ︰ 10) to regulate pH value be 3, continue to stir after 15min, add 3ml deionized water, stir 10min, standing 30min then, is that to add 4ml molar concentration be the SnCl of 1.4mol/L to 3 ︰ 1 again An Tai ︰ tin mol ratio again
45H
2o solution, stirs, and ageing 24h makes slowly polymerization between colloidal sol.Colloidal sol after ageing is transferred in autoclave at 180 ℃ of constant temperature and processed 24h, then make product in autoclave be cooled to room temperature, products therefrom is carried out to centrifugation, after separation, at 100 ℃, dry, grind into powder then, identified as samples is designated as s-hyth.By powder 550 ℃ of roasting 4h in Muffle furnace, obtain SnO
2-TiO
2solid solution.
Embodiment 2
6ml tetra-n-butyl titanate, 28ml absolute ethyl alcohol, 2.0ml glacial acetic acid are mixed, under constantly stirring, dropwise add the rare nitric acid (of 3ml Xiao Suan ︰ water=1 ︰ 10) to regulate pH value be 2, continue to stir after 15min, add 1ml deionized water, stir 10min, standing 30min then, by titanium: tin mol ratio is that to add 4ml molar concentration be the SnCl of 1.4mol/L to 3 ︰ 1 again again
45H
2o solution, stirs, and ageing 22h makes slowly polymerization between colloidal sol.Colloidal sol after ageing is transferred in autoclave and processed 22h at 175 ℃ of constant temperature, then make product in autoclave be cooled to room temperature, products therefrom is carried out to centrifugation, after separation, at 95 ℃, dry, then grind into powder, by powder 500 ℃ of roasting 6h in Muffle furnace, obtains SnO
2-TiO
2solid solution.
Embodiment 3
12.5ml tetra-n-butyl titanate, 52.5ml absolute ethyl alcohol, 2.5ml glacial acetic acid are mixed, under constantly stirring, dropwise add the rare nitric acid of 2.5ml (nitric acid: water=1 ︰ 10) regulating pH value is 4, continue to stir after 15min, add 7.5ml distilled water, stir 10min, standing 30min then, by titanium: tin mol ratio is that to add 4ml molar concentration be the SnCl of 1.4mol/L to 3 ︰ 1 again again
45H
2o solution, stirs, and ageing 26h makes slowly polymerization between colloidal sol.Colloidal sol after ageing is transferred in autoclave and processed 25h at 185 ℃ of constant temperature, then make product in autoclave be cooled to room temperature, products therefrom is carried out to centrifugation, after separation, at 110 ℃, dry, then grind into powder, by powder 600 ℃ of roasting 2h in Muffle furnace, obtains SnO
2-TiO
2solid solution.
Embodiment 4
6ml tetra-n-butyl titanate, 25ml absolute ethyl alcohol, 1.5ml glacial acetic acid are mixed, under constantly stirring, dropwise add the rare nitric acid (of 3ml Xiao Suan ︰ water=1 ︰ 10) to pH=3, continue to stir after 15min, then in mixed liquor after stirring, add 3ml deionized water, stir 10min, standing 30min, then to add 4ml molar concentration be the SnCl of 1.4mol/L
45H
2o solution, stirs, and stirs, and then ageing 24h, makes slowly polymerization between colloidal sol.Ready colloidal sol is dried in 100 ℃ of baking ovens, and then by drying and grinding into powder, identified as samples is designated as s-g.By gained powder 550 ℃ of roasting 4h in Muffle furnace, obtain SnO
2-TiO
2solid solution.
Embodiment 5
The following three parts of identical mixed solutions of preparation: by mol ratio Wei Tai ︰ Xi ︰ urea=3 ︰ 1 ︰ 60 of each material, the TiCl that is 2mol/L by 8ml concentration
4solution and 4ml concentration are 1.4mol/LSnCl
45H
2o solution mixes, and stirs 30min, and then adding 75ml concentration is the urea liquid of 6mol/L, stirs 1h.Above-mentioned three parts of identical mixed solutions are labeled as respectively to cop, cop-hyth, hyth, cop, two parts of mixed solutions of cop-hyth are being continued under the condition stirring in 80 ℃ of oil bath pans, isothermal reaction 8h, makes mixed solution precipitation completely; Then by completely the cop of precipitation put at room temperature cooling, ageing 24h, by products therefrom washing, centrifugal, at 60 ℃, dry, then will dry material grind into powder afterwards, standby; The turbid solution that is masked as cop-hyth is put into autoclave and in 180 ℃ of constant temperature, process 24h, then make product in autoclave be cooled to room temperature, by products therefrom washing, centrifugal, at 60 ℃, dry, then grind into powder, standby; The mixed solution that is masked as hyth is directly put into autoclave, and at 180 ℃, constant temperature is processed 24h, then makes product in autoclave be cooled to room temperature, by products therefrom washing, centrifugal, at 60 ℃, dry, and material grind into powder after then drying, standby; Each powder of above-mentioned gained is placed on respectively to 550 ℃ of roasting 4h in Muffle furnace, obtains sign and be respectively: the SnO of cop, cop-hyth, hyth
2-TiO
2solid solution.
At accompanying drawing 1, be catalyst crystalline phases variation diagram, as can be seen from the figure the crystal formation of obtained catalyst is pure rutile type; In accompanying drawing 2, can find out, the hot gained catalyst of sol-solvent form is comparatively unified, and each molecular distribution is good; In accompanying drawing 3, can find out, by above-mentioned 5 kinds of methods, prepare gained catalyst, under applying to ultraviolet light in the reaction of catalytic degradation methyl blue, all shown activity, especially best with the prepared catalyst activity of the hot method of sol-solvent, due to by the preparation of this method, make the polymerization between colloidal sol relatively good, obtain the less particle of particle diameter, there is larger specific area, more adsorption site.Higher photocatalytic activity may be by changing its electronic structure, improves Surface Oxygen hole number and surface hydroxyl number.Thereby make obtained catalyst activity better, higher than conventional method, prepare gained SnO far away
2-TiO
2composite Nano photochemical catalyst.
The present invention is the SnO preparing under sol-gel process and solvent-thermal method compound action
2-TiO
2composite Nano photochemical catalyst, makes the degree of polymerization between colloidal sol good, and prepared catalyst purity, activity are higher, good dispersion, and heat endurance is strong, reproducible; Further the present invention does not need to add in addition the activating substances such as surfactant, makes cost lower, has reduced greatly production cost; Production time shortens to 2～3d simultaneously, and simple to operate, safety; Gentleness comparatively when the presoma that further the inventive method is used react for butyl titanate, makes in production process danger lower, is of value to expansion suitability for industrialized production.
Claims (8)
1. a SnO
2-TiO
2the preparation method of composite Nano photochemical catalyst, is characterized in that, comprises following operating procedure:
(1) butyl titanate, absolute ethyl alcohol, glacial acetic acid are mixed, then adding rare nitre acid for adjusting pH value is 2～4, stirs 10～20min, adds water and stirs, standing;
(An Tai ︰ tin mol ratio, to be 3 ︰ 1 add SnCl to solution after mixing in step (1) to 2)
45H
2o solution, stirs, then ageing 22～26h;
(3) material after ageing in step (2) is put into autoclave and keep 175～185 ℃ of constant temperature to process 22～25h, then make material in autoclave be cooled to room temperature;
(4) by products therefrom centrifugation in step (3), at 95～110 ℃, dry, then roasting 2～6h at 500～600 ℃, obtains product.
2. SnO according to claim 1
2-TiO
2the preparation method of composite Nano photochemical catalyst, is characterized in that: the volume ratio of the butyl titanate adding in step (1), absolute ethyl alcohol, glacial acetic acid, rare nitric acid, water is 3～5 ︰ 14～21 ︰ 1 ︰ 1～3 ︰ 1～3.
3. SnO according to claim 1
2-TiO
2the preparation method of composite Nano photochemical catalyst, is characterized in that: the volume ratio of the butyl titanate adding in step (1), absolute ethyl alcohol, glacial acetic acid, rare nitric acid, water is 4 ︰ 17 ︰ 1 ︰ 2 ︰ 2.
4. SnO according to claim 1
2-TiO
2the preparation method of composite Nano photochemical catalyst, is characterized in that: the rare nitric acid described in step (1) is that nitric acid and water volume ratio are 1 ︰ 10.
5. SnO according to claim 1
2-TiO
2the preparation method of composite Nano photochemical catalyst, is characterized in that: described water is deionized water or distilled water.
6. SnO according to claim 1
2-TiO
2the preparation method of composite Nano photochemical catalyst, is characterized in that: SnCl used in step (2)
45H
2the molar concentration of O solution is 1.4mol/L.
7. SnO according to claim 1
2-TiO
2the preparation method of composite Nano photochemical catalyst, is characterized in that: in step (1), adding water mixing time is 10min, and time of repose is 30min.
8. SnO according to claim 1
2-TiO
2the preparation method of composite Nano photochemical catalyst, is characterized in that: after drying at 95～110 ℃ in step (4), after product is pulverized, then carry out roasting.
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| CN105086305A (en) * | 2015-08-31 | 2015-11-25 | 南宁市聚祥塑料制品有限责任公司 | Antibacterial preservative film |
| CN105199411A (en) * | 2015-08-31 | 2015-12-30 | 南宁市聚祥塑料制品有限责任公司 | Method for making mooncake support plastic box |
| CN107952289A (en) * | 2016-10-17 | 2018-04-24 | 秦素洁 | A kind of filter screen with purifying formaldehyde and preparation method thereof |
| CN107952367A (en) * | 2016-10-17 | 2018-04-24 | 秦素洁 | A kind of porous material for high-efficient purification formaldehyde and preparation method thereof |
| CN111617792A (en) * | 2020-04-26 | 2020-09-04 | 中国科学院化学研究所 | B, N codoped SnO responding to visible light2/TiO2Precursor and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105086305A (en) * | 2015-08-31 | 2015-11-25 | 南宁市聚祥塑料制品有限责任公司 | Antibacterial preservative film |
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| CN107952289A (en) * | 2016-10-17 | 2018-04-24 | 秦素洁 | A kind of filter screen with purifying formaldehyde and preparation method thereof |
| CN107952367A (en) * | 2016-10-17 | 2018-04-24 | 秦素洁 | A kind of porous material for high-efficient purification formaldehyde and preparation method thereof |
| CN111617792A (en) * | 2020-04-26 | 2020-09-04 | 中国科学院化学研究所 | B, N codoped SnO responding to visible light2/TiO2Precursor and preparation method and application thereof |
| CN111617792B (en) * | 2020-04-26 | 2021-08-03 | 中国科学院化学研究所 | B, N codoped SnO responding to visible light2/TiO2Precursor and preparation method and application thereof |
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