CN101214999A - Method for preparing doping titanium dioxide nano crystal - Google Patents
Method for preparing doping titanium dioxide nano crystal Download PDFInfo
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- CN101214999A CN101214999A CNA2007101648539A CN200710164853A CN101214999A CN 101214999 A CN101214999 A CN 101214999A CN A2007101648539 A CNA2007101648539 A CN A2007101648539A CN 200710164853 A CN200710164853 A CN 200710164853A CN 101214999 A CN101214999 A CN 101214999A
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- titanium dioxide
- compound
- dioxide nano
- nano crystal
- doping
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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 26
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 239000010936 titanium Substances 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- LGQXXHMEBUOXRP-UHFFFAOYSA-N tributyl borate Chemical compound CCCCOB(OCCCC)OCCCC LGQXXHMEBUOXRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract 2
- 239000012530 fluid Substances 0.000 abstract 2
- 238000004332 deodorization Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000001954 sterilising effect Effects 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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Abstract
The invention discloses a process for preparing doped titanium dioxide nanocrystal, the steps comprise as follows that compounds of titanium and to-be-doped compounds with elements are dissolved in organic solvent, then fluid A is obtained, the fluid A is slowly dropped into the aqueous solution pH value of which is less than 6, then, the aqueous solution is stirred to form stable colloidal sols, lastly, the colloidal sols are dried. The invention doesn't need special devices and high temperature conditions, the process of preparation is simple, and the colloidal sols of the doped titanium dioxide nanocrystal which are of pure anatase phase structure can be obtained at standard temperature. The obtained nanocrystal particles of doped titanium dioxide is uniform in size distribution, and the diameter of the nanocrystal particles is less than 10 nanometers, which is provided with excellent functions of photocatalysis, deodorization and sterilization.
Description
Technical field
The present invention relates to a kind of method for preparing doping titanium dioxide nano crystal.
Background technology
Metal-oxide semiconductor (MOS) titanium dioxide (TiO
2) be semiconductor material with wide forbidden band, energy gap is about 3.0～3.41eV, and is transparent in 0.35～12 mum wavelength interval, the specific refractory power height, and have characteristic of mechanical property height, stable chemical performance or the like.Detitanium-ore-type TiO
2Has photocatalysis characteristic, at numerous photocatalyst (TiO
2, ZnO, Fe
2O
3, CdS etc.) in, TiO
2Nontoxic with it, catalytic activity is high, good stability, characteristics such as cheap and easy to get are subject to people's attention.Utilize it that organic pollutant in water is carried out photocatalytic degradation, finally generate nonpoisonous and tasteless CO
2, H
2O and some simple inorganicss.TiO
2Can only absorb the light of ultraviolet band, make its photocatalysis efficiency under daily condition low.Therefore, investigators address this problem by the doping means.Prepare dopen Nano TiO at present
2Method mainly contain hydrolysis method, chemical precipitation method, sol-gel method, microemulsion method and gas-phase reaction method etc.Wherein sol-gel method is because of simple to operate, synthetic TiO
2Purity height and granularity and favored, but this method need be done further thermal treatment (more than 350 ℃), just can obtain crystalline TiO
2And heat treatment process causes TiO easily
2Particulate is grown up and is reunited, and has influenced TiO
2Photocatalysis performance, also limited TiO
2In the application that can not stand on the high-temperature heat treatment material.So, the Detitanium-ore-type TiO of synthetic crystallization under the lower condition of temperature
2Be TiO in recent years
2Difficult problem in the preparation and focus.If can prepare Detitanium-ore-type TiO being lower than under 100 ℃ the condition
2Nano particle, and can mix different elements to regulate control TiO
2The size of nano particle is for nano-TiO
2Practical application have great importance.
Summary of the invention
The purpose of this invention is to provide a kind of method that under normal temperature condition, prepares doping titanium dioxide nano crystal.
The method of doping titanium dioxide nano crystal, step is as follows:
1) with the compound of titanium with treat that the compound dissolution of doping element is in organic solvent, get A liquid, the mol ratio for the treatment of the compound of the compound of doping element and titanium is 0.001-0.3, if the compound of titanium and treat that the mole number sum of the compound of doping element is X, the mole number of organic solvent and the ratio of X are greater than 4;
2) be adjusted to less than 6 with the pH value of acid solution with water, get B liquid, the mole number of water and the ratio of X are greater than 20;
3) B liquid is dropwise splashed in the A liquid, stir up to forming stable sols;
4) colloidal sol is dry under 15-100 ℃, remove water and organic solvent, obtain doping titanium dioxide nano crystal.
The compound of above-mentioned titanium can be butyl (tetra) titanate, titanium chloride or isopropyl titanate.Said organic solvent can be one or more in ethanol, propyl alcohol, ethylene glycol, propylene glycol, tetrahydrofuran (THF), acetone and the butanols.The acid solution of said adjusting pH value is nitric acid or hydrochloric acid.The compound of said doped element is one or more in methyl ethyl diketone vanadyl, niobium hydroxide, tetraethyl silicate, butyl borate, nickelous nitrate and the chromium nitrate.
Beneficial effect of the present invention is:
The present invention need not special device and hot conditions, and the preparation method is simple, can obtain the colloidal sol of adulterated pure anatase octahedrite phase structure titania nanoparticles under normal temperature condition.The doping titanium dioxide nano crystal particle size distribution that the present invention makes is even, and diameter has excellent photochemical catalysis, deodorizing, bactericidal property less than 10 nanometers.
Description of drawings
Fig. 1 is the photo of the transmission electron microscope of doping titanium dioxide nano crystal, and the upper right corner is its diffraction ring;
Fig. 2 is the X ray diffracting spectrum of doping titanium dioxide nano crystal.
Embodiment
Further specify the present invention below in conjunction with specific examples.
Embodiment 1
1) butyl (tetra) titanate, methyl ethyl diketone vanadyl and ethanol are stirred 30min by 1: 0.15: 6 mixed in molar ratio in container, obtain A liquid;
2) with the pH value to 5 of nitric acid adjusting water, get B liquid, the ratio of the mole number of water and butyl (tetra) titanate and methyl ethyl diketone vanadyl mole number sum is 40;
3) B liquid is dropwise splashed in the A liquid, stir up to forming stable sols;
4) colloidal sol is poured in the floorage larger container, under normal temperature, ventilation condition, placed drying, remove water and organic solvent, obtain doping titanium dioxide nano crystal.
The titania-doped crystalline transmission electron microscope photo that makes as shown in Figure 1, the upper right corner of photo is the crystalline diffraction ring.Titania-doped X-ray diffraction in crystals collection of illustrative plates as shown in Figure 2.By Fig. 1, Fig. 2 as seen, this crystal is the anatase phase titanium dioxide nanocrystal, is of a size of 5 nanometers, and even size distribution.
Embodiment 2
1) isopropyl titanate, niobium hydroxide and ethanol are stirred 15min by 1: 0.001: 10 mixed in molar ratio in container, obtain A liquid;
2) with the pH value to 3 of nitric acid adjusting water, get B liquid, the ratio of the mole number sum of the mole number of water and isopropyl titanate and niobium hydroxide is 100;
3) B liquid is dropwise splashed in the A liquid, stir up to forming stable sols;
4) colloidal sol is poured in the floorage larger container, under normal temperature, ventilation condition, placed drying, remove water and organic solvent, obtain doping titanium dioxide nano crystal.
Prepared anatase phase titanium dioxide crystalline is of a size of 7 nanometers, and even size distribution.
Embodiment 3
1) titanium chloride, methyl ethyl diketone vanadyl and propyl alcohol are stirred 30min by 1: 0.3: 18 mixed in molar ratio in container, obtain A liquid;
2) with the pH value to 2 of hydrochloric acid adjusting water, get B liquid, the ratio of the mole number of water and titanium chloride and methyl ethyl diketone vanadyl mole number sum is 150;
3) B liquid is dropwise splashed in the A liquid, stir up to forming stable sols;
4) colloidal sol is poured in the floorage larger container, under normal temperature, ventilation condition, placed drying, remove water and organic solvent, obtain doping titanium dioxide nano crystal.
Prepared anatase phase titanium dioxide crystalline is of a size of 6 nanometers, and even size distribution.
Embodiment 4
1) titanium chloride, tetraethoxy and ethylene glycol are stirred 20min by 1: 0.1: 15 mixed in molar ratio in container, obtain A liquid;
2) with the pH value to 1 of hydrochloric acid adjusting water, get B liquid, the ratio of the mole number of water and titanium chloride and tetraethoxy mole number sum is 120;
3) B liquid is dropwise splashed in the A liquid, stir up to forming stable sols;
4) colloidal sol is poured in the floorage larger container, under normal temperature, ventilation condition, placed drying, remove water and organic solvent, obtain doping titanium dioxide nano crystal.
Prepared anatase phase titanium dioxide crystalline is of a size of 4 nanometers, and even size distribution.
Claims (5)
1. method for preparing doping titanium dioxide nano crystal is characterized in that may further comprise the steps:
1) with the compound of titanium with treat that the compound dissolution of doping element is in organic solvent, get A liquid, the mol ratio for the treatment of the compound of the compound of doping element and titanium is 0.001-0.3, if the compound of titanium and treat that the mole number sum of the compound of doping element is X, the mole number of organic solvent and the ratio of X are greater than 4;
2) be adjusted to less than 6 with the pH value of acid solution with water, get B liquid, the mole number of water and the ratio of X are greater than 20;
3) B liquid is dropwise splashed in the A liquid, stir up to forming stable sols;
4) colloidal sol is dry under 15-100 ℃, remove water and organic solvent, obtain doping titanium dioxide nano crystal.
2. the method for preparing doping titanium dioxide nano crystal according to claim 1, the compound that it is characterized in that said titanium are butyl (tetra) titanate, titanium chloride or isopropyl titanate.
3. the method for preparing doping titanium dioxide nano crystal according to claim 1 is characterized in that said organic solvent is one or more in ethanol, propyl alcohol, ethylene glycol, propylene glycol, tetrahydrofuran (THF), acetone and the butanols.
4. the method for preparing doping titanium dioxide nano crystal according to claim 1 is characterized in that the acid solution of said adjusting pH value is nitric acid or hydrochloric acid.
5. the method for preparing doping titanium dioxide nano crystal according to claim 1, the compound that it is characterized in that said doped element are one or more in methyl ethyl diketone vanadyl, niobium hydroxide, tetraethyl silicate, butyl borate, nickelous nitrate and the chromium nitrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101648539A CN101214999A (en) | 2007-12-27 | 2007-12-27 | Method for preparing doping titanium dioxide nano crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101648539A CN101214999A (en) | 2007-12-27 | 2007-12-27 | Method for preparing doping titanium dioxide nano crystal |
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| Publication Number | Publication Date |
|---|---|
| CN101214999A true CN101214999A (en) | 2008-07-09 |
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| CNA2007101648539A Pending CN101214999A (en) | 2007-12-27 | 2007-12-27 | Method for preparing doping titanium dioxide nano crystal |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102712497A (en) * | 2010-01-20 | 2012-10-03 | 萨克特本化学有限责任公司 | Anatase white pigment with high light and weather resistance |
| CN106865612A (en) * | 2017-02-27 | 2017-06-20 | 陕西科技大学 | A kind of coprecipitation prepares the method that indium niobium is co-doped with titanium dioxide powder |
| CN107519852A (en) * | 2016-06-22 | 2017-12-29 | 东北林业大学 | A kind of method that normal temperature prepares efficient nano titanium dioxide optical catalyst |
| CN109502638A (en) * | 2018-12-04 | 2019-03-22 | 浙江大学 | A kind of preparation method of titanium dioxide microballoon sphere |
| CN110280236A (en) * | 2019-06-14 | 2019-09-27 | 同济大学 | A kind of chromium, solid acid nanosheet photocatalyst of niobium codope and preparation method thereof |
| CN110787803A (en) * | 2019-09-04 | 2020-02-14 | 菏泽城建新型工程材料有限公司 | Ni-doped TiO2Nano-particle photocatalyst and preparation method thereof |
| CN111001398A (en) * | 2019-11-20 | 2020-04-14 | 浙江大学 | Modified titanium dioxide catalyst with special morphology and preparation method and application thereof |
-
2007
- 2007-12-27 CN CNA2007101648539A patent/CN101214999A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102712497A (en) * | 2010-01-20 | 2012-10-03 | 萨克特本化学有限责任公司 | Anatase white pigment with high light and weather resistance |
| CN102712497B (en) * | 2010-01-20 | 2015-03-18 | 萨克特本化学有限责任公司 | Anatase white pigment with high light and weather resistance |
| CN107519852A (en) * | 2016-06-22 | 2017-12-29 | 东北林业大学 | A kind of method that normal temperature prepares efficient nano titanium dioxide optical catalyst |
| CN106865612A (en) * | 2017-02-27 | 2017-06-20 | 陕西科技大学 | A kind of coprecipitation prepares the method that indium niobium is co-doped with titanium dioxide powder |
| CN106865612B (en) * | 2017-02-27 | 2019-01-25 | 陕西科技大学 | A kind of coprecipitation prepares the method that indium niobium is co-doped with titanium dioxide powder |
| CN109502638A (en) * | 2018-12-04 | 2019-03-22 | 浙江大学 | A kind of preparation method of titanium dioxide microballoon sphere |
| CN110280236A (en) * | 2019-06-14 | 2019-09-27 | 同济大学 | A kind of chromium, solid acid nanosheet photocatalyst of niobium codope and preparation method thereof |
| CN110787803A (en) * | 2019-09-04 | 2020-02-14 | 菏泽城建新型工程材料有限公司 | Ni-doped TiO2Nano-particle photocatalyst and preparation method thereof |
| CN111001398A (en) * | 2019-11-20 | 2020-04-14 | 浙江大学 | Modified titanium dioxide catalyst with special morphology and preparation method and application thereof |
| CN111001398B (en) * | 2019-11-20 | 2021-07-06 | 浙江大学 | Modified titanium dioxide catalyst with special morphology and preparation method and application thereof |
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