CN103214033A - Preparation method of size-controlled spherical mesoporous titanium dioxide - Google Patents
Preparation method of size-controlled spherical mesoporous titanium dioxide Download PDFInfo
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- CN103214033A CN103214033A CN201310167532XA CN201310167532A CN103214033A CN 103214033 A CN103214033 A CN 103214033A CN 201310167532X A CN201310167532X A CN 201310167532XA CN 201310167532 A CN201310167532 A CN 201310167532A CN 103214033 A CN103214033 A CN 103214033A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000000034 method 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
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 21
- 238000001291 vacuum drying Methods 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 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 19
- 239000000463 material Substances 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 8
- 239000002159 nanocrystal Substances 0.000 abstract description 5
- 239000010936 titanium Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 150000002148 esters Chemical class 0.000 abstract description 2
- 239000012798 spherical particle Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 235000014113 dietary fatty acids Nutrition 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000005886 esterification reaction Methods 0.000 abstract 1
- 229930195729 fatty acid Natural products 0.000 abstract 1
- 239000000194 fatty acid Substances 0.000 abstract 1
- 150000004665 fatty acids Chemical class 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000011163 secondary particle Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 8
- 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
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 230000001105 regulatory effect 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
- 238000005516 engineering process 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
- 150000001298 alcohols Chemical class 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
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- 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
- 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
- 239000002904 solvent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of size-controlled spherical mesoporous titanium dioxide and belongs to the technical field of materials. The preparation method comprises the following steps of: dissolving isopropyl titanate in organic fatty alcohol, and adding organic fatty acid for uniformly mixing; transferring the mixture to a hydrothermal reaction kettle for carrying out crystallization reaction; and centrifuging, washing and drying the powder in vacuum after the reaction to obtain a powder sample. The preparation method of the size-controlled spherical mesoporous titanium dioxide can be used for controlling a hydrolysis titanium source to produce titanium dioxide nanocrystals by utilizing water molecules slowly released in an esterification reaction process of organic alcohol and ester under the solvothermal condition; and the titanium dioxide nanocrystals are united into spherical secondary particles. A mesoporous structure is formed in a gap among the nanocrystals. Besides, the particle diameter of the secondary spherical particles is adjusted by adjusting the ratio of water molecule amount released in the heating process to the material amount. The preparation method of the size-controlled spherical mesoporous titanium dioxide is simple in synthesis steps, uniform in shape of the obtained particles, advanced in pore structure and controllable in particle size.
Description
Technical field
The invention belongs to the material technology field, relate to a kind of preparation method of inorganic oxide material, relate in particular to a kind of preparation method of size adjustable mesoporous spherical titanium dioxide.
Background technology
Titanium dioxide is important inorganic oxide, its natural abundance height, and can be widely used in numerous areas such as solar fuel cell, photocatalyst, gas and biosensor, lithium cell.
In order to improve the performance of titanium dioxide in these are used, people adopt the mode that reduces size of particles or introduce microvoid structure to improve the material specific surface area usually.With improve surface area of sample and compare by reducing size of particles, it is more desirable to introduce abundant pore structure, this is that special selects the shape effect and show exclusive optical characteristics because special pore structure helps active adsorption, the transmission of gas and liquid and other medium.In addition, when having the hundreds of nanometer of enriching pore structure and can show the specific surface suitable, have excellent more chemistry, physics and thermostability with nanoparticle to several microns particle.Wherein, the aperture is identified as mesoporous material between the material of 2-50 nm, and it has huge specific surface area and three-dimensional open-framework and excellent specific property that other porous material did not have, pore passage structure as high-sequential, the aperture of single distribution, shape is various, and hole wall composition and character are adjustable.In addition, its tempting part also is its potential using value in many fields such as catalysis, absorption, separation and light, electricity, magnetic.
So far, the research of synthesising mesoporous titanium dioxide is a lot, adds some structure directing agents but mainly depend in building-up process, as ionic liquid, tensio-active agent, superpolymer template etc.More residual organic groups have seriously covered the surfactivity position in this also feasible titanium dioxide sample that is obtained in structure, have reduced the performance in concrete the application.Also the method for some research by follow-up roasting attempts removing these organic segments, but can cause the unavoidable problem such as destruction, particle aggregation as particle diauxic growth, pore structure, do not deal with problems equally at all.
Summary of the invention
At the problems referred to above, the invention provides a kind of synthetic method of the directly synthetic controlled mesoporous TiO 2 of particle diameter.Under the solvent thermal condition, utilize the water molecules control hydrolysis titanium source that discharges lentamente in organic alcohols and the acid esters reaction process, produce titanium dioxide nano-crystal and be agglomerated into spherical offspring.Meso-hole structure then is formed at the space between the nanocrystal.In addition, regulate and control the particle diameter of secondary spherical particle by regulating and control the ratio that discharges in the heat-processed between molecular weight water and material quantity.The significant advantage of present method is that its synthesis step is very simple, and it is even to obtain particle morphology, the pore structure prosperity, and size of particles is controlled.
Method of the present invention is carried out according to the following steps:
(1) 0.1～2g isopropyl titanate is dissolved in the 45ml organic fatty alcohol, adds the 5ml organic aliphatic acid then, after mixing, move to hydrothermal reaction kettle, 120～240 ℃ of crystallizations 2～24 hours relate to equation and are in this process:
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 the reaction that powder sample is centrifugal, washing in 40～120 ℃ of vacuum-dryings 8～12 hours, promptly obtains powder sample.
(2) adopt RIGAKU D/Max 3400 x-ray diffractometers respectively:
Cu-K α/40KV/100mA, sweep velocity 1 degree/minute, analytic sample crystalline structure and thing are mutually; Adopt the ASAP2020 type specific surface determinator of U.S. Micromeritics company: degassing temperature, 120 ℃; The degassing time, 2h, the meso-hole structure and the pore size distribution thereof of mensuration powder sample; Hitachi S-4800 type scanning electronic microscope (SEM) and ZEISS LEO 922 type transmission electron microscopes (TEM), the pattern and the pore structure of observation nanoparticle.
Organic aliphatic acid used in the present invention is acetate or propionic acid, and Fatty Alcohol(C12-C14 and C12-C18) is ethanol, propyl alcohol or butanols.
Present method also can be used for synthetic other metal oxide, as WO
3, M
xWO
3(M is Cs, Rb, and K, Na, Li), SnO
2Deng.The present invention can use 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; need not to use template and follow-up roasting process; one step directly obtained mesoporous TiO 2; the protection of maximum possible surperficial activity site and pore structure; and the offspring particle diameter can be regulated and control; the surface area of sample height, even aperture distribution, pore structure prosperity.
Shown in Fig. 1-10, the spherical mesoporous TiO 2 of controllable size of the present invention's preparation, product cut size can be regulated and control between 400 nm～3 μ m, and most probable mesoporous aperture is 3～4 nm, and specific surface area is 140～170 m
2/ g, carbon content 0.5～2 % in the powder.The meso-hole structure prosperity of sample among the present invention, particle morphology is even, and the 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, can be used as numerous areas such as photocatalyst, solar cell, snitaryware, makeup filler.
Description of drawings
Fig. 1 is the X-ray diffraction spectrogram of spherical mesoporous TiO 2;
Fig. 2 is the scanning electron microscope diagram of the spherical mesoporous TiO 2 of particle diameter 420nm;
Fig. 3 is the scanning electron microscope diagram of the spherical mesoporous TiO 2 of particle diameter 850nm;
Fig. 4 is the scanning electron microscope diagram of the spherical mesoporous TiO 2 of particle diameter 1150nm;
Fig. 5 is the scanning electron microscope diagram of the spherical mesoporous TiO 2 of particle diameter 1.6 μ m;
Fig. 6 is the scanning electron microscope diagram of the spherical mesoporous TiO 2 of particle diameter 2 μ m;
Fig. 7 is the scanning electron microscope diagram of the spherical mesoporous TiO 2 of particle diameter 3 μ m;
Fig. 8 is for being the high resolution transmission electron microscopy figure of spherical mesoporous TiO 2;
Fig. 9 is the nitrogen adsorption and the desorption curve of spherical mesoporous TiO 2;
Figure 10 is the pore size distribution curve of spherical mesoporous TiO 2.
Embodiment
The present invention is further described below in conjunction with accompanying drawing.Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.Every technical solution of the present invention is made amendment or is equal to replacement, and do not break away 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 that adopts in this example is 7 mmol/L.
After in the 100ml hydrothermal reaction kettle, adding the 45ml dehydrated alcohol, be added dropwise to 0.1 g isopropyl titanate, at room temperature mix; Add acetate 5 ml again, treat that solution mixes fully after, sealed reactor, 200 ℃ leave standstill crystallization 4 h in baking oven.30 mL deionized waters and 30 mL absolute ethanol washings three times are used in centrifugation behind the cool to room temperature successively, after 60 ℃ of vacuum-drying, obtain titanium dioxide powder.
The mean diameter of the spherical titanium dioxide particle that obtains is 420nm, specific surface area 162.8 m
2/ g, mesoporous aperture 3.45nm, pore volume 0.92cc/g, gas adsorption constant 45.44.
Embodiment 2:
The concentration of the isopropyl titanate solute that adopts in this example is 14 mmol/L.
After in the 100ml hydrothermal reaction kettle, adding the 45ml dehydrated alcohol, be added dropwise to 0.2 g isopropyl titanate, at room temperature mix; Add acetate 5 ml again, treat that solution mixes fully after, sealed reactor, 200 ℃ leave standstill crystallization 4 h in baking oven.30 mL deionized waters and 30 mL absolute ethanol washings three times are used in centrifugation behind the cool to room temperature successively, after the vacuum-drying, obtain titanium dioxide powder.
The spherical titanium dioxide average particle diameter that obtains is 850nm, specific surface area 172.8 m
2/ g, mesoporous aperture 3.4nm, pore volume 0.11cc/g, gas adsorption constant 57.306.
Embodiment 3:
The concentration of the isopropyl titanate solute that adopts in this example is 28 mmol/L.
After in the 100ml hydrothermal reaction kettle, adding the 45ml dehydrated alcohol, be added dropwise to 0.4 g isopropyl titanate, at room temperature mix; Add acetate 5 ml again, treat that solution mixes fully after, sealed reactor, 200 ℃ leave standstill crystallization 4 h in baking oven.30 mL deionized waters and 30 mL absolute ethanol washings three times are used in centrifugation behind the cool to room temperature successively, after the vacuum-drying, obtain titanium dioxide powder.
The spherical titanium dioxide average particle diameter that obtains is 1150nm, specific surface area 181 m
2/ g, mesoporous aperture 3.86nm, pore volume 0.142cc/g, gas adsorption constant 34.831.
Embodiment 4:
The concentration of the isopropyl titanate solute that adopts in this example is 70 mmol/L.
After in the 100ml hydrothermal reaction kettle, adding the 45ml dehydrated alcohol, be added dropwise to 1 g isopropyl titanate, at room temperature mix; Add acetate 5 ml again, treat that solution mixes fully after, sealed reactor, 200 ℃ leave standstill crystallization 4 h in baking oven.30 mL deionized waters and 30 mL absolute ethanol washings three times are used in centrifugation behind the cool to room temperature successively, after the vacuum-drying, obtain titanium dioxide powder.
The spherical titanium dioxide average particle diameter that obtains is 1600nm, specific surface area 170 m
2/ g, mesoporous aperture 3.86nm, pore volume 0.106cc/g, gas adsorption constant 36.242.
Embodiment 5:
The concentration of the isopropyl titanate solute that adopts in this example is 105 mmol/L.
After in the 100ml hydrothermal reaction kettle, adding the 45ml dehydrated alcohol, be added dropwise to 1.5 g isopropyl titanates, at room temperature mix; Add acetate 5 ml again, treat that solution mixes fully after, sealed reactor, 200 ℃ leave standstill crystallization 4 h in baking oven.30 mL deionized waters and 30 mL absolute ethanol washings three times are used in centrifugation behind the cool to room temperature successively, after the vacuum-drying, obtain titanium dioxide powder.
The spherical titanium dioxide average particle diameter that obtains is 2000nm, specific surface area 174.7 m
2/ g, mesoporous aperture 3.4nm, pore volume 0.109cc/g, gas adsorption constant 40.8.
Embodiment 6:
The concentration of the isopropyl titanate solute that adopts in this example is 140 mmol/L.
After in the 100ml hydrothermal reaction kettle, adding the 45ml dehydrated alcohol, be added dropwise to 2 g isopropyl titanates, at room temperature mix; Add acetate 5 ml again, treat that solution mixes fully after, sealed reactor, 200 ℃ leave standstill crystallization 4 h in baking oven.30 mL deionized waters and 30 mL absolute ethanol washings three times are used in centrifugation behind the cool to room temperature successively, after the vacuum-drying, obtain titanium dioxide powder.
The spherical titanium dioxide average particle diameter that obtains is 3000nm, specific surface area 171.6 m
2/ g, mesoporous aperture 3.42nm, pore volume 0.1cc/g, gas adsorption constant 37.8.
Embodiment 7:
This example is the active evaluation method of photocatalytic degradation oxynitride and the result of catalyzer of the present invention.
The oxynitride photocatalysis oxidation reaction carries out on a fluidized bed reaction unit, and the reaction system volume is 373 cm
3Powder sample is scattered in the conversion zone of one 20 mm * 16 mm * 0.5 mm, NO gas with 1ppm is reactant, light source is 450W high voltage mercury lamp and preposition Fuji triacetyl cellulose matter optical filter (only allowing wavelength to pass through greater than the 510nm visible light), light application time is 10min in the reaction process, and the photocatalytic activity of sample is represented with the transformation efficiency of oxynitride.
Under the above-mentioned reaction conditions, different-grain diameter titanium dioxide (be labeled as the Ti-particle dia, represent the spherical mesoporous TiO 2 of 420nm as Ti-420) and commercialization titanium dioxide optical catalyst P25 list in table 1 to the comparing result of transformation efficiency of the oxides of nitrogen:
The transformation efficiency of oxynitride on 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 |
The result shows that 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 that the present invention is prepared is active high, and the preparation method is simple, the active height of visible light.
Claims (5)
1. the preparation method of the spherical mesoporous TiO 2 of controllable size is characterized in that described method steps is as follows:
0.1～2g isopropyl titanate is dissolved in the 45ml organic fatty alcohol, add the 5ml organic aliphatic acid then, after mixing, move to hydrothermal reaction kettle, 120～240 ℃ of crystallizations 2～24 hours, after the reaction that powder sample is centrifugal, washing, vacuum-drying 8～12 hours promptly obtains titanium dioxide powder.
2. the preparation method of the spherical mesoporous TiO 2 of controllable size according to claim 1 is characterized in that described organic aliphatic acid is acetate or propionic acid.
3. the preparation method of the spherical mesoporous TiO 2 of controllable size according to claim 1 is characterized in that described organic fatty alcohol is ethanol, propyl alcohol or butanols.
4. the preparation method of the spherical mesoporous TiO 2 of controllable size according to claim 1, the particle diameter that it is characterized in that described titanium dioxide powder is 400 nm～3 μ m.
5. the preparation method of the spherical mesoporous TiO 2 of controllable size according to claim 1 is characterized in that described vacuum-drying temperature is 40～120 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482697A (en) * | 2013-09-06 | 2014-01-01 | 浙江大学 | Method for preparing titanium dioxide microspheres with adjustable particle sizes under anhydrous solvothermal condition |
| CN103553125A (en) * | 2013-10-22 | 2014-02-05 | 渤海大学 | Method for preparing small particle size anatase nano TiO2 |
| 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 |
| CN104386744A (en) * | 2014-11-05 | 2015-03-04 | 浙江工业大学 | Method for preparing nano-porous titanium dioxide based on titanium-oxygen-cluster compounds |
| CN111100763A (en) * | 2019-12-31 | 2020-05-05 | 东莞市华畅机电科技有限公司 | Atomized cleaning agent and preparation method thereof |
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| CN103482697A (en) * | 2013-09-06 | 2014-01-01 | 浙江大学 | Method for preparing titanium dioxide microspheres with adjustable particle sizes under anhydrous solvothermal condition |
| CN103553125A (en) * | 2013-10-22 | 2014-02-05 | 渤海大学 | Method for preparing small particle size anatase nano TiO2 |
| 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 |
| CN104386744A (en) * | 2014-11-05 | 2015-03-04 | 浙江工业大学 | Method for preparing nano-porous titanium dioxide based on titanium-oxygen-cluster compounds |
| CN111100763A (en) * | 2019-12-31 | 2020-05-05 | 东莞市华畅机电科技有限公司 | Atomized cleaning agent and preparation method thereof |
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