CN103214033B - The preparation method of the controlled spherical mesoporous titanium dioxide of size - Google Patents
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- 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 abstract description 13
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 9
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 5
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 5
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 26
- 239000000463 material Substances 0.000 abstract description 8
- 239000010936 titanium Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002159 nanocrystal Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
- 150000001298 alcohols Chemical class 0.000 abstract description 2
- 238000005886 esterification reaction Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000012798 spherical particle Substances 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 6
- 229960000935 dehydrated alcohol Drugs 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- 229910017488 Cu K Inorganic materials 0.000 description 1
- 229910017541 Cu-K Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- -1 alcohols salt Chemical class 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The preparation method of the controlled spherical mesoporous titanium dioxide of size, belongs to field of material technology.Described method steps is as follows: be dissolved in by isopropyl titanate in organic fatty alcohol, then add organic aliphatic acid, after mixing, moves to hydrothermal reaction kettle and carries out crystallization, after reaction, powder sample is centrifugal, and washing, vacuum-drying, namely obtains powder sample.The present invention, under solvent thermal condition, utilizes the water molecules controlled hydrolysis titanium source discharged lentamente in organic alcohols and Esterification reaction process, produces titanium dioxide nano-crystal and is agglomerated into spherical offspring.Meso-hole structure is then formed at the space between nanocrystal.In addition, the particle diameter of secondary spherical particle is regulated and controled by the ratio discharged between molecular weight water and material quantity in regulation and control heat-processed.The synthesis step of present method is very simple, and obtain particle morphology even, pore structure is flourishing, and size of particles is controlled.
Description
Technical field
The invention belongs to field of material technology, relate to a kind of preparation method of inorganic oxide material, particularly relate to a kind of preparation method of size adjustable mesoporous spherical titanium dioxide.
Background technology
Titanium dioxide is important inorganic oxide, and its natural abundance is high, and can be widely used in solar fuel cell, photocatalyst, gas and the numerous areas such as biosensor, lithium cell.
In order to improve titanium dioxide performance in such applications, people adopt the mode reducing size of particles or introduce microvoid structure to improve material specific surface area usually.With improve compared with surface area of sample by reducing size of particles, introduce abundant pore structure more desirable, this is that special selects shape effect and show exclusive optical characteristics because special pore structure contributes to active adsorption, the transmission of gas and liquid and other medium.In addition, have while the hundreds of nanometer of enriching pore structure can show the specific surface suitable with nanoparticle to the particle of several microns, there is more excellent chemistry, physics and thermostability.Wherein, aperture is identified as mesoporous material between the material of 2-50 nm, and it has the excellent specific property that huge specific surface area and three-dimensional open-framework and other porous material do not have, as the pore passage structure of high-sequential, the aperture of single distribution, various shapes, hole wall composition and character controllable.In addition, its tempting part is also its potential using value in many fields such as catalysis, absorption, separation and optical, electrical, magnetic.
So far, the research of synthesising mesoporous titanium dioxide is a lot, but depends on and in building-up process, add some structure directing agents, as ionic liquid, tensio-active agent, superpolymer template etc.This also makes more residual organic groups in obtained titanium dioxide sample in structure, seriously cover Adsorption, reduce performance in a particular application.Also some research attempts these organic segments of removing by the method for follow-up roasting, but can cause the inevitably problem such as destruction, particle aggregation as particle diauxic growth, pore structure, does not deal with problems equally at all.
Summary of the invention
For the problems referred to above, the invention provides a kind of synthetic method of direct synthesis size tunable mesoporous TiO 2.Under solvent thermal condition, utilize the water molecules controlled hydrolysis titanium source discharged lentamente in organic alcohols and Esterification reaction process, produce titanium dioxide nano-crystal and be agglomerated into spherical offspring.Meso-hole structure is then formed at the space between nanocrystal.In addition, the particle diameter of secondary spherical particle is regulated and controled by the ratio discharged between molecular weight water and material quantity in regulation and control heat-processed.The significant advantage of present method is that its synthesis step is very simple, and obtain particle morphology even, pore structure is flourishing, and size of particles is controlled.
Method of the present invention is carried out according to the following steps:
(1) be dissolved in 45ml organic fatty alcohol by 0.1 ~ 2g isopropyl titanate, then add 5ml organic aliphatic acid, after mixing, move to hydrothermal reaction kettle, 120 ~ 240 DEG C of crystallizations 2 ~ 24 hours, relating to equation in this process is:
CH
3CH
2OH + CH
3COOH = CH
3CH
2OOCCH
3+ H
2O
(i-PrO)
4Ti + 4H
2O = Ti(OH)
4+ 4i-PrOH
Ti(OH)
4= TiO
2+ 2 H
2O
After reaction, powder sample is centrifugal, washing, in 40 ~ 120 DEG C of vacuum-dryings 8 ~ 12 hours, namely obtains powder sample.
(2) RIGAKU D/Max 3400 x-ray diffractometer is adopted respectively:
Cu-K α/40KV/100mA, sweep velocity 1 degree/min, analytic sample crystalline structure and thing phase; Adopt the ASAP2020 type Determination of Specific Surface Area instrument of Micromeritics company of the U.S.: degassing temperature, 120 DEG C; Degassing time, 2h, measures meso-hole structure and the pore size distribution thereof of powder sample; Hitachi S-4800 type scanning electronic microscope (SEM) and ZEISS LEO 922 type transmission electron microscope (TEM), the pattern of observation nanoparticle and pore structure.
Organic aliphatic acid used in the present invention is acetic acid or propionic acid, and fatty alcohol is ethanol, propyl alcohol or butanols.
Present method also may be used for synthesizing other metal oxide, as WO
3, M
xwO
3(M is Cs, Rb, K, Na, Li), SnO
2deng.The present invention can use the facile hydrolysis materials such as respective metal alcohols salt, metal chloride, organometallics to be starting raw material.
The present invention makes full use of the process of slowly-releasing water; without the need to using template and follow-up roasting process; one step directly obtains mesoporous TiO 2; the activity site protecting surface of maximum possible and pore structure; and offspring particle diameter can regulate and control; surface area of sample is high, even aperture distribution, and pore structure is flourishing.
As Figure 1-10 shows, the controlled spherical mesoporous titanium dioxide of size prepared by the present invention, product cut size can regulate and control between 400 nm ~ 3 μm, and most probable mesoporous pore size is 3 ~ 4 nm, and specific surface area is 140 ~ 170 m
2/ g, carbon content 0.5 ~ 2 % in powder.In the present invention, the meso-hole structure of sample is flourishing, and particle morphology is even, and visible light catalytic performance is 6 times of commercialization titanium dioxide powder P25.Because prepared nano titania/micron ball has higher specific surface, controlled dimensions, certain visible absorption, even mesoporous structure, the numerous areas such as photocatalyst, solar cell, snitaryware, makeup filler can be used as.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction spectrogram of spherical mesoporous titanium dioxide;
Fig. 2 is the scanning electron microscope diagram of particle diameter 420nm spherical mesoporous titanium dioxide;
Fig. 3 is the scanning electron microscope diagram of particle diameter 850nm spherical mesoporous titanium dioxide;
Fig. 4 is the scanning electron microscope diagram of particle diameter 1150nm spherical mesoporous titanium dioxide;
Fig. 5 is the scanning electron microscope diagram of particle diameter 1.6 μm of spherical mesoporous titanium dioxide;
Fig. 6 is the scanning electron microscope diagram of particle diameter 2 μm of spherical mesoporous titanium dioxide;
Fig. 7 is the scanning electron microscope diagram of particle diameter 3 μm of spherical mesoporous titanium dioxide;
The high resolution transmission electron microscopy figure that Fig. 8 is spherical mesoporous titanium dioxide;
Fig. 9 is nitrogen adsorption and the desorption curve of spherical mesoporous titanium dioxide;
Figure 10 is the pore size distribution curve of spherical mesoporous titanium dioxide.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.Everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment 1:
The concentration of the isopropyl titanate solute adopted in this example is 7 mmol/L.
Add 45ml dehydrated alcohol in 100ml hydrothermal reaction kettle after, be added dropwise to 0.1 g isopropyl titanate, be at room temperature uniformly mixed; Add acetic acid 5 ml again, after solution mixes completely, sealed reactor, 200 DEG C of standing crystallization 4 h in baking oven.Centrifugation after cool to room temperature, uses 30 mL deionized waters and 30 mL absolute ethanol washings three times successively, after 60 DEG C of vacuum-drying, obtains titanium dioxide powder.
The mean diameter of the spherical titanium dioxide particle obtained is 420nm, specific surface area 162.8 m
2/ g, mesoporous pore size 3.45nm, pore volume 0.92cc/g, gas adsorption constant 45.44.
Embodiment 2:
The concentration of the isopropyl titanate solute adopted in this example is 14 mmol/L.
Add 45ml dehydrated alcohol in 100ml hydrothermal reaction kettle after, be added dropwise to 0.2 g isopropyl titanate, be at room temperature uniformly mixed; Add acetic acid 5 ml again, after solution mixes completely, sealed reactor, 200 DEG C of standing crystallization 4 h in baking oven.Centrifugation after cool to room temperature, uses 30 mL deionized waters and 30 mL absolute ethanol washings three times successively, after vacuum-drying, obtains titanium dioxide powder.
The spherical titanium dioxide average particle diameter obtained is 850nm, specific surface area 172.8 m
2/ g, mesoporous pore size 3.4nm, pore volume 0.11cc/g, gas adsorption constant 57.306.
Embodiment 3:
The concentration of the isopropyl titanate solute adopted in this example is 28 mmol/L.
Add 45ml dehydrated alcohol in 100ml hydrothermal reaction kettle after, be added dropwise to 0.4 g isopropyl titanate, be at room temperature uniformly mixed; Add acetic acid 5 ml again, after solution mixes completely, sealed reactor, 200 DEG C of standing crystallization 4 h in baking oven.Centrifugation after cool to room temperature, uses 30 mL deionized waters and 30 mL absolute ethanol washings three times successively, after vacuum-drying, obtains titanium dioxide powder.
The spherical titanium dioxide average particle diameter obtained is 1150nm, specific surface area 181 m
2/ g, mesoporous pore size 3.86nm, pore volume 0.142cc/g, gas adsorption constant 34.831.
Embodiment 4:
The concentration of the isopropyl titanate solute adopted in this example is 70 mmol/L.
Add 45ml dehydrated alcohol in 100ml hydrothermal reaction kettle after, be added dropwise to 1 g isopropyl titanate, be at room temperature uniformly mixed; Add acetic acid 5 ml again, after solution mixes completely, sealed reactor, 200 DEG C of standing crystallization 4 h in baking oven.Centrifugation after cool to room temperature, uses 30 mL deionized waters and 30 mL absolute ethanol washings three times successively, after vacuum-drying, obtains titanium dioxide powder.
The spherical titanium dioxide average particle diameter obtained is 1600nm, specific surface area 170 m
2/ g, mesoporous pore size 3.86nm, pore volume 0.106cc/g, gas adsorption constant 36.242.
Embodiment 5:
The concentration of the isopropyl titanate solute adopted in this example is 105 mmol/L.
Add 45ml dehydrated alcohol in 100ml hydrothermal reaction kettle after, be added dropwise to 1.5 g isopropyl titanates, be at room temperature uniformly mixed; Add acetic acid 5 ml again, after solution mixes completely, sealed reactor, 200 DEG C of standing crystallization 4 h in baking oven.Centrifugation after cool to room temperature, uses 30 mL deionized waters and 30 mL absolute ethanol washings three times successively, after vacuum-drying, obtains titanium dioxide powder.
The spherical titanium dioxide average particle diameter obtained is 2000nm, specific surface area 174.7 m
2/ g, mesoporous pore size 3.4nm, pore volume 0.109cc/g, gas adsorption constant 40.8.
Embodiment 6:
The concentration of the isopropyl titanate solute adopted in this example is 140 mmol/L.
Add 45ml dehydrated alcohol in 100ml hydrothermal reaction kettle after, be added dropwise to 2 g isopropyl titanates, be at room temperature uniformly mixed; Add acetic acid 5 ml again, after solution mixes completely, sealed reactor, 200 DEG C of standing crystallization 4 h in baking oven.Centrifugation after cool to room temperature, uses 30 mL deionized waters and 30 mL absolute ethanol washings three times successively, after vacuum-drying, obtains titanium dioxide powder.
The spherical titanium dioxide average particle diameter obtained is 3000nm, specific surface area 171.6 m
2/ g, mesoporous pore size 3.42nm, pore volume 0.1cc/g, gas adsorption constant 37.8.
Embodiment 7:
This example is evaluation method and the result of the photocatalytic degradation oxynitride activity of catalyzer of the present invention.
Oxynitride photocatalysis oxidation reaction carries out on a fluidized bed reaction unit, and reaction system volume is 373 cm
3.Powder sample is scattered in the conversion zone of 20 mm × 0.5, mm × 16 mm, with the NO gas of 1ppm for reactant, light source is 450W high voltage mercury lamp and preposition Fuji triacetyl cellulose quality optical filter (only allowing wavelength to be greater than 510nm visible ray to pass through), in reaction process, light application time is 10min, and the photocatalytic activity of sample represents with the transformation efficiency of oxynitride.
Under above-mentioned reaction conditions, different-grain diameter titanium dioxide (being labeled as Ti-particle dia, as Ti-420 represents the spherical mesoporous titanium dioxide of 420nm) and the comparing result of commercialization titanium dioxide optical catalyst P25 to transformation efficiency of the oxides of nitrogen list in table 1:
The transformation efficiency of oxynitride in table 1 different catalysts
Catalyzer | P25 | Ti-420 | Ti-850 | Ti-1150 | Ti-1600 | Ti-2000 | Ti-3000 |
Transformation efficiency (%) | 4.2 | 24.4 | 9.5 | 8.5 | 8.61 | 11.7 | 10.6 |
Result shows, catalyzer of the present invention all has very high photocatalytic activity, and its activity is far above business-like titanium dioxide powder.The advantage of the catalyzer prepared by the present invention is active high, and preparation method is simple, and the activity of visible ray is high.
Claims (2)
1. a preparation method for the controlled spherical mesoporous titanium dioxide of size, is characterized in that described method steps is as follows:
0.1 ~ 2g isopropyl titanate is dissolved in 45ml organic fatty alcohol, described organic fatty alcohol is ethanol, propyl alcohol or butanols, then adds 5ml organic aliphatic acid, and described organic aliphatic acid is acetic acid or propionic acid, after mixing, move to hydrothermal reaction kettle, 120 ~ 240 DEG C of crystallizations 2 ~ 24 hours, after reaction, powder sample is centrifugal, washing, vacuum-drying temperature is 40 ~ 120 DEG C, and vacuum-drying 8 ~ 12 hours, namely obtains titanium dioxide powder.
2. the preparation method of the controlled spherical mesoporous titanium dioxide of size according to claim 1, is characterized in that the particle diameter of described titanium dioxide powder is 400 nm ~ 3 μm.
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CN103553125B (en) * | 2013-10-22 | 2015-09-16 | 渤海大学 | Prepare the method for small particle size anatase-type nanometer titanium dioxide |
CN104192902A (en) * | 2014-08-28 | 2014-12-10 | 云南大学 | Preparation method of modified mesoporous TiO2 for removing fluorinion in lead and zinc smelting waste water |
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CN101130159A (en) * | 2007-09-20 | 2008-02-27 | 中国科学院广州地球化学研究所 | Method for producing interpose porus titanium dioxide photocatalyst by hydro-thermal method in weak acid condition |
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CN101130159A (en) * | 2007-09-20 | 2008-02-27 | 中国科学院广州地球化学研究所 | Method for producing interpose porus titanium dioxide photocatalyst by hydro-thermal method in weak acid condition |
CN101792116A (en) * | 2009-05-25 | 2010-08-04 | 中国科学院等离子体物理研究所 | Method for preparing carboxylic acid-chemically modified metal oxide nanoparticles |
CN102153138A (en) * | 2010-11-02 | 2011-08-17 | 中山大学 | Graded titanium dioxide microspheres consisting of nano rods and nano granules |
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Non-Patent Citations (1)
Title |
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油酸修饰纳米TiO2粉体的制备及其光催化活性;陈友存;《安庆师范学院学报(自然科学版)》;20041130;第10卷(第04期);第1-3页 * |
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