CN102744059B - Preparation method of ordered mesoporous titania/silver photocatalyst - Google Patents
Preparation method of ordered mesoporous titania/silver photocatalyst Download PDFInfo
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- CN102744059B CN102744059B CN201210245316.8A CN201210245316A CN102744059B CN 102744059 B CN102744059 B CN 102744059B CN 201210245316 A CN201210245316 A CN 201210245316A CN 102744059 B CN102744059 B CN 102744059B
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Abstract
The invention discloses a preparation method of ordered mesoporous titania/silver photocatalyst, relating to a preparation method of titania/silver and aiming to solve the technical problems of small specific surface area, poor orderliness and low photocatalytic activity of mesoporous titania/silver photocatalyst prepared by prior arts. The preparation method comprises the steps of silver solution preparation, titanium precursor preparation, titania/silver gel preparation, and heat treatment. The inventive photocatalyst has specific surface area of 120-160 m<2>/g, has the advantages of uniform mesopores and high catalytic activity; can be applied to photocatalysis field, and water treatment field of lake, ocean, municipal sewage and industrial sewage.
Description
Technical field
The present invention relates to the preparation method of titanium dioxide/silver-colored photochemical catalyst.
Background technology
TiO
2the processing that is used for environmental contaminants as photochemical catalyst is one of focus of research in recent years.Wherein mesoporous TiO 2 has larger specific area.Thereby make its surface can adsorb more water and hydroxyl, and the water of adsorption and hydroxyl can the hydroxyl radical free radical that generation strong oxidizing property is reacted in hole occur with light, they are main species of photocatalysis degradation organic contaminant.In addition mesoporous TiO,
2flourishing orderly mesopore orbit is more conducive to the diffusion of reactant and product, therefore can greatly improve photocatalytic activity.But TiO
2band gap (3.2eV) wider, spectral response range is narrower, absorbing wavelength mainly concentrates on ultraviolet region (< 387.5nm), and the recombination rate of its photo-generated carrier is higher, causes quantum efficiency low, to TiO
2carry out doping vario-property, strengthen its photocatalytic activity.Surface noble metal loading is the effective way that reduces photo-generated carrier recombination rate, and conventional noble metal has Pt, Au, Ag, Pd and Ru.
Titania modified by Argentine toxicity is relatively little, and cost is lower, thereby obtains people's broad research.The preparation method of the composite of mesoporous TiO 2/silver has hydro-thermal method, nanometer casting, electrodeposition process and wet infusion process at present, the cost of above-mentioned these methods is high, complex process, productive rate is low, equipment needed thereby is expensive, and the specific area of the composite of the mesoporous TiO 2/silver of preparation is at 100m
2below/g, specific surface is little, and the order in hole is poor, thereby causes photocatalytic activity low.
Summary of the invention
The present invention will solve that existing titanium dioxide/silver composite material specific area is little, order is poor, thereby causes the technical problem that photocatalytic activity is low, and the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst is provided.
The preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst of invention carries out according to the following steps:
One, take surfactant, solvent, strong oxidizer, Yin Yuan, wherein the mass ratio of surfactant and solvent is 0.01～0.25: 1, the mass ratio of strong oxidizer and surfactant is 0.05～0.2: 1, and the mass ratio of silver-colored source and surfactant is 0.001～0.2: 1; Then by the surfactant dissolves taking in solvent, then add strong oxidizer, stir after 0.5～36 hour, then add in ，Yu darkroom, silver-colored source and stir 1～24 hour, obtain silver-colored solution;
Two, take titanium source and solvent, wherein the mass ratio of titanium source and solvent is 0.025～0.2: 1, then titanium source is added in solvent, stirs 0.5～36 hour, obtains titanium precursor body;
Three, measure titanium precursor body prepared by silver-colored solution prepared by step 1 and step 2 and join in container, stir 0.5～24 hour, then room temperature ageing, dries, obtain titanium dioxide/silver gel, wherein the mass ratio in the silver-colored source in silver-colored solution and the titanium source in titanium precursor body is 0.001～0.5;
Four, titanium dioxide/silver gel step 3 being obtained is put into roasting in Muffle furnace, and sintering temperature is 300～900 ℃, obtains ordered mesoporous titanium dioxide/silver-colored photochemical catalyst.
Surfactant described in step 1 is that a kind of in triblock copolymer (P123, F127), polyvinylpyrrolidone (PVP), lauryl sodium sulfate (SDS), softex kw (CTAB), acrylonitrile-butadiene-styrene copolymer (ABS), PEI (PEI), Brij-35 (Brij-35), polyethylene glycol (PEG-400) and triethanolamine (TEA) or both mix in any proportion.
Strong oxidizer described in step 1 is KNO
3, KMnO
4, K
2cr
2o
7, KClO
3, MnO
2, HClO, H
2o
2, dense H
2sO
4, dense HNO
3with a kind of or two kinds of mixing in any proportion in chloroazotic acid.
Solvent described in step 1 is a kind of or two kinds of mixing in any proportion in deionized water, ethanol, isopropyl alcohol and n-butanol.
Silver-colored source described in step 1 is silver nitrate or silver ammino solution.
Solvent described in step 2 is a kind of of deionized water, methyl alcohol, ethanol, isopropyl alcohol and the tert-butyl alcohol or wherein several mixing.
Titanium source described in step 2 is titanyl sulfate, titanium tetrachloride, titanium sulfate, butyl titanate, isopropyl titanate or tetraethyl titanate.
The ordered mesoporous titanium dioxide that the present invention is prepared with sol-gal process/silver-colored photochemical catalyst is Anatase, is conducive to the raising of the separative efficiency in light induced electron and hole, is suitable for photocatalyst, and its specific area is 120～160m
2/ g.Deposition of silver is in TiO
2surface can cause the redistribution of carrier, can suppress the compound of light induced electron and hole, thereby the photocatalysis of raising catalyst is lived and had good dispersiveness, effectively catalyze and degrade organic pollutants.And the mesoporous aperture of ordered mesoporous titanium dioxide of the present invention/silver-colored photochemical catalyst homogeneous, duct is flourishing, and order is high, is beneficial to the diffusion of reactant and product.Preparation technology of the present invention is simple, cost is low, environmental pollution is little, equipment needed thereby is simple, and is easy to realize commercialization.Can be applicable to photocatalysis field.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the ordered mesoporous titanium dioxide/silver-colored photochemical catalyst of embodiment 1 preparation;
Fig. 2 is the N of the ordered mesoporous titanium dioxide/silver-colored photochemical catalyst of embodiment 1 preparation
2adsorption-desorption isollaothermic chart;
Fig. 3 is the pore size distribution curve figure of the ordered mesoporous titanium dioxide/silver-colored photochemical catalyst of embodiment 1 preparation;
Fig. 4 is the TEM photo of the ordered mesoporous titanium dioxide/silver-colored photochemical catalyst of embodiment 1 preparation.
The specific embodiment
The specific embodiment one: the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst of this specific embodiment carries out according to the following steps:
One, take surfactant, solvent, strong oxidizer, Yin Yuan, wherein the mass ratio of surfactant and solvent is 0.01～0.25: 1, the mass ratio of strong oxidizer and surfactant is 0.05～0.2: 1, and the mass ratio of silver-colored source and surfactant is 0.001～0.2: 1; Then by the surfactant dissolves taking in solvent, then add strong oxidizer, stir after 0.5～36 hour, then add in ，Yu darkroom, silver-colored source and stir 1～24 hour, obtain silver-colored solution;
Two, take titanium source and solvent, wherein the mass ratio of titanium source and solvent is 0.025～0.2: 1, then titanium source is added in solvent, stirs 0.5～36 hour, obtains titanium precursor body;
Three, measure titanium precursor body prepared by silver-colored solution prepared by step 1 and step 2 and join in container, stir 0.5～24 hour, then room temperature ageing, dries, obtain titanium dioxide/silver gel, wherein the mass ratio in the silver-colored source in silver-colored solution and the titanium source in titanium precursor body is 0.001～0.5;
Four, titanium dioxide/silver gel step 3 being obtained is put into roasting in Muffle furnace, and sintering temperature is 300～900 ℃, obtains ordered mesoporous titanium dioxide/silver-colored photochemical catalyst.
The ordered mesoporous titanium dioxide that present embodiment is prepared with sol-gal process/silver-colored photochemical catalyst is Anatase, is conducive to the raising of the separative efficiency in light induced electron and hole, is suitable for photocatalyst, and its specific area is 120～160m
2/ g.Deposition of silver is in TiO
2surface can cause the redistribution of carrier, can suppress the compound of light induced electron and hole, thereby the photocatalysis of raising catalyst is lived and had good dispersiveness, effectively catalyze and degrade organic pollutants.And the mesoporous aperture of ordered mesoporous titanium dioxide of the present invention/silver-colored photochemical catalyst homogeneous, duct is flourishing, and order is high, is beneficial to the diffusion of reactant and product.Preparation technology of the present invention is simple, cost is low, environmental pollution is little, equipment needed thereby is simple, and is easy to realize commercialization.Can be applicable to photocatalysis field.
The specific embodiment two: present embodiment is different from the specific embodiment one is that surfactant described in step 1 is triblock copolymer (P123, F127), polyvinylpyrrolidone (PVP), lauryl sodium sulfate (SDS), softex kw (CTAB), acrylonitrile-butadiene-styrene copolymer (ABS), PEI (PEI), Brij-35 (Brij-35), a kind of in polyethylene glycol (PEG-400) and triethanolamine (TEA) or both mix in any proportion.Other is identical with the specific embodiment one.
Execute mode three: present embodiment is different from the specific embodiment one or two is that solvent described in step 1 is that a kind of in deionized water, ethanol, isopropyl alcohol and n-butanol or two kinds mix in any proportion.Other is identical with the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three is that time of stirring after strong oxidizer that adds described in step 1 is 1-36 hour.Other is identical with one of specific embodiment one to three.
The specific embodiment five: present embodiment is different from one of specific embodiment one to four is that strong oxidizer described in step 1 is KNO
3, KMnO
4, K
2cr
2o
7, KClO
3, MnO
2, HClO, H
2o
2, dense H
2sO
4, dense HNO
3with a kind of or two kinds of mixing in any proportion in chloroazotic acid.Other is identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five is that silver-colored source described in rapid one is silver nitrate or silver ammino solution.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: present embodiment is different from one of specific embodiment one to six is that titanium source described in rapid two is titanyl sulfate, titanium tetrachloride, titanium sulfate, butyl titanate, isopropyl titanate or tetraethyl titanate.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: present embodiment is different from one of specific embodiment one to seven is that solvent is that one or both of deionized water, methyl alcohol, ethanol, isopropyl alcohol and the tert-butyl alcohol mix in any proportion described in step 2.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: present embodiment is different from one of specific embodiment one to eight is that mixing time described in step 2 is 0.5-20 hour.Other is identical with one of specific embodiment one to eight.
The specific embodiment ten: present embodiment is different from one of specific embodiment one to nine is that digestion time described in step 3 is 12-48 hour, 20～25 ℃ of Aging Temperatures, humidity is 40-60%.Other is identical with one of specific embodiment one to nine.
The specific embodiment 11: present embodiment is different from one of specific embodiment one to ten is that bake out temperature described in step 3 is 30-80 ℃, and drying time is 1-10 days.Other is identical with one of specific embodiment one to ten.
The specific embodiment 12: present embodiment is different from one of specific embodiment one to 11 be present embodiment different with the specific embodiment one be that heat-treating atmosphere described in step 4 is the mist of one or more gases in air, oxygen, nitrogen, argon gas and helium, gas flow is 30～2000mL/min.Other is identical with one of specific embodiment one to 11.
The specific embodiment 13: present embodiment is different from one of specific embodiment one to 12 be present embodiment different with the specific embodiment one be that heating rate described in step 4 is 1-15 ℃/min, be warming up to 350-900 ℃, temperature retention time is 1～5h.Other is identical with one of specific embodiment one to 12.
By following verification experimental verification beneficial effect of the present invention:
Embodiment 1: the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst of the present embodiment carries out according to the following steps:
One, take 1g surfactant P123 and be dissolved in 20mL deionized water, stir 2 hours, add wherein 0.5mL strong oxidizer HNO
3, stir 24 hours, make surfactant terminating functional groups be oxidized to carboxyl, then add 0.2g silver nitrate, making the molar fraction of Ag in complex is 5%, and in darkroom, stirs 24 hours, obtains silver-colored solution;
Two, take titanyl sulfate 2g and be dissolved in 20mL deionized water, stir 24 hours, obtain titanium precursor body;
Three, step 1 gained silver solution is joined in step 2 gained titanium precursor body, stir 12 hours, by colloidal sol, in 25 ℃ of ageings 24 hours, ageing humidity was 40-60%, and in 50 ℃ of oven dry 10 days, obtained titanium dioxide/silver gel;
Four, step 3 gained gel is calcined in air atmosphere, gas flow is 1000mL/min, and programming rate is 1 ℃/min, is warming up to 500 ℃, insulation 2h, cooling after, obtain a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst.
The XRD spectra of the ordered mesoporous titanium dioxide that this test makes/silver-colored photochemical catalyst as shown in Figure 1, as can be seen from Figure 1, ordered mesoporous titanium dioxide/silver-colored photochemical catalyst be anatase crystal, and have higher crystallinity.
The N of the ordered mesoporous titanium dioxide that this test makes/silver-colored photochemical catalyst
2adsorption-desorption isollaothermic chart as shown in Figure 2; As can be seen from Figure 2, N
2adsorption-desorption thermoisopleth is IV shape adsorption curve and has H1 type hysteresis loop, and titanium dioxide/silver that synthesized is described is order mesoporous structure, and the specific area that adopts BET formula to calculate according to adsorption curve in nitrogen adsorption-desorption isotherm is 139m
2/ g.
The pore size distribution curve figure of the ordered mesoporous titanium dioxide that this test makes/silver-colored photochemical catalyst as shown in Figure 3; As can be seen from Figure 3, ordered mesoporous titanium dioxide/silver-colored photochemical catalyst has the pore-size distribution of homogeneous, and most probable aperture is about 4.5nm.
The TEM photo of the ordered mesoporous titanium dioxide that this test makes/silver-colored photochemical catalyst as shown in Figure 4; As can be seen from Figure 4, photochemical catalyst has the meso-hole structure of high-sequential.
The ordered mesoporous titanium dioxide that this test is made/silver-colored photochemical catalyst, carry out the application test of photocatalytic degradation, adopt 0.1g catalyst, 10W ultraviolet light, irradiate 3h, difficult degradation poisonous and harmful organic pollution, dyestuff, virus etc. in 20mL water body are processed.
The ordered mesoporous titanium dioxide making by known example 1 of above demonstration test/silver-colored photocatalyst treatment efficiency reaches 99.9%, and the catalyst after recovery can Reusability.
Claims (10)
1. a preparation method for ordered mesoporous titanium dioxide/silver-colored photochemical catalyst, is characterized in that carrying out the preparation method of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to the following steps:
One, take surfactant, solvent, strong oxidizer, Yin Yuan, wherein the mass ratio of surfactant and solvent is 0.01～0.25:1, the mass ratio of strong oxidizer and surfactant is 0.05～0.2:1, the mass ratio of silver source and surfactant is 0.001～0.2:1, then by the surfactant dissolves taking in solvent, then add strong oxidizer, stir after 0.5～36 hour, add again in ，Yu darkroom, silver-colored source and stir 1～24 hour, obtain silver-colored solution;
Two, take titanium source and solvent, wherein the mass ratio of titanium source and solvent is 0.025～0.2:1, then titanium source is added in solvent, stirs 0.5～36 hour, obtains titanium precursor body;
Three, measure titanium precursor body prepared by silver-colored solution prepared by step 1 and step 2 and join in container, stir 0.5～24 hour, then room temperature ageing, dries, obtain titanium dioxide/silver gel, wherein the mass ratio in the silver-colored source in silver-colored solution and the titanium source in titanium precursor body is 0.001～0.5;
Four, titanium dioxide/silver gel step 3 being obtained is put into roasting in Muffle furnace, obtains ordered mesoporous titanium dioxide/silver-colored photochemical catalyst.
2. the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to claim 1, is characterized in that surfactant described in step 1 is that a kind of in triblock copolymer, polyvinylpyrrolidone, lauryl sodium sulfate, softex kw, acrylonitrile-butadiene-styrene copolymer, PEI, Brij-35, polyethylene glycol and triethanolamine or both mix in any proportion.
3. the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to claim 1 and 2, is characterized in that solvent described in step 1 is that a kind of in deionized water, ethanol, isopropyl alcohol and n-butanol or two kinds mix in any proportion.
4. the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to claim 1, is characterized in that the strong oxidizer described in step 1 is KNO
3, KMnO
4, K
2cr
2o
7, KClO
3, MnO
2, HClO, H
2o
2, dense H
2sO
4, dense HNO
3with a kind of or two kinds of mixing in any proportion in chloroazotic acid.
5. the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to claim 1, is characterized in that the silver-colored source described in step 1 is silver nitrate or silver ammino solution.
6. the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to claim 1, is characterized in that the titanium source described in step 2 is titanyl sulfate, titanium tetrachloride, titanium sulfate, butyl titanate, isopropyl titanate or tetraethyl titanate.
7. the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to claim 1, is characterized in that described in step 2 that solvent is that a kind of of deionized water, methyl alcohol, ethanol, isopropyl alcohol and the tert-butyl alcohol or both mix in any proportion.
8. the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to claim 1, is characterized in that the digestion time described in step 3 is 12-48 hour, 20～25 ℃ of Aging Temperatures, and humidity is 40-60%.
9. the preparation method of a kind of ordered mesoporous titanium dioxide/silver-colored photochemical catalyst according to claim 1, is characterized in that the bake out temperature described in step 3 is 30-80 ℃, and drying time is 1-10 days.
10. the preparation method of a kind of ordered mesoporous titanium dioxide photochemical catalyst according to claim 1, it is characterized in that the calcination atmosphere described in step 4 is the mist of one or more gases in air, oxygen, nitrogen, argon gas and helium, gas flow is 30～2000mL/min, heating rate is 1～15 ℃/min, 300～900 ℃ of sintering temperatures, temperature retention time is 1～5h.
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| CN103212409B (en) * | 2013-01-26 | 2015-02-04 | 吉首大学 | Porous-carbon-material-loaded mesoporous TiO2-Ag complex, and preparation method thereof |
| CN103192075B (en) * | 2013-04-16 | 2015-04-22 | 杨晓红 | Preparation method of core-shell composite material wrapped in titanium dioxide nanoparticle coating |
| CN103316673B (en) * | 2013-06-27 | 2015-07-08 | 中国空间技术研究院 | Silver-carbon-codoped bicrystal mesoporous titanium dioxide visible light photocatalyst and preparation method thereof |
| FR3016813B1 (en) | 2014-01-27 | 2017-11-24 | Total Sa | VISIBLE-ABSORBING TI02-BASED MATERIAL AND METHOD OF MANUFACTURING THE SAME |
| CN105582916B (en) * | 2016-01-14 | 2018-01-05 | 内江洛伯尔材料科技有限公司 | A kind of titanium dioxide is sequentially depositing the preparation method of the photochemical catalyst of nanogold and rhodium |
| CN110366444B (en) * | 2018-02-09 | 2022-04-26 | 纳琦环保科技有限公司 | Synthetic method of composite photocatalytic material with photo-thermal synergistic effect |
| CN108246364B (en) * | 2018-03-05 | 2020-05-26 | 常州大学 | Preparation method of silver oxide doped crystalline polyimide composite visible light photocatalyst |
| CN108821333B (en) * | 2018-05-29 | 2021-02-26 | 上海师范大学 | Preparation method of noble metal in-situ modified mesoporous titanium oxide material |
| CN109529823A (en) * | 2018-12-07 | 2019-03-29 | 武汉工程大学 | A kind of silver carried titanium dioxide hollow sphere and preparation method thereof |
| CN110721679A (en) * | 2019-11-01 | 2020-01-24 | 天津科技大学 | Preparation method of photocatalyst |
| CN113397829A (en) * | 2021-06-17 | 2021-09-17 | 莱西市蔚来设计中心 | Antibacterial deodorizing paper diaper |
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