CN102228836B - Composite oxide photochemical catalyst Li3Co2Nb(1-x)TaxO6 responded by visible light and preparation method thereof - Google Patents
Composite oxide photochemical catalyst Li3Co2Nb(1-x)TaxO6 responded by visible light and preparation method thereof Download PDFInfo
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- CN102228836B CN102228836B CN 201110094368 CN201110094368A CN102228836B CN 102228836 B CN102228836 B CN 102228836B CN 201110094368 CN201110094368 CN 201110094368 CN 201110094368 A CN201110094368 A CN 201110094368A CN 102228836 B CN102228836 B CN 102228836B
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- photochemical catalyst
- taxo6
- li3co2nb
- visible light
- composite oxide
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- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000003054 catalyst Substances 0.000 title abstract description 28
- 239000000126 substance Substances 0.000 claims abstract description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 17
- 239000011941 photocatalyst Substances 0.000 claims description 16
- 239000013064 chemical raw material Substances 0.000 claims description 9
- 230000003292 diminished effect Effects 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract 1
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 239000011812 mixed powder Substances 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 7
- 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 6
- 229940012189 methyl orange Drugs 0.000 description 6
- 230000005855 radiation Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000003905 agrochemical Substances 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a composite oxide photochemical catalyst Li3Co2Nb(1-x)TaxO6 responded by visible light and a preparation method thereof. The chemical composition general formula of the composite oxide photochemical catalyst is shown as Li3Co2Nb(1-x)TaxO6, wherein x is more than or equal to 0 and less than or equal to 1. The method comprises the following steps: weighing and mixing chemical raw materials with analytical purity being 99.9% such as Li2CO3, CoO and Nb2O5 as well as Ta2O5 in accordance with the chemical formula Li3Co2Nb(1-x)TaxO6, wherein x is more than or equal to 0 and less than or equal to 1; placing the raw material mixture in a ball grinding tank, adding zirconia balls and absolute ethyl alcohol, carrying out ball grinding for 12 hours, mixing and grinding finely, taking out and drying, and sieving by a 200-mesh sieve; and carrying out presintering on evenly-mixed powder, keeping temperature for 8-10 hours, naturally cooling to room temperature, and using a ball grinding machine and other smashing means to diminish the particle diameter to be less than 2mu m, thus obtaining the composite oxide photochemical catalyst Li3Co2Nb(1-x)TaxO6. The preparation method is simple and is low in cost. The photochemical catalyst has the advantage of good catalytic properties, stability and application prospects; and the photochemical catalyst can be used for decomposing harmful chemicals under irradiation of the visible light.
Description
Technical field
The present invention relates to a kind of visible light-responded composite oxide photocatalyst Li
3Co
2Nb
1-xTa
xO
6(0≤x≤1) and preparation method thereof belongs 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 having absorbed the photon that is 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 the water and the agricultural chemicals in the atmosphere and the organic matters such as odorant decompose, yet the band gap of titanium dioxide is 3.2eV, only under than the short ultraviolet irradiation of 400nm, just can show activity, can only be indoor or the local work of uviol lamp arranged, almost can not utilize visible light, 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 maximum near sunshine medium wavelength visible light intensity 500nm on earth's surface, wavelength is that the energy of the visible region of 400nm-750nm approximately is 43% of sunshine gross energy, so in order to utilize efficiently solar spectrum, searching has the attention that visible light-responded photochemical catalyst has caused people.
Catalysis material is having important application prospect aspect the solution energy and the environmental problem.In the last few years, photochemical catalyst has caused countries in the world scientist's concern, many famous research institutions and enterprise drop into the research that huge fund is engaged in photochemical catalyst mechanism and application in succession, and photochemical catalyst has begun to enter the stage of applying in many fields such as antibiotic, deodorization, antifouling and water treatments.Some scientists think that because photochemical catalyst has good depollution of environment effect, along with going deep into of various countries' research work, this new material will become one of most promising brand-new material product of 21 century.
Although photocatalysis research has been carried out the several years, but at present report to have visible light-responded photochemical catalyst kind still very limited, exist still that light conversion efficiency is low, the problem such as poor stability and spectrum respective range are narrow, be very necessary so research and develop the new visible light-responded high efficiency photocatalyst that has.
Summary of the invention
The purpose of this invention is to provide a kind of have visible light-responded compound oxide photocatalyst with and preparation method thereof.
A kind of visible light-responded compound oxide photocatalyst that has provided by the invention is characterized in that the chemical composition general formula of described compound oxide photocatalyst is: Li
3Co
2Nb
1-xTa
xO
60≤x≤1.
The preparation method of above-mentioned visible light-responded compound oxide photocatalyst, carry out according to the following steps:
1) with 99.9% analytically pure chemical raw material Li
2CO
3, CoO, Nb
2O
5And Ta
2O
5, press Li
3Co
2Nb
1-xTa
xO
6Chemical formula weigh batching, wherein 0≤x≤1;
2) raw material that step (1) prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 12h mixes levigately, takes out oven dry, 200 mesh sieves;
3) powder that step (2) is mixed is 800-900 ℃ of pre-burning, and insulation 8-10h, naturally cools to room temperature, then by pulverizing means such as ball mills particle diameter is diminished, and is lower than 2 μ m, can obtain composite oxide photocatalyst Li
3Co
2Nb
1-xTa
xO
6Powder.
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
The below will be specifically described the present invention:
1, in order to obtain employed composite oxides among the present invention, at first use solid-phase synthesis to prepare powder, namely various oxides or carbonate as raw material are measured than mixing according to the target constitutional chemistry, synthetic in air atmosphere under normal pressure again.
2, in order effectively to utilize light, the size of the photochemical catalyst among the present invention is preferably in micron level, or even nano particle, and specific area is larger.With the oxide powder of solid-phase synthesis preparation, its particle is large and surface area is less, but can particle diameter be diminished by pulverizing means such as ball mills.
3, as the simulation organic pollution, its concentration is 20mg/L with methyl orange in photocatalysis experiment of the present invention; The addition of bismuth-system compound oxide photocatalyst is 1g/L; Light source uses the xenon lamp of 300W, and the vessel that reactive tank uses pyrex to make obtain wavelength greater than 420nm long wavelength's light by wave filter, then shine photochemical catalyst; Catalysis time is set as 120min.
Embodiment
The present invention is described in detail as the basis take concrete practical operation example for the below.
Embodiment 1:
1) with 99.9% analytically pure chemical raw material Li
2CO
3, CoO and Nb
2O
5, press Li
3Co
2NbO
6The chemical formula weigh batching;
2) raw material for preparing is mixed, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 12h mixes levigately, takes out oven dry, 200 mesh sieves;
3) the above-mentioned powder that mixes is 800 ℃ of pre-burnings, and insulation 8h, naturally cools to room temperature, then by pulverizing means such as ball mills particle diameter diminished, and is lower than 2 μ m, can obtain composite oxide photocatalyst Li
3Co
2NbO
6Powder.
Prepared photochemical catalyst, under the radiation of visible light of wavelength greater than 420nm, 120min reaches 97.1% to the methyl orange clearance.
Embodiment 2:
1) with 99.9% analytically pure chemical raw material Li
2CO
3, CoO and Ta
2O
5, press Li
3Co
2TaO
6The chemical formula weigh batching;
2) raw material for preparing is mixed, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 12h mixes levigately, takes out oven dry, 200 mesh sieves;
3) the above-mentioned powder that mixes is 900 ℃ of pre-burnings, and insulation 10h, naturally cools to room temperature, then by pulverizing means such as ball mills particle diameter diminished, and is lower than 2 μ m, can obtain composite oxide photocatalyst Li
3Co
2TaO
6Powder.
Prepared photochemical catalyst, under the radiation of visible light of wavelength greater than 420nm, 120min reaches 98.9% to the methyl orange clearance.
Embodiment 3:
1) with 99.9% analytically pure chemical raw material Li
2CO
3, CoO, Nb
2O
5, Ta
2O
5, press Li
3Co
2Nb
0.5Ta
0.5O
6The chemical formula weigh batching;
2) raw material for preparing is mixed, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 12h mixes levigately, takes out oven dry, 200 mesh sieves;
3) the above-mentioned powder that mixes is 850 ℃ of pre-burnings, and insulation 9h, naturally cools to room temperature, then by pulverizing means such as ball mills particle diameter diminished, and is lower than 2 μ m, can obtain composite oxide photocatalyst Li
3Co
2Nb
0.5Ta
0.5O
6Powder.
Prepared photochemical catalyst, under the radiation of visible light of wavelength greater than 420nm, 120min reaches 98.2% to the methyl orange clearance.
Embodiment 4:
1) with 99.9% analytically pure chemical raw material Li
2CO
3, CoO, Nb
2O
5, Ta
2O
5, press Li
3Co
2Nb
0.2Ta
0.8O
6The chemical formula weigh batching.
2) chemical raw material for preparing is mixed, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 12h mixes levigately, takes out oven dry, 200 mesh sieves.
3) the above-mentioned powder that mixes is 880 ℃ of pre-burnings, and insulation 9h, naturally cools to room temperature, then pulverizes by ball mill particle diameter is diminished, and is lower than 2 μ m, can obtain composite oxide photocatalyst Li
3Co
2Nb
0.2Ta
0.8O
6Powder.
Prepared photochemical catalyst, under the radiation of visible light of wavelength greater than 420nm, 120min reaches 98.1% to the methyl orange clearance.
Embodiment 5:
1) with 99.9% analytically pure chemical raw material Li
2CO
3, CoO, Nb
2O
5, Ta
2O
5, press Li
3Co
2Nb
0.7Ta
0.3O
6The chemical formula weigh batching.
2) chemical raw material for preparing is mixed, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 12h mixes levigately, takes out oven dry, 200 mesh sieves.
3) the above-mentioned powder that mixes is 830 ℃ of pre-burnings, and insulation 9h, naturally cools to room temperature, then pulverizes by ball mill particle diameter is diminished, and is lower than 2 μ m, can obtain composite oxide photocatalyst Li
3Co
2Nb
0.7Ta
0.3O
6Powder.
Prepared photochemical catalyst, under the radiation of visible light of wavelength greater than 420nm, 120min reaches 98.5% to the methyl orange clearance.
The present invention never is limited to above embodiment.Have and Nb, the element of Ta analog structure and chemical property such as V, Sb etc. also can make the photochemical catalyst with analogous crystalline structure of the present invention and performance.The bound of each raw material, interval value, and the bound of technological parameter (such as temperature, time etc.), interval value can both realize the present invention, do not enumerate one by one embodiment at this.
The made photocatalyst powder of above inventive embodiments can be carried on the multiple matrix surface.Matrix can be glass, pottery, active carbon, quartz sand etc., and photochemical catalyst can be carried on matrix surface with the form of film.
Claims (1)
1. the application of composite oxides in visible light-responded photocatalysis is characterized in that the chemical composition general formula of described composite oxides is: Li
3Co
2Nb
1-xTa
xO
6, 0≤x≤1 wherein;
Preparation method's step of described composite oxides is:
1) with 99.9% analytically pure chemical raw material Li
2CO
3, CoO, Nb
2O
5And Ta
2O
5, press Li
3Co
2Nb
1-xTa
xO
6, chemical formula weigh batching, wherein 0≤x≤1;
2) raw material that step (1) prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 12h mixes levigately, takes out oven dry, 200 mesh sieves;
3) powder that step (2) is mixed is 800-900 ℃ of pre-burning, and insulation 8-10h, naturally cools to room temperature, then by ball mill pulverizing means particle diameter is diminished, and is lower than 2 μ m, can obtain composite oxide photocatalyst Li
3Co
2Nb
1-xTa
xO
6Powder.
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|---|---|---|---|
| CN 201110094368 CN102228836B (en) | 2011-04-13 | 2011-04-13 | Composite oxide photochemical catalyst Li3Co2Nb(1-x)TaxO6 responded by visible light and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110094368 CN102228836B (en) | 2011-04-13 | 2011-04-13 | Composite oxide photochemical catalyst Li3Co2Nb(1-x)TaxO6 responded by visible light and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102228836A CN102228836A (en) | 2011-11-02 |
| CN102228836B true CN102228836B (en) | 2013-01-23 |
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|---|---|---|---|---|
| CN103191751A (en) * | 2013-04-16 | 2013-07-10 | 桂林理工大学 | Pore structured niobate photocatalyst K6MNb15O42 and preparation method thereof |
| CN103877968B (en) * | 2014-04-07 | 2016-05-18 | 桂林理工大学 | Visible light-responded photocatalyst Li3Nb3Si2O13And preparation method thereof |
| CN104437514B (en) * | 2014-12-28 | 2016-09-28 | 桂林理工大学 | Visible light-responded photocatalyst Co3znFeSbO8and preparation method thereof |
| WO2016170454A1 (en) * | 2015-04-23 | 2016-10-27 | Umicore | Cathode material for a lithium-ion rechargeable battery |
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| CN100493698C (en) * | 2007-10-12 | 2009-06-03 | 桂林工学院 | Composite oxide photocatalyst containing lithium and preparation method |
| CN101757905B (en) * | 2010-01-02 | 2011-10-05 | 桂林理工大学 | Visible light responding composite oxide photocatalyst Li6Ti5Nb2-xTaxO18 and preparation method |
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