CN101862661B - Method for preparing V-S co-doped titanium dioxide photocatalyst - Google Patents
Method for preparing V-S co-doped titanium dioxide photocatalyst Download PDFInfo
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- CN101862661B CN101862661B CN2010101936237A CN201010193623A CN101862661B CN 101862661 B CN101862661 B CN 101862661B CN 2010101936237 A CN2010101936237 A CN 2010101936237A CN 201010193623 A CN201010193623 A CN 201010193623A CN 101862661 B CN101862661 B CN 101862661B
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- Prior art keywords
- titanium dioxide
- ethanol
- sol
- water
- tio
- Prior art date
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000011941 photocatalyst Substances 0.000 title abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 16
- 230000003287 optical effect Effects 0.000 claims description 16
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 238000003980 solgel method Methods 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 229940041260 vanadyl sulfate Drugs 0.000 abstract 1
- 229910000352 vanadyl sulfate Inorganic materials 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 description 11
- 239000002253 acid Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 125000005287 vanadyl group Chemical group 0.000 description 1
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Abstract
The invention discloses a method for preparing a V-S co-doped titanium dioxide photocatalyst, which adopts a sol-gel method and comprises the following steps: 1), dissolving and mixing tetrabutyl orthotita and vanadylsulfate, which are precursors, in ethanol to obtain solution A; 2), mixing water and ethanol to obtain aqueous solution of ethanol; 3), adding the solution A into the aqueous solution of ethanol to perform a hydrolysis reaction, aging the product of the hydrolysis reaction to obtain titanium dioxide sol; and 4), drying the titanium dioxide sol under an infrared lamp. In the invention, a special device and a high temperature condition are not required, the preparation method is simple and low in cost and makes the realization of industrial production easily, and the prepared V-S co-doped titanium dioxide photocatalyst has high V-S co-doped titanium dioxide photocatalytic performance.
Description
Technical field
The present invention relates to the preparation method of titanium dioxide optical catalyst, especially utilize sol-gel process to prepare V, the method for the titanium dioxide optical catalyst that S mixes altogether.
Background technology
TiO
2Be important semiconductor material with wide forbidden band, the performance that has unique aspects such as electricity, optics and photochemistry owing to it causes that people pay close attention to widely.Anatase phase block TiO
2Band gap be about 3.2eV, it can only response wave length less than the light of 387nm, but since in sunshine the energy less than the light of this wavelength very little, be about 3～4%, 40% concentration of energy at visible region, how to utilize visible light to become TiO
2Move towards significant obstacle of practicability.
Doping is the important method that changes semiconductor property, Asahi R, and people such as Morikawa T are at N doped Ti O
2The aspect obtains important breakthrough, causes one and takes turns TiO
2The upsurge of doping vario-property.Can effectively utilize visible light in view of single-element mixes, the research of mixing altogether is at the recent extensive concern that obtains the researcher.
Summary of the invention
The purpose of this invention is to provide a kind of preparation V, the method for the titanium dioxide optical catalyst that S mixes altogether is to realize expanding TiO
2The photoresponse scope is improved the photocatalytic activity of titanium dioxide nanocrystalline.
Preparation V of the present invention, the method for the titanium dioxide optical catalyst that S mixes altogether, employing be sol-gel process, may further comprise the steps:
1) be precursor with butyl titanate and vanadic sulfate, wherein to account for the molar fraction of total precursor be 7～20% to vanadic sulfate, and precursor is dissolved mixing in ethanol, obtains solution A;
2) with water and ethanol according to mol ratio 10～400: 3 mix, and regulating the pH value is 1～7, obtains ethanol water;
3) solution A is dropwise joined in the ethanol water, reaction is hydrolyzed.Wherein the mol ratio of butyl titanate and vanadic sulfate and water is 1: 20～800, and reaction finishes, and ageing 48～72 hours obtains TiO 2 sol;
4) TiO 2 sol is dry under infrared lamp, obtain V, the titanium dioxide optical catalyst that S mixes altogether.
Beneficial effect of the present invention is:
1. the present invention is through V, and S mixes altogether, has changed TiO
2Band structure, expanded the photoresponse scope effectively, have excellent photocatalysis performance.
2. the present invention need not special device and hot conditions, and building-up process technology is simple, easy to operate, cost is low, is easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is V, and S mixes the X ray diffracting spectrum of titanium dioxide optical catalyst altogether; Wherein curve a is V, and S volume altogether is 0, and curve b is V, and S volume altogether is 10%;
Fig. 2 is V, and S mixes titanium dioxide optical catalyst light degradation to methyl orange under radiation of visible light altogether, and wherein curve a is V, and S volume altogether is 0, and curve b is V, and S volume altogether is 10%.
The specific embodiment
Further specify the present invention below in conjunction with instantiation.
1) be precursor with butyl titanate and vanadic sulfate, wherein to account for the molar fraction of total precursor be 10% to vanadic sulfate, and precursor is dissolved mixing in ethanol, obtains solution A;
2) water and ethanol are mixed according to mol ratio at 200: 3, using the nitre acid for adjusting pH value is 1, obtains ethanol water;
3) solution A is dropwise joined in the ethanol water, the reaction that is hydrolyzed, wherein the mol ratio of butyl titanate and vanadic sulfate and water is 1: 400, and reaction finishes, and ageing 72 hours obtains TiO 2 sol;
4) TiO 2 sol is dry under infrared lamp, obtaining crystallite dimension is the V about 4nm, and S mixes the titanium dioxide optical catalyst powder altogether.
Comparative example
Method is with embodiment 1, difference be vanadic sulfate altogether volume be 0, i.e. sulfur acid vanadyl not.
Light degradation to methyl orange under radiation of visible light is as shown in Figure 2.It shows 10%V, and the optically catalytic TiO 2 that S mixes altogether is active to be increased.
1) be precursor with butyl titanate and vanadic sulfate, wherein to account for the molar fraction of total precursor be 15% to vanadic sulfate, and precursor is dissolved mixing in ethanol, obtains solution A;
2) water and ethanol are mixed according to mol ratio at 400: 3, using the nitre acid for adjusting pH value is 5, obtains ethanol water;
3) solution A is dropwise joined in the ethanol water, the reaction that is hydrolyzed, wherein the mol ratio of butyl titanate and vanadic sulfate and water is 1: 40, and reaction finishes, and ageing 48 hours obtains TiO 2 sol.
4) TiO 2 sol is dry under infrared lamp, obtaining crystallite dimension is the V about 4nm, and S mixes the titanium dioxide optical catalyst powder altogether.
The titanium dioxide optical catalyst that 15%V, S mix altogether light degradation rate to methyl orange under radiation of visible light 4h is about 70%.
1) be precursor with butyl titanate and vanadic sulfate, wherein to account for the molar fraction of total precursor be 20% to vanadic sulfate, and precursor is dissolved mixing in ethanol, obtains solution A.
2) water and ethanol are mixed according to mol ratio at 20: 3, using the nitre acid for adjusting pH value is 7, obtains ethanol water;
3) solution A is dropwise joined in the ethanol water, the reaction that is hydrolyzed, wherein the mol ratio of butyl titanate and vanadic sulfate and water is 1: 800, and reaction finishes, and ageing 60 hours obtains TiO 2 sol.
4) TiO 2 sol is dry under infrared lamp, obtaining crystallite dimension is the V about 4nm, and S mixes the titanium dioxide optical catalyst powder altogether.
The titanium dioxide optical catalyst that 20%V, S mix altogether light degradation rate to methyl orange under radiation of visible light 4h is about 50%.
Claims (1)
1. one kind prepares V, and the method for the titanium dioxide optical catalyst that S mixes altogether is characterized in that may further comprise the steps:
1) be precursor with butyl titanate and vanadic sulfate, wherein to account for the molar fraction of total precursor be 7～20% to vanadic sulfate, and precursor is dissolved mixing in ethanol, obtains solution A;
2) with water and ethanol according to mol ratio 10～400: 3 mix, and regulating the pH value is 1～7, obtains ethanol water;
3) solution A is dropwise joined in the ethanol water, the reaction that is hydrolyzed, wherein the mol ratio of butyl titanate and vanadic sulfate and water is 1: 20～800, and reaction finishes, and ageing 48～72 hours obtains TiO 2 sol;
4) TiO 2 sol is dry under infrared lamp, obtain V, the titanium dioxide optical catalyst that S mixes altogether.
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| CN101862661B true CN101862661B (en) | 2012-01-04 |
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| CN103657685B (en) * | 2013-11-27 | 2015-08-26 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of titanium dioxide optical catalyst of sulphur vanadium codope |
| CN109012697B (en) * | 2018-08-04 | 2020-11-10 | 中国计量大学 | Sunlight all-band TiO2/VS4Method for preparing photocatalyst |
| CN108889312B (en) * | 2018-08-04 | 2020-11-10 | 中国计量大学 | A kind of preparation method of sunlight full-band photocatalytic nanoarray |
| CN108889311B (en) * | 2018-08-04 | 2020-11-10 | 中国计量大学 | A kind of preparation method of sunlight full-band photocatalytic composite material |
| CN108889310B (en) * | 2018-08-04 | 2020-11-10 | 中国计量大学 | Preparation method of sunlight full-waveband photocatalytic composite film |
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| EP1755779A1 (en) * | 2004-06-09 | 2007-02-28 | Basf Aktiengesellschaft | Method for the production of multi-metal oxide masses |
| CN1308069C (en) * | 2004-08-31 | 2007-04-04 | 中国建筑材料科学研究院 | High activity photo catalyzed air purifying powder material and its preparation method and application |
| CN101480611B (en) * | 2009-02-04 | 2010-12-08 | 北京科技大学 | A vanadium-doped titanium-based flue gas denitrification catalytic material and preparation method thereof |
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