CN105435828A - Fe and N co-doped mesoporous TiO2 microsphere array visible light photocatalyst and preparation method - Google Patents
Fe and N co-doped mesoporous TiO2 microsphere array visible light photocatalyst and preparation method Download PDFInfo
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- CN105435828A CN105435828A CN201511030931.7A CN201511030931A CN105435828A CN 105435828 A CN105435828 A CN 105435828A CN 201511030931 A CN201511030931 A CN 201511030931A CN 105435828 A CN105435828 A CN 105435828A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a Fe and N co-doped mesoporous TiO2 microsphere array visible light photocatalyst and a preparation method and belongs to the technical field of TiO2 photocatalysis. The photocatalyst is a three-dimensional ordered Fe and N co-doped mesoporous TiO2 microsphere array prepared with a two-step template method, and microspheres are arranged orderly in a three-dimensional manner, have uniform size and obvious mespores and are all anatase. TiO2 is modified through Fe and N co-doping, and the Fe and N co-doped TiO2 microsphere array is obtained; due to a slow photon effect and a multiple scattering effect of the microsphere array and the excellent mass transfer performance and high specific surface area of a hierarchical porous (macroporous or mesoporous) material, light absorption of TiO2 can be improved. The smallest band gap of Fe and N co-doped TiO2 is realized at the optimal doping content, and absorbed light is extended to visible light. The solar energy utilization rate can be increased by the aid of Fe and N co-doped TiO2. The method is easy to operate and control, and the visible light photocatalytic performance is good.
Description
Technical field
The present invention relates to field of titanium dioxide photocatalysis, particularly the preparation of Fe, N codope titanium dioxide micro-sphere array visible-light photocatalyst and application thereof.
Background technology
Along with the propelling of global industry process, environmental pollution, energy crisis, greenhouse effects have become the significant problem of 21 century facing mankind, how to realize the focus that environmental protection and sustainable development become research both at home and abroad.Large quantity research shows, various poisonous and hazardous pollutant in water and air, the various alkane discharged in Chemical Manufacture, fragrant hydrocarbons and their derivates, halides, polycyclic aromatic hydrocarbon and heterocyclic compound etc. greatly can by photocatalytic degradations.TiO
2owing to having stable chemical nature, fast light burn into resistance to chemical attack, harmless, cheap, energy gap is moderate, have the features such as very strong oxidisability, thus become the photochemical catalyst having application potential in conductor photocatalysis research field most.But due to TiO
2the energy gap of Anatase is wider is 3.2eV, the ultraviolet light (namely wavelength is less than or equal to 387.5nm) that energy is equal to or greater than its energy gap can only be absorbed, absorbing wavelength threshold value mostly in ultra-violet (UV) band, and these ultraviolet lights only account for solar energy less than 5%.Therefore pure TiO
2be difficult to utilize visible ray or solar energy, be difficult to be committed to commercial Application; (2) photo-quantum efficiency is low, and light induced electron and hole, very easily in body phase and surface recombination, are difficult to realize effective separation and utilization.
In order to solve this two key problems, improve light-catalysed efficiency, a large amount of work has been attempted in scientific research circle, by TiO
2micro-structural, pattern and the control of size and the method for modification improve TiO
2photocatalytic activity.The method mainly ion doping of modification, utilize physics or chemical method, ion is incorporated into titanium dioxide lattice structure inner, thus in its lattice, introduce new electric charge, formation defect or change lattice types, affect the moving situation in light induced electron and hole, adjust the band structure of its distribution or change titanium dioxide, finally cause the photocatalytic activity of titanium dioxide to change.Generally there is nonmetal (N, S, C, F) to adulterate at present, also have the doping of rare earth metal, transition metal, as: Fe
3+, Co
2+deng.Codope is also the focus of research, and the effect of Fe, N codope is best.In addition, TiO is changed
2the pattern of nano particle, just it can be prepared into nanometer rods, nano wire, nanotube, hollow ball and fiber etc.
Template and sol-gal process, in conjunction with the work of forefathers, combine by the present invention, have prepared a kind of high performance Fe, N codope titanium dioxide micro-sphere array visible-light photocatalyst.The method can be synthesized at normal temperatures, the microstructure of controllable gel, and technique is simple, easy to operate.The catalyst that the method is prepared is specially adapted to catalytic degradation organic dyestuff (as: rhodamine B) under radiation of visible light, reaches very high degradation rate.
Summary of the invention
The object of the invention is a kind of method preparing high performance Fe, N codope titanium dioxide micro-sphere array photochemical catalyst, make the titanium dioxide microballoon sphere array photo catalysis agent of Fe, N codope have excellent visible light catalytic performance.
A kind of Fe, N codope titanium dioxide mesoporous microsphere array visible-light photocatalyst, it is characterized in that, Fe, N codope titanium dioxide mesoporous microsphere be Fe, N codope titanium dioxide form there is mesoporous micro-sphere structure, Fe, N codope titanium dioxide mesoporous microsphere array is the array structure of the three-dimensional order that described Fe, N codope titanium dioxide mesoporous microsphere is formed.
High performance Fe of the present invention, N codope titanium dioxide micro-sphere array visible-light photocatalyst are prepared in the steps below:
(1) Stobe method is utilized to synthesize 200 ~ 500nm monodisperse silica sphere particle;
By the ammoniacal liquor of deionized water, 13mol/L and absolute ethyl alcohol mixing, the ammoniacal liquor of deionized water: 13mol/L: the volume ratio of absolute ethyl alcohol is (2 ~ 7): (7 ~ 10): 40, add the mixture of ethyl orthosilicate and the ethanol mixed again, ethyl orthosilicate in the mixture of ethyl orthosilicate and ethanol: the ratio of ethanol is (2 ~ 5) g:40ml, 15 ~ 24h is stirred in 15 ~ 30 DEG C, after reaction terminates, repeatedly clean with absolute ethyl alcohol, obtain the monodisperse silica microspheres of 200 ~ 500nm; Preferably every 2-7ml deionized water correspondence 2 ~ 5g ethyl orthosilicate;
(2) silicon dioxide microsphere slow speed centrifugation self assembly step (1) obtained, ramped heating schedule removes water and absolute ethyl alcohol, calcine at 750 DEG C, be immersed in the mixed solution of initator and polymer monomer again, the mass ratio of initator and polymer monomer is (0.5 ~ 1.5): 100, is polymerized, then removes unnecessary polymer, soak with 2 ~ 10wt%HF solution and remove silica template, obtain polymer template;
(3) preparation of Fe, N codope mesoporous TiO 2 precursor liquid: dropwise joined in hydrochloric acid solution by isopropyl titanate (TTIP), stirs 0.5 ~ 1h, is designated as solution A; In ethanolic solution, add mesoporous dose of P123, be stirred to dissolving, be designated as B solution; Wherein isopropyl titanate: hydrochloric acid solution: ethanol: P123 is (2 ~ 3) g:(2 ~ 2.5) g:(4 ~ 16) ml:(0.8 ~ 2) g; Then B solution is divided into two parts, portion adds source of iron FeCl
36H
2o, Fe/Ti molar percentage is 0.025%-0.1%, is stirred to evenly, is designated as C solution; Another part adds nitrogenous source TMAH, and N/Ti mol ratio is 0.1-0.3 (preferably 0.2), is stirred to evenly, is designated as solution D; First C solution is added solution A under agitation, then solution D is added above-mentioned solution under agitation, continue to stir 1-5h;
(4) polymer template obtained in step (2) is immersed in 3-6h in Fe, N codope mesoporous TiO 2 precursor liquid of step (3), then ageing 2-4 days is taken out, 3-6h is calcined in the Muffle furnace of 350-450 DEG C, remove polymer template and P123 template, obtain the high performance Fe of anatase, N codope titanium dioxide micro-sphere array visible-light photocatalyst.
Above-mentioned initator is selected from benzoyl peroxide or azodiisobutyronitrile.
Above-mentioned polymer monomer is selected from styrene or methyl methacrylate.
The photocatalyst applications of Fe, N codope titanium dioxide micro-sphere array prepared by the present invention is tested in photocatalytic degradation, take visible ray as light source, and rhodamine B is that target degradation product carries out photocatalytic degradation process, achieves good degradation effect.
Adopt Fe, N codope titanium dioxide micro-sphere array photochemical catalyst that the present invention prepares, microsphere diameter is about 100-300nm, for anatase structured, and Fe
3+, N is all doped to TiO
2in lattice, reduce TiO
2energy gap, make absorption light expand to visible ray from ultraviolet light, improve the utilization rate to solar energy.In addition, Fe
3+enter TiO
2in lattice, Fe
3+become the center of catching light induced electron, thus reduce the right recombination rate of photo-generate electron-hole, improve photo-quantum efficiency.This preparation method well can control the size of obtained titanium dioxide ball by the silica template being easy to prepare, preparation parameter is easy to control, reproducible.Fe, N codope titanium dioxide opal photocatalyst applications of preparation being tested in photocatalytic degradation, take visible ray as light source, and rhodamine B is that target degradation product carries out photocatalytic degradation process, compared to business photochemical catalyst, achieves good degradation effect.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of Fe, N codope titanium dioxide micro-sphere array prepared by embodiment 1;
Fig. 2 is the transmission electron microscope picture of Fe, N codope titanium dioxide micro-sphere array prepared by embodiment 3;
Fig. 3 is the XRD figure of Fe, N codope titanium dioxide micro-sphere array prepared by embodiment 4;
Fig. 4 is the photocatalytic degradation curve of Fe, N codope titanium dioxide micro-sphere array prepared by embodiment 4.
Detailed description of the invention
Below in conjunction with example, method of the present invention is further described.These examples have further described and demonstrated the embodiment in the scope of the invention.The example provided only for illustration of object, any restriction is not formed to the present invention, various change can be carried out to it under the condition not deviating from spirit and scope of the invention.
Embodiment 1
(1) volume is respectively the mixing of the deionized water of 18ml, 60ml, 320ml, the ammoniacal liquor of 13mol/L and absolute ethyl alcohol, 30 DEG C are stirred 1h, add the ethyl orthosilicate of the 29.16g mixed and the absolute ethyl alcohol mixture of 400ml again, 20h is stirred in 30 DEG C, after reaction terminates, repeatedly clean by ethanol and deionized water, slow speed centrifugation 10h self assembly, calcine at 750 DEG C, be immersed in benzoyl peroxide again and methyl methacrylate mass ratio is in the solution of 1:84, be polymerized at 60 DEG C.Remove unnecessary polymer with oxolane, be the HF solution removal silica template of 5% with mass fraction, obtain PMMA (polymethyl methacrylate) antitemplate.
(2) 2.84g isopropyl titanate is dropwise joined in 2.4g hydrochloric acid solution, stir 1h, be designated as solution A; In 4g absolute ethyl alcohol, add 1.16g mesoporous dose of P123, be stirred to dissolving, be designated as B solution; Then B solution is divided into two parts, portion adds 0.2g0.65%FeCl
3.6H
2the ethanolic solution (Fe/Ti mol ratio is 0.05%, namely takes 0.2g) of O, is stirred to evenly, is designated as C solution; Another part adds 0.75g nitrogenous source TMAH (N/Ti mol ratio is 0.2, namely takes 0.75g), is stirred to evenly, is designated as solution D; First C solution is added solution A under agitation, then solution D is added above-mentioned solution under agitation, continue to stir 1h;
The polymer template obtained in step (1) is immersed in 4h in the titanium colloidal sol of step (2), then ageing 2-4 days is taken out, 4h is calcined in the Muffle furnace of 400 DEG C, remove polymer template PMMA and P123 template, obtain the three-dimensional ordered mesoporous TiO of Fe, N codope of anatase
2microballoon.
Products obtained therefrom shows through ESEM (SEM) analysis, the sphere diameter of silica prepared by this method is 290nm, the PMMA counter opal template prepared relatively perfectly oppositely replicates the structure of SiO2 colloidal crystal, thus obtain orderly big-hole back opal template, owing to being interconnected by window between PMMA counter opal template internal holes, so whole template can be filled fully when the TiO2 precursor liquid of Fe, N codope injects time, remove after PMMA template through calcining, just obtain the TiO of three-dimensional order Fe, N codope
2micro-sphere array.Although finally obtain the TiO of Fe, N codope
2sample maintains original arrangement, due to TiO in calcination process
2the contraction of precursor liquid volume, obviously can observe microsphere diameter and obviously diminish (170nm), relative to original SiO
2microsphere diameter reduces 41%, Fe, N codope rear surface becomes coarse, is schemed, be Anatase from XRD.
The titanium dioxide microballoon sphere array catalyst taking Fe, N codope of the above-mentioned preparation of 0.02g carries out the experiment of visible light photocatalytic degradation rhodamine B, and rhodamine B concentration is 5mgL
-1, after radiation of visible light 100min, the degradation rate of rhodamine B is 94.2%.
Embodiment 2
The preparation method of the titanium dioxide microballoon sphere array catalyst of Fe, N codope, step is with embodiment 1, and difference is: 0.65%FeCl used
3.6H
2the ethanolic solution quality of O is 0.1g
The titanium dioxide opal catalyst taking Fe, N codope of the above-mentioned preparation of 0.02g carries out the experiment of visible light photocatalytic degradation rhodamine B, and rhodamine B concentration is 5mgL
-1, rhodamine after radiation of visible light 100min
Embodiment 3
The preparation method of the titanium dioxide opal catalyst of Fe, N codope, step is with embodiment 1, and difference is: 0.65%FeCl used
3.6H
2the ethanolic solution quality of O is 0.3g
The titanium dioxide opal catalyst taking Fe, N codope of the above-mentioned preparation of 0.02g carries out the experiment of visible light photocatalytic degradation rhodamine B, and rhodamine B concentration is 5mgL
-1, after radiation of visible light 100min, the degradation rate of rhodamine B is 91.2%.
Embodiment 4
The preparation method of the titanium dioxide opal catalyst of Fe, N codope, step is with embodiment 1, and difference is: 0.65%FeCl used
3.6H
2the quality of the ethanolic solution of O is 0.4g
The titanium dioxide opal catalyst taking Fe, N codope of the above-mentioned preparation of 0.02g carries out the experiment of visible light photocatalytic degradation rhodamine B, and rhodamine B concentration is 5mgL
-1, after radiation of visible light 100min, the degradation rate of rhodamine B is 77.0%.
Embodiment 5
The preparation method of the titanium dioxide opal catalyst of Fe, N codope, step is with embodiment 1, and difference is: the quality of nitrogenous source TMAH used is 0.375g
The titanium dioxide opal catalyst taking Fe, N codope of the above-mentioned preparation of 0.02g carries out the experiment of visible light photocatalytic degradation rhodamine B, and rhodamine B concentration is 5mgL
-1, after radiation of visible light 100min, the degradation rate of rhodamine B is 64.3%.
Embodiment 6
The preparation method of the titanium dioxide opal catalyst of Fe, N codope, step is with embodiment 1, and difference is: the quality of nitrogenous source TMAH used is 1.125g
The titanium dioxide opal catalyst taking Fe, N codope of the above-mentioned preparation of 0.02g carries out the experiment of visible light photocatalytic degradation rhodamine B, and rhodamine B concentration is 5mgL
-1, after radiation of visible light 100min, the degradation rate of rhodamine B is 72.6%.
Claims (5)
1. Fe, N codope titanium dioxide mesoporous microsphere array visible-light photocatalyst, it is characterized in that, Fe, N codope titanium dioxide mesoporous microsphere is the micro-sphere structure with meso-porous hollow that Fe, N codope titanium dioxide is formed, and Fe, N codope titanium dioxide mesoporous microsphere array is the array structure of the three-dimensional order that described Fe, N codope titanium dioxide mesoporous microsphere is formed.
2. a preparation method for Fe, N codope titanium dioxide mesoporous microsphere array visible-light photocatalyst, is characterized in that, comprise the following steps:
(1) Stobe method is utilized to synthesize 200 ~ 500nm monodisperse silica sphere particle;
(2) silicon dioxide microsphere slow speed centrifugation self assembly step (1) obtained, ramped heating schedule removes water and absolute ethyl alcohol, calcine at 750 DEG C, be immersed in the mixed solution of initator and polymer monomer again, the mass ratio of initator and polymer monomer is (0.5 ~ 1.5): 100, is polymerized, then removes unnecessary polymer, soak with 2 ~ 10wt%HF solution and remove silica template, obtain polymer template;
(3) preparation of Fe, N codope mesoporous TiO 2 precursor liquid: dropwise joined in hydrochloric acid solution by isopropyl titanate (TTIP), stirs 0.5 ~ 1h, is designated as solution A; In ethanolic solution, add mesoporous dose of P123, be stirred to dissolving, be designated as B solution; Wherein isopropyl titanate: hydrochloric acid solution: ethanol: P123 is (2 ~ 3) g:(2 ~ 2.5) g:(4 ~ 16) ml:(0.8 ~ 2) g; Then B solution is divided into two parts, portion adds source of iron FeCl
3.6H
2o, Fe/Ti molar percentage is 0.025%-0.1%, is stirred to evenly, is designated as C solution; Another part adds nitrogenous source TMAH, and N/Ti mol ratio is 0.1-0.3 (preferably 0.2), is stirred to evenly, is designated as solution D; First C solution is added solution A under agitation, then solution D is added above-mentioned solution under agitation, continue to stir 1-5h;
(4) polymer template obtained in step (2) is immersed in 3-6h in Fe, N codope mesoporous TiO 2 precursor liquid of step (3), then ageing 2-4 days is taken out, 3-6h is calcined in the Muffle furnace of 350-450 DEG C, remove polymer template and P123 template, obtain the high performance Fe of anatase, N codope titanium dioxide micro-sphere array visible-light photocatalyst.
3. according to the method for claim 1, it is characterized in that, step (1) utilizes Stobe method to synthesize the method for 200 ~ 500nm monodisperse silica sphere particle: by deionized water, the ammoniacal liquor of 13mol/L and absolute ethyl alcohol mixing, the ammoniacal liquor of deionized water: 13mol/L: the volume ratio of absolute ethyl alcohol is (2 ~ 7): (7 ~ 10): 40, add the mixture of ethyl orthosilicate and the ethanol mixed again, ethyl orthosilicate in the mixture of ethyl orthosilicate and ethanol: the ratio of ethanol is (2 ~ 5) g:40ml, 15 ~ 24h is stirred in 15 ~ 30 DEG C, after reaction terminates, repeatedly clean with absolute ethyl alcohol, obtain the monodisperse silica microspheres of 200 ~ 500nm, preferably every 2-7ml deionized water correspondence 2 ~ 5g ethyl orthosilicate.
4. according to the method for claim 1, it is characterized in that, initator is selected from benzoyl peroxide or azodiisobutyronitrile.
5. according to the method for claim 1, it is characterized in that, polymer monomer is selected from styrene or methyl methacrylate.
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| CN108435176A (en) * | 2018-04-04 | 2018-08-24 | 安徽工程大学 | A kind of Fe2O3 doping TiO2Octahedron nanometer particle and preparation method thereof |
| CN108686689A (en) * | 2017-04-12 | 2018-10-23 | 中国科学院宁波材料技术与工程研究所 | Mesopore surfaces defect Mo-N-TiO2The preparation method of microballoon catalysis material |
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