CN103464167A - Visible-light response niobate composite oxide photocatalyst KCuNb3O9 and preparation method thereof - Google Patents
Visible-light response niobate composite oxide photocatalyst KCuNb3O9 and preparation method thereof Download PDFInfo
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- CN103464167A CN103464167A CN2013103781836A CN201310378183A CN103464167A CN 103464167 A CN103464167 A CN 103464167A CN 2013103781836 A CN2013103781836 A CN 2013103781836A CN 201310378183 A CN201310378183 A CN 201310378183A CN 103464167 A CN103464167 A CN 103464167A
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Abstract
The invention discloses a visible-light response niobate composite oxide photocatalyst KCuNb3O9 and a preparation method thereof. A chemical composition formula of the niobate photocatalyst is KCuNb3O9. The invention further discloses the preparation method of the photocatalyst. The preparation method is simple and low in cost; and the prepared photocatalyst has excellent catalysis performance, has an effect of decomposing a harmful chemical substance under visible-light irradiation, is good in stability, and has a good application prospect.
Description
Technical field
The present invention relates to a kind of visible light-responded niobates compound oxide photocatalyst KCuNb
3o
9and preparation method thereof, belong to inorganic field of photocatalytic material.
Background technology
Along with socioeconomic development, people more and more pay close attention to for the energy and ecological environment, solve energy shortage and problem of environmental pollution and be realize sustainable development, improve people's living standard and safeguard national security in the urgent need to.
From phase late 1970s, people proposed to utilize in the photochemical catalyst decomposition water and atmosphere in agricultural chemicals and the organic matter such as odorant, and application examples such as self-cleaning that scribble the surface of solids of photochemical catalyst.The principle of light-catalyzed reaction is that photochemical catalyst is after the photon absorbed higher than its band-gap energy, hole and electronics have been generated, these holes and electronics carry out respectively oxidation reaction and reduction reaction, reach the purpose of decomposing harmful chemical, organic-biological matter and sterilization.Photochemical catalyst has many kinds, and wherein most representative is titanium dioxide (TiO
2), utilized titanium dioxide in water and the agricultural chemicals in atmosphere and the organic matters such as odorant decomposed, yet the band gap of titanium dioxide is 3.2eV, only under the ultraviolet irradiation shorter than 400nm, just can show activity, can only be indoor or the local work of uviol lamp arranged, almost can not utilize visible ray, this has limited the use of titanium dioxide optical catalyst greatly.
Consider the practicality of photochemical catalyst in decomposing harmful substances, utilizing sunshine is indispensable as light source.Irradiation is near sunshine medium wavelength visible light intensity maximum 500nm on earth's surface, the energy of the visible region that wavelength is 400nm ~ 750nm is approximately 43% of sunshine gross energy, so for efficient utilization, the R and D of bismuth series photocatalyst have obtained a series of great achievements, and bismuthous compound is as BiVO
4, Bi
2moO
6, Bi
2mo
2o
9, Bi
2mo
3o
12and Bi
2wO
4be reported under visible ray and there is good absorption.In addition, a series of niobiums (tantalum) hydrochlorate photochemical catalyst is widely studied owing to having higher photocatalytic activity.For example, niobate photocatalyst Pb
3nb
4o
13, BiNbO
4and Bi
2mNbO
7(M=Al, Ga, In, Y, rare earth element or Fe) etc. with niobium potassium compound oxide photocatalyst as KNbO
3, KNb
3o
8, K
4nb
6o
17and K
6nb
10.6o
30deng all thering is photocatalysis performance preferably.
Although photocatalysis research has been carried out the several years, but at present report to have visible light-responded niobate photocatalyst kind still very limited, still exist that light conversion efficiency is low, poor stability and the problem such as the spectrum respective range is narrow, so research and develop the new visible light-responded efficient niobate photocatalyst that has, be very necessary.Existing document [D. Groult, M. Hervieu, B. Raveau, J. Solid. State. Chem., 1984,53 (2): 184-192.] has been reported niobates KCuNb
3o
9synthesis and structure, but have not yet to see the research report of relevant this compounds photocatalysis performance.We are to KCuNb
3o
9, KCuTa
3o
9, NaCuNb
3o
9and NaCuNb
3o
9carry out Photocatalytic Performance Study Deng niobium, tantalates, found that KCuNb
3o
9there is excellent visible light-responded photocatalysis performance, but the compound of other composition do not have visible light-responded photocatalysis performance.
Summary of the invention
The purpose of this invention is to provide a kind of visible light-responded photochemical catalyst KCuNb that has
3o
9and preparation method thereof.
The chemical constitution formula with visible light-responded niobate photocatalyst the present invention relates to is: KCuNb
3o
9.
Preparation method's concrete steps of above-mentioned visible light-responded niobate photocatalyst are:
(1) by 99.9% analytically pure chemical raw material K
2cO
3, CuO and Nb
2o
5, press KCuNb
3o
9the chemical formula weigh batching.
(2) raw material step (1) prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 8 hours, be mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed is 1000 ~ 1050 ℃ of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, then by ball mill pulverizing means, particle diameter diminished, and lower than 2 μ m, obtains niobates KCuNb
3o
9powder.
Preparation method of the present invention is simple, cost is low, and the photochemical catalyst of preparation has good catalytic performance, has the effect of decomposing harmful chemical, organic-biological matter and sterilization under radiation of visible light.
The specific embodiment
Below will be specifically described the present invention:
1, the composite oxides in order to obtain using in the present invention, at first used solid-phase synthesis to prepare powder, the various oxides as raw material or carbonate measured than being mixed according to the target constitutional chemistry, more synthetic in air atmosphere under normal pressure.
2, in order effectively to utilize light, the size of the photochemical catalyst in the present invention is preferably in micron level, or even nano particle, and specific area is larger.The oxide powder prepared with solid-phase synthesis, its particle is large and surface area is less, but can particle diameter be diminished by ball mill pulverizing means.
3, photocatalysis experiment of the present invention is usingd methyl orange as the simulation organic pollution, and its concentration is 20mg/L; Niobate photocatalyst KCuNb
3o
9addition be 1g/L; Light source is used the xenon lamp of 300W, and the vessel that reactive tank is used pyrex to make, obtain by wave filter the light that wavelength is greater than 420nm long wavelength, then irradiates photochemical catalyst; Catalysis time is set as 120 minutes.
Embodiment 1:
(1) by 99.9% analytically pure chemical raw material K
2cO
3, CuO and Nb
2o
5, press KCuNb
3o
9the chemical formula weigh batching.
(2) raw material step (1) prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 8 hours, be mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed is 1000 ℃ of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, then by ball mill pulverizing means, particle diameter diminished, and lower than 2 μ m, obtains niobates KCuNb
3o
9powder.
Prepared photochemical catalyst, be greater than at wavelength under the radiation of visible light of 420nm, the methyl orange clearance reached to 97.8% in 120 minutes.
Embodiment 2:
(1) by 99.9% analytically pure chemical raw material K
2cO
3, CuO and Nb
2o
5, press KCuNb
3o
9the chemical formula weigh batching.
(2) raw material step (1) prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 8 hours, be mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed is 1030 ℃ of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, then by ball mill pulverizing means, particle diameter diminished, and lower than 2 μ m, obtains niobates KCuNb
3o
9powder.
Prepared photochemical catalyst, be greater than at wavelength under the radiation of visible light of 420nm, the methyl orange clearance reached to 98.2% in 120 minutes.
Embodiment 3:
(1) by 99.9% analytically pure chemical raw material K
2cO
3, CuO and Nb
2o
5, press KCuNb
3o
9the chemical formula weigh batching.
(2) raw material step (1) prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 8 hours, be mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed is 1050 ℃ of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, then by ball mill pulverizing means, particle diameter diminished, and lower than 2 μ m, obtains niobates KCuNb
3o
9powder.
Prepared photochemical catalyst, be greater than at wavelength under the radiation of visible light of 420nm, and 120min reaches 98% to the methyl orange clearance.
The present invention never is limited to above embodiment.The bound of each temperature, interval value can realize the present invention, at this, do not enumerate embodiment.
The made photocatalyst powder of above inventive embodiments can be carried on multiple matrix surface.Matrix can be glass, pottery, active carbon or quartz sand etc., and photochemical catalyst can be carried on matrix surface with the form of film.
Claims (1)
1. a niobates, as the application of visible light-responded photochemical catalyst, is characterized in that the chemical constitution formula of described niobates is: KCuNb
3o
9;
Preparation method's concrete steps of described niobates are:
(1) by 99.9% analytically pure chemical raw material K
2cO
3, CuO and Nb
2o
5, press KCuNb
3o
9the chemical formula weigh batching;
(2) raw material step (1) prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 8 hours, be mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves;
(3) powder step (2) mixed is 1000 ~ 1050 ℃ of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, then by ball mill pulverizing means, particle diameter diminished, and lower than 2 μ m, obtains niobates KCuNb
3o
9powder.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104646004A (en) * | 2015-02-26 | 2015-05-27 | 桂林理工大学 | Photocatalyst LiCu2Nb7O20 with visible light response and preparation method thereof |
CN104646002A (en) * | 2015-02-28 | 2015-05-27 | 桂林理工大学 | Photocatalyst KCuSb5O14 with visible light response and preparation method thereof |
CN104667905A (en) * | 2015-02-28 | 2015-06-03 | 桂林理工大学 | Photocatalyst LiSm2NbO6 with visible light response and preparation method thereof |
CN104667942A (en) * | 2015-02-26 | 2015-06-03 | 桂林理工大学 | Photocatalyst LiCuNb5O14 with visible light response and preparation method thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1036593A1 (en) * | 1999-03-16 | 2000-09-20 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Titanium dioxide photocatalyst with Fe3+ ions added thereon |
CN1736593A (en) * | 2005-07-28 | 2006-02-22 | 武汉理工大学 | Copper doped niobium potassium compound oxide photocatalyst and preparation process |
CN102205246A (en) * | 2011-03-25 | 2011-10-05 | 桂林理工大学 | Visible light-responsive composite oxide photocatalyst LiCuNb1-xTaxO4 and preparation method thereof |
-
2013
- 2013-08-27 CN CN201310378183.6A patent/CN103464167B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1036593A1 (en) * | 1999-03-16 | 2000-09-20 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Titanium dioxide photocatalyst with Fe3+ ions added thereon |
CN1736593A (en) * | 2005-07-28 | 2006-02-22 | 武汉理工大学 | Copper doped niobium potassium compound oxide photocatalyst and preparation process |
CN102205246A (en) * | 2011-03-25 | 2011-10-05 | 桂林理工大学 | Visible light-responsive composite oxide photocatalyst LiCuNb1-xTaxO4 and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
D.GROULT等: "A Pentagonal Tunnel Structure with Copper in Square Planar Coordination: The Oxides KCuNb3O9 and KCuTa3O9", 《JOURNAL OF SOLID STATE CHEMISTRY》, vol. 53, 31 December 1984 (1984-12-31) * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104646004A (en) * | 2015-02-26 | 2015-05-27 | 桂林理工大学 | Photocatalyst LiCu2Nb7O20 with visible light response and preparation method thereof |
CN104667942A (en) * | 2015-02-26 | 2015-06-03 | 桂林理工大学 | Photocatalyst LiCuNb5O14 with visible light response and preparation method thereof |
CN104646002A (en) * | 2015-02-28 | 2015-05-27 | 桂林理工大学 | Photocatalyst KCuSb5O14 with visible light response and preparation method thereof |
CN104667905A (en) * | 2015-02-28 | 2015-06-03 | 桂林理工大学 | Photocatalyst LiSm2NbO6 with visible light response and preparation method thereof |
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Effective date of registration: 20201203 Address after: 535300 Hequn village committee, Jiangcheng street, Pubei County, Qinzhou City, Guangxi Zhuang Autonomous Region Patentee after: Pubei gaomai New Energy Technology Co.,Ltd. Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin Construction Road No. 12 Patentee before: GUILIN University OF TECHNOLOGY |
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Granted publication date: 20150415 Termination date: 20210827 |