CN103464130A - Method of preparing titanium dioxide meso-pore material with adjustable pore diameter - Google Patents
Method of preparing titanium dioxide meso-pore material with adjustable pore diameter Download PDFInfo
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- CN103464130A CN103464130A CN2013104021661A CN201310402166A CN103464130A CN 103464130 A CN103464130 A CN 103464130A CN 2013104021661 A CN2013104021661 A CN 2013104021661A CN 201310402166 A CN201310402166 A CN 201310402166A CN 103464130 A CN103464130 A CN 103464130A
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- titanium dioxide
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- acetic acid
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000011148 porous material Substances 0.000 title abstract description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 239000010936 titanium Substances 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- -1 titanium alkoxide Chemical class 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 36
- 239000013335 mesoporous material Substances 0.000 claims description 36
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 12
- 238000007605 air drying Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical group [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 4
- PLMFYJJFUUUCRZ-UHFFFAOYSA-M decyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCC[N+](C)(C)C PLMFYJJFUUUCRZ-UHFFFAOYSA-M 0.000 claims description 3
- FDCJDKXCCYFOCV-UHFFFAOYSA-N 1-hexadecoxyhexadecane Chemical compound CCCCCCCCCCCCCCCCOCCCCCCCCCCCCCCCC FDCJDKXCCYFOCV-UHFFFAOYSA-N 0.000 claims description 2
- 235000017858 Laurus nobilis Nutrition 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 235000005212 Terminalia tomentosa Nutrition 0.000 claims description 2
- 244000125380 Terminalia tomentosa Species 0.000 claims description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000002336 sorption--desorption measurement Methods 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005297 material degradation process Methods 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 3
- IEQAICDLOKRSRL-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-(2-dodecoxyethoxy)ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO IEQAICDLOKRSRL-UHFFFAOYSA-N 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- NLMKTBGFQGKQEV-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-(2-hexadecoxyethoxy)ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CCCCCCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO NLMKTBGFQGKQEV-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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Abstract
The invention discloses a method of preparing a titanium dioxide meso-pore material with an adjustable pore diameter. The method comprises the steps of dissolving titanium alkoxide in ethanol, and uniformly mixing to obtain an A liquid; dissolving a surfactant in a mixed liquor of water, acetic acid, acetonitride and diacetone, and uniformly mixing to obtain a B liquid, or mixing the water, the acetic acid, the acetonitride and the diacetone, and uniformly mixing to obtain the B liquid; dropwise adding the A liquid into the B liquid, uniformly mixing, and carrying out ageing on a mixture to obtain a titanium dioxide sol; and pouring the sol into a culture dish, drying the sol in the air, and then carrying out heat treatment on the sol to obtain the titanium dioxide meso-pore material. The method has the advantages that the preparation technology is simple, the cost is low, the obtained titanium dioxide meso-pore material has larger meso-pore diameter and wider pore diameter distribution, and the photocatalytic activity is good.
Description
Technical field
The present invention relates to a kind of method for preparing the adjustable titanium dioxide mesoporous material in aperture.
Background technology
Titanium dioxide is in water pollution control, solar cell, and lithium ion battery, the fields such as fine chemistry industry are widely used.Wherein, optically catalytic TiO 2 organic matter or heavy metal ion are especially noticeable.The nanoscale anatase phase titanium dioxide compares rutile titanium dioxide and brookite type titanium dioxide has higher photocatalytic activity.In addition, the specific area of material, the factors such as degree of crystallinity have material impact to photocatalytic activity.In recent years, the anatase titanium dioxide mesoporous material that has higher degree of crystallinity causes people's interest.
Yet, due to the presoma of titanium, as the titanium alkoxide, titanium tetrachloride etc., be hydrolyzed too violently, makes that controlled to prepare titanium dioxide mesoporous material very difficult.At present, the researcher proposes to adopt the module units of the titania nanoparticles of previously prepared titanium dioxide nanocrystalline or functionalization as titanium dioxide mesoporous material, effect by the structure guiding agent, self assembly under certain condition forms titanium dioxide mesoporous material, finally removes the structure guiding agent and obtains titanium dioxide mesoporous material.The method can effectively solve the titanium precursor body and be hydrolyzed too fast problem.Yet the adjusting of mesoporous titanium dioxide pore size and pore size distribution is not effectively realized.And the relation of mesoporous titanium dioxide pore size and pore size distribution and material light catalysis activity is not also by deep report.
Summary of the invention
The method that the purpose of this invention is to provide the adjustable titanium dioxide mesoporous material in a kind of technique is simple, cost is low preparation aperture.
The method of the titanium dioxide mesoporous material that preparation of the present invention aperture is adjustable comprises the following steps:
1) the titanium alkoxide is dissolved in ethanol, the molar concentration of titanium alkoxide in ethanol is 0.1 ~ 5 M, stirs and obtains A liquid;
By surfactant dissolves in the mixed liquor of water, acetic acid, acetonitrile and acetylacetone,2,4-pentanedione, stir and obtain B liquid, perhaps water, acetic acid, acetonitrile and acetylacetone,2,4-pentanedione are mixed, stir and obtain B liquid, surfactant: water: acetic acid: acetonitrile: the mol ratio of acetylacetone,2,4-pentanedione is 0～1:20～100:5～20:5～30:0.1～1;
2) A liquid is dropwise added to B liquid, after stirring, ageing 2 h, obtain TiO 2 sol, and the molar concentration of titanium dioxide in colloidal sol is 0.01 ~ 1 M;
3) TiO 2 sol is poured into to culture dish at air drying 24 h, then under 450 ℃, carried out the heat treatment of 2 h, obtain titanium dioxide mesoporous material.
In the present invention, described titanium alkoxide can be tetraethyl titanate, isopropyl titanate or butyl titanate.
Described surfactant can be one or more in polyoxyethylene laurel ether (Brij-35), polyethylene glycol cetyl ether (Brij-58), softex kw (CTAB) and DTAB (DTAB).
In preparation process of the present invention, the surfactant range of choice of interpolation is wider, can be cationic surface active agent, can be also nonionic surface active agent, the good stability of the colloidal tio 2 of acquisition, and coagulation not, the colloidal particle particle diameter is little, is evenly distributed; The aperture of the titanium dioxide mesoporous material obtained can be regulated by the amount of the water yield and surfactant.
Preparation technology of the present invention is simple, cost is low, and the titanium dioxide mesoporous material of acquisition has larger mesoporous aperture and wider pore-size distribution, and photocatalytic activity is good.
The accompanying drawing explanation
Fig. 1 is the grading curve of colloidal particle in colloidal tio 2.
Fig. 2 is the X ray diffracting spectrum of titanium dioxide; In figure: the collection of illustrative plates that curve a is embodiment 1, the collection of illustrative plates that curve b is embodiment 2;
Fig. 3 is the transmission electron microscope photo of the titanium dioxide mesoporous material of embodiment 2 preparations.
Fig. 4 is the transmission electron microscope photo of the titanium dioxide mesoporous material of embodiment 3 preparations.
Fig. 5 be embodiment 1 preparation titanium dioxide mesoporous material nitrogen adsorption/desorption isotherms and BJH pore size distribution curve;
Fig. 6 be embodiment 2 preparation titanium dioxide mesoporous material nitrogen adsorption/desorption isotherms and BJH pore size distribution curve.
Fig. 7 is the photocatalytic activity curve of titanium dioxide mesoporous material degradation of methylene blue under UV-irradiation; Wherein curve a is embodiment 1, and curve b is embodiment's 2.
The specific embodiment
Embodiment 1
1) 3.4 ml butyl titanates are dissolved in 5 ml ethanol, stir and obtain A liquid; By 5 ml water, 5 ml acetonitriles, 3 ml acetic acid, 0.2 ml acetylacetone,2,4-pentanedione mixes, and stirs and obtains B liquid.
2) A liquid is dropwise added to B liquid, after stirring, ageing 2 h, obtain the transparence TiO 2 sol.
The TiO 2 sol explanation colloidal tio 2 particle of transparence has less size and dispersed preferably.As shown in Figure 1, as can be seen from the figure the hydrodynamics diameter of colloidal tio 2 particle is 4 nm to the grading curve that adopts dynamic light scattering to record colloidal particle in colloidal tio 2.
3) TiO 2 sol is poured into to culture dish at air drying 24 h, then under 450 ℃, carried out the heat treatment of 2 h, obtain titanium dioxide mesoporous material.
The X ray diffracting spectrum of the titanium dioxide mesoporous material of preparation is as shown in curve a in Fig. 2, and its diffraction maximum is consistent with the standard diagram of anatase phase titanium dioxide, illustrates that products obtained therefrom is anatase phase titanium dioxide.As shown in Figure 5, the aperture of titanium dioxide mesoporous material is about 5.5 nm as we know from the figure for the nitrogen adsorption/desorption isotherms of the titanium dioxide mesoporous material of preparation and BJH pore size distribution curve, and pore-size distribution is narrower.Under UV-irradiation, adopt the photocatalytic activity curve of the titanium dioxide mesoporous material degradation of methylene blue prepared as shown in curve a in Fig. 7.
Embodiment 2
1) 3.4 ml butyl titanates are dissolved in 5 ml ethanol, stir and obtain A liquid, 6 g Brij-35 are dissolved in to 5 ml water, 5 ml acetonitriles, 3 ml acetic acid, in the aqueous solution of 0.2 ml acetylacetone,2,4-pentanedione, stir and obtain B liquid.
2) A liquid is dropwise added to B liquid, after stirring, ageing 2 h, obtain the transparence TiO 2 sol.
3) TiO 2 sol is poured into to culture dish at air drying 24 h, then under 450 ℃, carried out the heat treatment of 2 h, obtain titanium dioxide mesoporous material.
The X ray diffracting spectrum of the titanium dioxide mesoporous material of preparation is as shown in curve b in Fig. 2, and product is anatase phase titanium dioxide as we know from the figure.By the Scherrer formula, calculate, its crystal average diameter is 10 nm.The transmission electron microscope photo of the titanium dioxide mesoporous material of preparation is as Fig. 3.Have as we can see from the figure the mesopore orbit of two kinds of different sizes in mesoporous material, a kind of is the particle packing hole, and another kind is the micella hole.As shown in Figure 6, the aperture of titanium dioxide mesoporous material is about 6.5 nm as we know from the figure for the nitrogen adsorption/desorption isotherms of the titanium dioxide mesoporous material of preparation and BJH pore size distribution curve, and aperture presents obvious bimodal distribution.Under UV-irradiation, adopt the photocatalytic activity curve of the titanium dioxide mesoporous material degradation of methylene blue prepared as shown in curve b in Fig. 7.
Embodiment 3
1) 1.3 ml isopropyl titanates are dissolved in 5 ml ethanol, stir and obtain A liquid, 1 g CTAB is dissolved in to 8 ml water, 6 ml acetonitriles, 2 ml acetic acid, in the aqueous solution of 0.3 ml acetylacetone,2,4-pentanedione, stir and obtain B liquid.
2) A liquid is dropwise added to B liquid, after stirring, ageing 2 h, obtain the transparence TiO 2 sol.
3) TiO 2 sol is poured into to culture dish at air drying 24 h, then under 450 ℃, carried out the heat treatment of 2 h, obtain titanium dioxide mesoporous material.
The transmission electron microscope photo of the titanium dioxide mesoporous material of preparation is as Fig. 4.As we can see from the figure the preparation titanium dioxide mesoporous material in have two kinds mesoporous, a kind of is the particle packing hole, another kind is the micella hole.
Claims (3)
1. a method for preparing the adjustable titanium dioxide mesoporous material in aperture is characterized in that comprising the following steps:
1) the titanium alkoxide is dissolved in ethanol, the molar concentration of titanium alkoxide in ethanol is 0.1 ~ 5 M, stirs and obtains A liquid;
By surfactant dissolves in the mixed liquor of water, acetic acid, acetonitrile and acetylacetone,2,4-pentanedione, stir and obtain B liquid, perhaps water, acetic acid, acetonitrile and acetylacetone,2,4-pentanedione are mixed, stir and obtain B liquid, surfactant: water: acetic acid: acetonitrile: the mol ratio of acetylacetone,2,4-pentanedione is 0～1:20～100:5～20:5～30:0.1～1;
2) A liquid is dropwise added to B liquid, after stirring, ageing 2 h, obtain TiO 2 sol, and the molar concentration of titanium dioxide in colloidal sol is 0.01 ~ 1 M;
3) TiO 2 sol is poured into to culture dish at air drying 24 h, then under 450 ℃, carried out the heat treatment of 2 h, obtain titanium dioxide mesoporous material.
2. the method for the adjustable titanium dioxide mesoporous material in preparation according to claim 1 aperture, is characterized in that described titanium alkoxide is tetraethyl titanate, isopropyl titanate or butyl titanate.
3. the method for adjustable titanium dioxide mesoporous material according to the described preparation of claim 1 aperture, is characterized in that described surfactant is one or more in polyoxyethylene laurel ether, polyethylene glycol cetyl ether, softex kw and DTAB.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103990444A (en) * | 2014-06-04 | 2014-08-20 | 沈阳化工大学 | Preparation method of graphene-homemade TiO2 nanowire photocatalyst |
| CN104030347A (en) * | 2014-07-03 | 2014-09-10 | 重庆大学 | Titanium dioxide sol and coating type denitration catalyst |
| CN105013500A (en) * | 2014-04-23 | 2015-11-04 | 同济大学 | Heterogeneous Fenton catalyst for degrading azo dye wastewater as well as preparation method and application of heterogeneous Fenton catalyst |
| RU2600767C1 (en) * | 2015-07-27 | 2016-10-27 | Государственное образовательное учреждение высшего профессионального образования "Челябинский государственный педагогический университет" | Method of producing titanium dioxide |
| CN108837806A (en) * | 2018-06-28 | 2018-11-20 | 沈阳理工大学 | A kind of preparation method of water treatment ceramsite filter |
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2013
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105013500A (en) * | 2014-04-23 | 2015-11-04 | 同济大学 | Heterogeneous Fenton catalyst for degrading azo dye wastewater as well as preparation method and application of heterogeneous Fenton catalyst |
| CN103990444A (en) * | 2014-06-04 | 2014-08-20 | 沈阳化工大学 | Preparation method of graphene-homemade TiO2 nanowire photocatalyst |
| CN104030347A (en) * | 2014-07-03 | 2014-09-10 | 重庆大学 | Titanium dioxide sol and coating type denitration catalyst |
| RU2600767C1 (en) * | 2015-07-27 | 2016-10-27 | Государственное образовательное учреждение высшего профессионального образования "Челябинский государственный педагогический университет" | Method of producing titanium dioxide |
| CN108837806A (en) * | 2018-06-28 | 2018-11-20 | 沈阳理工大学 | A kind of preparation method of water treatment ceramsite filter |
| CN108837806B (en) * | 2018-06-28 | 2020-11-06 | 沈阳理工大学 | Preparation method of water treatment ceramsite filter material |
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