CN105080531A - Method for preparing neodymium-doped mesopore titanium dioxide microballoon photocatalyst - Google Patents
Method for preparing neodymium-doped mesopore titanium dioxide microballoon photocatalyst Download PDFInfo
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Abstract
The invention relates to a method for preparing a neodymium-doped mesopore titanium dioxide microballoon photocatalyst. The method includes the following steps that (1) absolute ethyl alcohol and a KCl solution are added into cetylamine to be evenly stirred and mixed, then tetraisopropyl titanate is added to be evenly stirred, and after standing, filtering, washing and drying are conducted, a precursor sample is obtained; (2) the precursor sample is placed in a reaction vessel, absolute ethyl alcohol and water are added, then neodymium nitrate is added to be evenly stirred, a hydrothermal reaction is carried out under the airtight condition, cooling, filtering and drying are conducted, and thus a neodymium-doped titanium dioxide sample is obtained; (3) the neodymium-doped titanium dioxide sample is roasted and then cooled, namely the neodymium-doped mesopore titanium dioxide microballoon photocatalyst is obtained. Compared with the prior art, the method has the advantages of being simple in technology, excellent in photocatalytic performance, good in degradation effect on methyl orange and the like.
Description
Technical field
The present invention relates to a kind of preparation method of titanic oxide microsphere photocatalyst, especially relate to a kind of preparation method of neodymium-doped mesoporous TiO 2 microsphere photocatalyst.
Background technology
In recent years, TiO
2owing to having, stable chemical nature, safety non-toxic, preparation are simple, low price, directly can utilize the advantages such as solar energy, have broad application prospects (silicate journal in photocatalytic degradation environmental pollution pollutant etc., 2010,38 (01): 68-73; University Of Qingdao's journal (natural science edition), 2014,27 (03): 19-23,52; Catalysis journal, 2014,35 (09): 1578-1589).But TiO
2as photochemical catalyst, also exist significantly not enough, as greater band gap, the sunshine of 3% ~ 5% can only be utilized, mainly at ultraviolet band, limit its practical application (Chinese Journal of Inorganic Chemistry, 2007,23 (04): 738-742; Catalysis journal, 2013,34 (06): 1076-1086).Not enough in order to make up these, improve the utilization rate of sunshine, researcher is to TiO
2the method modifications (catalysis journal, 2013,34 (06): 1076-1086) such as semiconductors coupling, doped metallic elements, doped with non-metals element are carried out.Wherein, doped metallic elements is simple due to method, and effectively can improve photocatalysis effect, therefore, is improve TiO
2the effective ways of photochemical catalyst.In addition, the specific surface of photochemical catalyst is also a key factor of the performance affecting catalyst, high-specific surface area not only can provide the reactant of high concentration for photocatalysis environment by suction-operated, and a large amount of activated centres can be produced, thus accelerate catalytic rate (silicate journal, 2014,42 (9): 1195-1202).Therefore, the TiO of high-ratio surface is synthesized
2photochemical catalyst is TiO
2one of focus of photochemical catalyst.There is due to mesoporous material the features such as large specific area, synthesising mesoporous titanium dioxide becomes the target that many scientific researchers are made great efforts, and when research also finds mesoporous TiO 2 degradable organic pollutant, there is very high reaction rate constant (silicate journal, 2014,42 (9): 1195-1202; University Of Science and Technology Of Tianjin's journal, 2013,28 (6): 24-27).But at present pure titinium dioxide mesoporous material is mainly concentrated on to the research of mesoporous TiO 2, therefore, in order to improve the performance of pure titinium dioxide mesoporous material photochemical catalyst further, particularly important to the research of its doping.
Chinese patent 200910114867.9 discloses a kind of preparation method of boron-doped titanium dioxide visible-light responsive photocatalyst, sol-gel process and solid reaction process is adopted boron element to be replaced part oxygen element in titanium dioxide, boron source and TiO 2 precursor is utilized to react, generate boron doped titanium dioxide optical catalyst, this patent technique is simple, but the degradation effect of its catalyst prepared to methyl orange is undesirable.
Summary of the invention
Object of the present invention is exactly provide a kind of preparation method of neodymium-doped mesoporous TiO 2 microsphere photocatalyst to overcome defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
A preparation method for neodymium-doped mesoporous TiO 2 microsphere photocatalyst, comprises the following steps:
(1) in cetylamine, add absolute ethyl alcohol and KCl solution, after being uniformly mixed, then add metatitanic acid four isopropyl ester, stir, leave standstill, filter, washing, after drying, obtain precursor samples;
(2) precursor samples is inserted in reaction vessel, add absolute ethyl alcohol and water, then add neodymium nitrate, after stirring, obtain mixed solution, in confined conditions hydro-thermal reaction, then cold filtration is dry, obtains neodymium-doped titanium dioxide sample;
(3) cool after the roasting of neodymium-doped titanium dioxide sample, namely obtain neodymium-doped mesoporous TiO 2 microsphere photocatalyst.
The mixing time added in step (1) after metatitanic acid four isopropyl ester is 10 ~ 120min, and time of repose is 6 ~ 36h, and baking temperature is 50 ~ 70 DEG C.
The ratio of the addition of the cetylamine described in step (1), absolute ethyl alcohol, KCl solution and metatitanic acid four isopropyl ester is 1g:50 ~ 500mL:0.5 ~ 5mL:1 ~ 5mL, and the concentration of described KCl solution is 0.1mol/L.
Reaction vessel described in step (2) is hydrothermal reaction kettle, add that the precursor samples in hydrothermal reaction kettle, absolute ethyl alcohol and water account for hydrothermal reaction kettle compactedness altogether 60%.
The ratio of the addition of precursor samples, absolute ethyl alcohol, water and the neodymium nitrate described in step (2) is 1g:5 ~ 50mL:5 ~ 50mL:0.001 ~ 0.2g.
Mixing time in step (2) is 5 ~ 60min, and the temperature of hydro-thermal reaction is 110 ~ 200 DEG C, and the reaction time is 2 ~ 60h, and baking temperature is 50 ~ 70 DEG C.
In step (3), the sintering temperature of neodymium-doped titanium dioxide sample is 300 ~ 600 DEG C, and roasting time is 0.5 ~ 5h.
Metatitanic acid four isopropyl ester of the present invention is hydrolyzed in reactant liquor, under the effect of cetylamine, form the presoma of mesoporous TiO 2 ball, carry out, in hydrothermal treatment process, carrying out neodymium atom doping, after high-temperature roasting, titanium dioxide carries out crystallization, and neodymium atom also can better be mixed in titanium dioxide lattice, and passes through roasting, eliminate the intergranular organic matter of titanium dioxide crystal, thus form the TiO 2 porous ball of particle composition.Define new doped energy-band after being adulterated by neodymium, trapped electrons or hole on the photon excitation making energy less to impurity energy level, thus energy gap is narrowed, effectively improve the utilization rate to sunshine, improve photocatalysis efficiency.In addition, the ball that mesoporous TiO 2 microballoon is made up of particle, has very Large ratio surface, in photocatalysis to degrade organic matter process, titanium dioxide granule fully can contact with organic matter, has a lot of photocatalytic activity site, thus can effective degradable organic pollutant.
Compared with prior art, the present invention has the following advantages:
1) technique is simple: the present invention is by first configuring precursor mixed solution, and reaction, roasting prepare neodymium-doped mesoporous TiO 2 microsphere photocatalyst, and course of reaction is simple;
2) organic pollutant degradation is effective: the neodymium-doped mesoporous TiO 2 microsphere photocatalyst that the present invention obtains, neodymium ion is owing to there being a lot of configuration, multiple complex compound can be formed, and the f track of neodymium ion is conducive to the organic absorption of plane of crystal, new doped energy-band is defined after being adulterated by neodymium, energy gap, effective raising is to the utilization rate of sunshine, significant raising photocatalysis efficiency, in addition, the ball that neodymium-doped mesoporous TiO 2 microballoon is made up of particle, there is very Large ratio surface, in photocatalysis to degrade organic matter process, titanium dioxide granule fully can contact with organic matter, there is a lot of photocatalytic activity site, thus effective degradable organic pollutant.In the experiment of photo-catalytic degradation of methyl-orange, the neodymium-doped mesoporous TiO 2 microsphere photocatalyst also demonstrating the present invention's synthesis possesses excellent photocatalysis performance, is particularly useful for methyl orange of degrading.
Accompanying drawing explanation
Fig. 1 is SEM (SEM) figure of the neodymium-doped mesoporous TiO 2 microsphere photocatalyst in the embodiment of the present invention 1;
Fig. 2 is transmission electron microscope (TEM) figure of the neodymium-doped mesoporous TiO 2 microsphere photocatalyst in the embodiment of the present invention 1;
Fig. 3 is the photocatalysis performance figure of the neodymium-doped mesoporous TiO 2 microsphere photocatalyst in the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.The present embodiment is implemented premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
A preparation method for neodymium-doped mesoporous TiO 2 microsphere photocatalyst, comprises the following steps:
(1) get 0.9944g cetylamine and be placed in flask, add the KCl solution that 100mL absolute ethyl alcohol and 0.8mL concentration are 0.1mol/L, at room temperature strong agitation, then adds 2mL metatitanic acid four isopropyl ester, then after stirring 30min, leaves standstill 18h.Filtration washing, at baking oven with 60 DEG C of dry precursor samples obtaining white mesoporous titanium dioxide microspheres;
(2) precursor samples of getting mesoporous titanium dioxide microspheres prepared by 1g step (1) joins in hydrothermal reaction kettle liner, add 20mL absolute ethyl alcohol and 10mL pure water again, keep the compactedness of 60%, then add 0.06g neodymium nitrate, stir 30min, then airtight hydrothermal reaction kettle, in 160 DEG C of reaction 16h, after cooling, filter, at baking oven with 60 DEG C of dryings, obtain the titanium dioxide sample of neodymium-doped;
(3) titanium dioxide sample of getting neodymium-doped prepared by step (2) in 500 DEG C of roasting 2h, after cooling, is taken out, is defined the mesoporous TiO 2 microsphere photocatalyst of neodymium-doped in Muffle furnace.SEM figure and the TEM figure of the neodymium-doped mesoporous TiO 2 microsphere photocatalyst of synthesis is shown in Fig. 1 and Fig. 2 respectively.
(4) the mesoporous TiO 2 microsphere photocatalyst 40mg of neodymium-doped prepared by step (3) is got, joining 50ml concentration is in the methyl orange solution of 0.01g/L, lucifuge stirs 1h, reach adsorption equilibrium, then under 300W xenon lamp, carry out stirring light-catalyzed reaction, photocatalysis performance figure as shown in Figure 3.
Embodiment 2
A preparation method for neodymium-doped mesoporous TiO 2 microsphere photocatalyst, comprises the following steps:
(1) get 0.9944g cetylamine and be placed in flask, add the KCl solution that 100mL absolute ethyl alcohol and 0.8mL concentration are 0.1mol/L, at room temperature strong agitation, then adds 2mL metatitanic acid four isopropyl ester, then after stirring 30min, leaves standstill 18h.Filtration washing, at baking oven with 60 DEG C of dry precursor samples obtaining white mesoporous titanium dioxide microspheres;
(2) precursor samples of getting mesoporous titanium dioxide microspheres prepared by 1g step (1) joins in hydrothermal reaction kettle liner, add 20mL absolute ethyl alcohol and 10mL pure water again, keep the compactedness of 60%, then add 0.04g neodymium nitrate, stir 30min, then airtight hydrothermal reaction kettle, in 160 DEG C of reaction 16h, after cooling, filter, at baking oven with 60 DEG C of dryings, obtain the titanium dioxide sample of neodymium-doped;
(3) titanium dioxide sample of getting neodymium-doped prepared by step (2) in 500 DEG C of roasting 2h, is taken out after cooling, is defined neodymium-doped mesoporous TiO 2 microsphere photocatalyst in Muffle furnace.
Embodiment 3
A preparation method for neodymium-doped mesoporous TiO 2 microsphere photocatalyst, comprises the following steps:
(1) get 1g cetylamine and be placed in flask, add the KCl solution that 50ml absolute ethyl alcohol and 0.5ml concentration are 0.1mol/L, at room temperature strong agitation, add 1ml metatitanic acid four isopropyl ester again, stir 10min again, after leaving standstill 6h, filtration washing, then at the baking oven inner drying of 50 DEG C, precursor samples is obtained;
(2) precursor samples, absolute ethyl alcohol and water that step (1) is obtained are added in hydrothermal reaction kettle liner with the addition of 1g:5ml:5ml ratio, keep the compactedness of hydrothermal reaction kettle 60%, and then neodymium nitrate is added in hydrothermal reaction kettle, the interpolation mass ratio of neodymium nitrate and precursor samples is 0.001:1, after stirring 5min, airtight hydrothermal reaction kettle is hydro-thermal reaction 30h at 110 DEG C, cold filtration again after reacting completely, at the baking oven inner drying of 50 DEG C, obtain neodymium-doped titanium dioxide sample;
(3) neodymium-doped titanium dioxide sample to be inserted in Muffle furnace roasting 5h at 300 DEG C, take out after cooling, namely obtain neodymium-doped mesoporous TiO 2 microsphere photocatalyst.
Embodiment 4
A preparation method for neodymium-doped mesoporous TiO 2 microsphere photocatalyst, comprises the following steps:
(1) get 1g cetylamine and be placed in flask, add the KCl solution that 500ml absolute ethyl alcohol and 5ml concentration are 0.1mol/L, at room temperature strong agitation, add 5ml metatitanic acid four isopropyl ester again, stir 120min again, after leaving standstill 36h, filtration washing, then at the baking oven inner drying of 70 DEG C, precursor samples is obtained;
(2) precursor samples, absolute ethyl alcohol and water that step (1) is obtained are added in hydrothermal reaction kettle liner with the addition of 1g:50ml:50ml ratio, keep the compactedness of hydrothermal reaction kettle 60%, and then neodymium nitrate is added in hydrothermal reaction kettle, the interpolation mass ratio of neodymium nitrate and precursor samples is 0.2:1, after stirring 60min, airtight hydrothermal reaction kettle is hydro-thermal reaction 2h at 200 DEG C, cold filtration again after reacting completely, at the baking oven inner drying of 70 DEG C, obtain neodymium-doped titanium dioxide sample;
(3) neodymium-doped titanium dioxide sample to be inserted in Muffle furnace roasting 0.5h at 600 DEG C, take out after cooling, namely obtain neodymium-doped mesoporous TiO 2 microsphere photocatalyst.
Embodiment 5
A preparation method for neodymium-doped mesoporous TiO 2 microsphere photocatalyst, comprises the following steps:
(1) get 1g cetylamine and be placed in flask, add the KCl solution that 200ml absolute ethyl alcohol and 5ml concentration are 0.1mol/L, at room temperature strong agitation, add 3ml metatitanic acid four isopropyl ester again, stir 60min again, after leaving standstill 20h, filtration washing, then at the baking oven inner drying of 70 DEG C, precursor samples is obtained;
(2) precursor samples, absolute ethyl alcohol and water that step (1) is obtained are added in hydrothermal reaction kettle liner with the addition of 1g:50ml:30ml ratio, keep the compactedness of hydrothermal reaction kettle 60%, and then neodymium nitrate is added in hydrothermal reaction kettle, the interpolation mass ratio of neodymium nitrate and precursor samples is 0.15:1, after stirring 30min, airtight hydrothermal reaction kettle is hydro-thermal reaction 60h at 150 DEG C, cold filtration again after reacting completely, at the baking oven inner drying of 70 DEG C, obtain neodymium-doped titanium dioxide sample;
(3) neodymium-doped titanium dioxide sample to be inserted in Muffle furnace roasting 2h at 500 DEG C, take out after cooling, namely obtain neodymium-doped mesoporous TiO 2 microsphere photocatalyst.
Claims (7)
1. a preparation method for neodymium-doped mesoporous TiO 2 microsphere photocatalyst, is characterized in that, comprises the following steps:
(1) in cetylamine, add absolute ethyl alcohol and KCl solution, after being uniformly mixed, then add metatitanic acid four isopropyl ester, stir, leave standstill, filter, washing, after drying, obtain precursor samples;
(2) precursor samples is inserted in reaction vessel, add absolute ethyl alcohol and water, then add neodymium nitrate, after stirring, hydro-thermal reaction in confined conditions, then cold filtration is dry, obtains neodymium-doped titanium dioxide sample;
(3) cool after the roasting of neodymium-doped titanium dioxide sample, namely obtain neodymium-doped mesoporous TiO 2 microsphere photocatalyst.
2. the preparation method of a kind of neodymium-doped mesoporous TiO 2 microsphere photocatalyst according to claim 1, it is characterized in that, the mixing time added in step (1) after metatitanic acid four isopropyl ester is 10 ~ 120min, and time of repose is 6 ~ 36h, and baking temperature is 50 ~ 70 DEG C.
3. the preparation method of a kind of neodymium-doped mesoporous TiO 2 microsphere photocatalyst according to claim 1, it is characterized in that, the ratio of the addition of the cetylamine described in step (1), absolute ethyl alcohol, KCl solution and metatitanic acid four isopropyl ester is 1g:50 ~ 500mL:0.5 ~ 5mL:1 ~ 5mL, and the concentration of described KCl solution is 0.1mol/L.
4. the preparation method of a kind of neodymium-doped mesoporous TiO 2 microsphere photocatalyst according to claim 1, it is characterized in that, reaction vessel described in step (2) is hydrothermal reaction kettle, add that the precursor samples in hydrothermal reaction kettle, absolute ethyl alcohol and water account for hydrothermal reaction kettle compactedness altogether 60%.
5. the preparation method of a kind of neodymium-doped mesoporous TiO 2 microsphere photocatalyst according to claim 4, it is characterized in that, the ratio of the addition of precursor samples, absolute ethyl alcohol, water and the neodymium nitrate described in step (2) is 1g:5 ~ 50mL:5 ~ 50mL:0.001 ~ 0.2g.
6. the preparation method of a kind of neodymium-doped mesoporous TiO 2 microsphere photocatalyst according to claim 1, it is characterized in that, the mixing time in step (2) is 5 ~ 60min, and the temperature of hydro-thermal reaction is 110 ~ 200 DEG C, reaction time is 2 ~ 60h, and baking temperature is 50 ~ 70 DEG C.
7. the preparation method of a kind of neodymium-doped mesoporous TiO 2 microsphere photocatalyst according to claim 1, is characterized in that, in step (3), the sintering temperature of neodymium-doped titanium dioxide sample is 300 ~ 600 DEG C, and roasting time is 0.5 ~ 5h.
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CN117101641B (en) * | 2023-09-25 | 2024-04-30 | 中国人民解放军火箭军工程大学 | Neodymium-doped mesoporous titanium dioxide nano photocatalyst and preparation method and application thereof |
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