CN102872855B - Visible-light response lithium-containing oxide photocatalyst and preparation method thereof - Google Patents
Visible-light response lithium-containing oxide photocatalyst and preparation method thereof Download PDFInfo
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- CN102872855B CN102872855B CN201210394297.5A CN201210394297A CN102872855B CN 102872855 B CN102872855 B CN 102872855B CN 201210394297 A CN201210394297 A CN 201210394297A CN 102872855 B CN102872855 B CN 102872855B
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011941 photocatalyst Substances 0.000 title abstract description 14
- 239000002223 garnet Substances 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 15
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 14
- 239000013064 chemical raw material Substances 0.000 claims description 8
- 230000003292 diminished effect Effects 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 abstract 2
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 1
- 235000010216 calcium carbonate Nutrition 0.000 abstract 1
- 238000001816 cooling 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
- 238000012216 screening Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 5
- 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
- 230000005855 radiation Effects 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction 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
- 150000001412 amines Chemical class 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229940087654 iron carbonyl Drugs 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 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
Abstract
The invention discloses visible-light response lithium-containing garnet structure oxide photocatalyst and a preparation method thereof. The lithium-containing garnet structure oxide photocatalyst has a chemical composition formula of LiCa3Mg1-xZnxV3O12, wherein x is more than or equal to 0 and is less than or equal to 1. The preparation method comprises the following steps of: 1) weighing and burdening 99.9% analytically-pure chemical raw materials Li2CO3, CaCO3, MgO, ZnO and V2O5 according to the chemical formula of LiCa3Mg1-xZnxV3O12, wherein x is more than or equal to 0 and is less than or equal to 1; 2) mixing the burdened raw materials in step 1), putting into a ball-milling tank, adding zirconia balls and absolute ethyl alcohol, carrying out ball milling for 2-8 hours, mixing, levigating, taking out to dry, and screening by a sieve of 200 meshes; and 3) pre-sintering the materials obtained in step 2) at the temperature of 850-925DEG C, keeping temperature for 6-8 hours, naturally cooling to the room temperature, and reducing the particle diameter by smashing means, such as a ball mill to reach 2mu m. The preparation method disclosed by the invention is simple and low in cost, the prepared photocatalyst has the excellent catalytic performance, and has the action on decomposing harmful chemical substances and organic biomasses as well as sterilizing under the irradiation of visible light.
Description
Technical field
The present invention relates to a kind of visible light-responded otide containing lighium object light catalyst LiCa
3mg
1-xzn
xv
3o
12(0≤x≤1) and preparation method thereof, belongs to inorganic field of photocatalytic material.
Background technology
Environmental pollution is the problem that countries in the world are extremely paid close attention to, and has caused drinking water source, the industry water source quality of people's lives constantly to decline, and causes atmosphere pollution constantly to aggravate, and causes the continuous destruction of ecological environment, and the mankind's existence is constituted a serious threat.In order to address these problems, people control by the whole bag of tricks and curb environmental pollution.
From phase late 1970s, people proposed to utilize in 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.At present, the photochemical catalyst using is mainly titanium dioxide, utilized titanium dioxide to decompose organic matters such as the agricultural chemicals in water and in atmosphere and odorants, yet the band gap of titanium dioxide is 3.2eV, only under the ultraviolet irradiation shorter than 400nm, just can show activity, can only almost can not utilize visible ray indoor or have the local work of uviol lamp, 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 is approximately 43% of sunshine gross energy, so in order to utilize efficiently solar spectrum, find and there is the attention that visible light-responded photochemical catalyst has caused people.At present report to have visible light-responded photochemical catalyst kind still very limited, so research and develop the new visible light-responded high efficiency photocatalyst that has, be very necessary.
Document [Neurgaokar RR, Hummel FA, Substitutions in Vanadate Garnets, Mater. Res. Bull., 1975, 10 [1]: 51-55], [Bayer G. The reaction of metal carbonyls and amines. I. Iron carbonyl with piperidine and n-butylamine. The initial stages of the reaction [J]. J. Am. Ceram. Soc., 1965, 48 (12): 600-605], [Yan little Song, Li Wanwan, Liu Ji, Sun Kang, a kind ofly be applicable to the single-phase white luminescent powder that black light LED excites, luminous journal., 2010, 31(1): 39-43] report respectively
?garnet structure oxide LiCa
3mgV
3o
12, LiCa
3znV
3o
12crystal structure and as the application of the luminescent material of near ultraviolet excitation, but do not relate to relevant photocatalysis performance and application thereof.In order to explore the new visible light-responded high efficiency photocatalyst that has, we are LiCa to chemical composition general formula
3mg
1-xzn
xv
3o
12series carried out Photocatalytic Performance Study containing lithium garnet structure oxide thing, found that this compounds has excellent visible light-responded photocatalysis performance.
Summary of the invention
The object of this invention is to provide a kind of have visible light-responded containing lithium garnet structure oxidation photocatalyst with and preparation method thereof.
Provided by the invention a kind ofly have the visible light-responded chemical constitution formula containing lithium garnet structure oxidation photocatalyst and be: LiCa
3mg
1-xzn
xv
3o
12(0≤x≤1).
The above-mentioned visible light-responded preparation method containing lithium garnet structure oxidation photocatalyst carries out according to the following steps:
1) by 99.9% analytically pure chemical raw material Li
2cO
3, CaCO
3, MgO, ZnO and V
2o
5, by LiCa
3mg
1-xzn
xv
3o
12chemical formula weigh batching, wherein 0≤x≤1;
2) raw material step (1) being prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 2-8 hour, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves;
3) by step (2) gained powder 850～925 ℃ of pre-burnings, and be incubated 6～8 hours, naturally cool to room temperature, then by pulverizing means such as ball mills, particle diameter is diminished, reach 2 μ m, can obtain containing lithium garnet structure oxidation photocatalyst LiCa
3mg
1-xzn
xv
3o
12(0≤x≤1) powder.
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
To be specifically described the present invention below:
1, the composite oxides in order to obtain using in the present invention, are first used solid-phase synthesis to prepare powder, the various oxides as raw material or carbonate measured than mixing according to 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 of preparing with solid-phase synthesis, its particle is compared with large and surface area is less, but can particle diameter be diminished by pulverizing means such as ball mills.
3, photocatalysis experiment of the present invention is usingd methyl orange as simulation organic pollution, and its concentration is 20mg/L; The addition of scherbinaite garnet structure oxide photochemical catalyst is 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 irradiate photochemical catalyst; Catalysis time is set as 120min.
Embodiment 1:
1) by 99.9% analytically pure chemical raw material Li
2cO
3, CaCO
3, MgO and V
2o
5, by LiCa
3mgV
3o
12chemical formula weigh batching.
2) chemical raw material step (1) being prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 2 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
3) by step (2) gained powder 850 ℃ of pre-burnings, and be incubated 8 hours, naturally cool to room temperature, then by pulverizing means such as ball mills, particle diameter is diminished, reach 2 μ m, can obtain containing lithium garnet structure oxidation photocatalyst LiCa
3mgV
3o
12powder.
Prepared photochemical catalyst, is greater than at wavelength under the radiation of visible light of 420nm, methyl orange clearance is reached to 99% in 120 minutes.
Embodiment 2:
1) by 99.9% analytically pure chemical raw material Li
2cO
3, CaCO
3, MgO, ZnO and V
2o
5, by LiCa
3mg
0.6zn
0.4v
3o
12chemical formula weigh batching.
2) chemical raw material step (1) being prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 4 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
3) by step (2) gained powder 900 ℃ of pre-burnings, and be incubated 7 hours, naturally cool to room temperature, then by pulverizing means such as ball mills, particle diameter is diminished, reach 2 μ m, can obtain containing lithium garnet structure oxidation photocatalyst LiCa
3mg
0.6zn
0.4v
3o
12powder.
Prepared photochemical catalyst, is greater than at wavelength under the radiation of visible light of 420nm, methyl orange clearance is reached to 99.4% in 120 minutes.
Embodiment 3:
1) by 99.9% analytically pure chemical raw material Li
2cO
3, CaCO
3, ZnO and V
2o
5, by LiCa
3znV
3o
12chemical formula weigh batching.
2) chemical raw material step (1) being prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
3) by step (2) gained powder 925 ℃ of pre-burnings, and be incubated 6 hours, naturally cool to room temperature, then by pulverizing means such as ball mills, particle diameter is diminished, reach 2 μ m, can obtain containing lithium garnet structure oxidation photocatalyst LiCa
3znV
3o
12powder.
Prepared photochemical catalyst, is greater than at wavelength under the radiation of visible light of 420nm, methyl orange clearance is reached to 99.2% in 120 minutes.
The present invention is never limited to above embodiment.Have with the element of the analog structures such as Mg and chemical property as Ni, Co, Cu etc. also can make the photochemical catalyst with analogous crystalline structure of the present invention and performance.Bound, the interval value of each technological parameter (as temperature, time etc.) 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, quartz sand etc., and photochemical catalyst can be carried on matrix surface with the form of film.
Claims (1)
1. the application as visible light-responded photochemical catalyst containing lithium garnet structure oxide, is characterized in that the described chemical constitution formula containing lithium garnet structure oxide is: LiCa
3mg
1-xzn
xv
3o
12, wherein: 0≤x≤1;
Described preparation method's step containing lithium garnet structure oxide is:
1) by 99.9% analytically pure chemical raw material Li
2cO
3, CaCO
3, MgO, ZnO and V
2o
5, by LiCa
3mg
1-xzn
xv
3o
12chemical formula weigh batching, wherein 0≤x≤1;
2) raw material step (1) being prepared mixes, and puts into ball grinder, adds zirconia ball and absolute ethyl alcohol, and ball milling 2-8 hour, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves;
3) by step (2) gained powder 850～925 ℃ of pre-burnings, and be incubated 6～8 hours, naturally cool to room temperature, then by ball mill pulverizing means, particle diameter is diminished, reach 2 μ m, can obtain containing lithium garnet structure oxide LiCa
3mg
1-xzn
xv
3o
12powder.
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| CN102872855B true CN102872855B (en) | 2014-09-17 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105268428A (en) * | 2015-10-10 | 2016-01-27 | 桂林理工大学 | Visible light responsive photocatalyst Li3ZnBi5O10 and preparation method thereof |
| CN106268751A (en) * | 2016-07-19 | 2017-01-04 | 桂林理工大学 | Visible light-responded photocatalyst Li2caZnGeO5and preparation method thereof |
| CN109111227A (en) * | 2018-09-24 | 2019-01-01 | 桂林理工大学 | LiCa3ZnV3O12The preparation method of microwave dielectric ceramic |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3544479A (en) * | 1967-12-28 | 1970-12-01 | Gen Electric | Lithium vanadium garnet phosphors |
| US6372095B1 (en) * | 1998-09-08 | 2002-04-16 | Kabushiki Kaisha Meidensha | Method for decomposing bromic acid by photocatalyst and apparatus therefor |
| CN102228828A (en) * | 2011-04-13 | 2011-11-02 | 桂林理工大学 | Composite oxide photocatalyst Li2ZnM3O8 and its preparation method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010046604A (en) * | 2008-08-21 | 2010-03-04 | Utsunomiya Univ | Photocatalyst, method for producing hydrogen and method for decomposing organic matter |
-
2012
- 2012-10-17 CN CN201210394297.5A patent/CN102872855B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3544479A (en) * | 1967-12-28 | 1970-12-01 | Gen Electric | Lithium vanadium garnet phosphors |
| US6372095B1 (en) * | 1998-09-08 | 2002-04-16 | Kabushiki Kaisha Meidensha | Method for decomposing bromic acid by photocatalyst and apparatus therefor |
| CN102228828A (en) * | 2011-04-13 | 2011-11-02 | 桂林理工大学 | Composite oxide photocatalyst Li2ZnM3O8 and its preparation method |
Non-Patent Citations (7)
| Title |
|---|
| .1965,全文. * |
| GERHARD BAYER.Vanadates A3B2V3O12 with Garnet Structure.< * |
| GERHARD BAYER.Vanadates A3B2V3O12 with Garnet Structure.<Journal of the American Ceramic Society>.1965,全文. |
| Journal of the American Ceramic Society> * |
| R.R. Neurgaonkar,F.A. Hummel.Substitutions in vanadate garnets.《Materials Research Bulletin》.1975,全文. * |
| V掺杂ZnO性质的第一性原理研究;王丽丽等;《山东建筑大学学报》;20120430;全文 * |
| 王丽丽等.V掺杂ZnO性质的第一性原理研究.《山东建筑大学学报》.2012, |
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Granted publication date: 20140917 Termination date: 20211017 |
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