CN105688923A - Preparing method and application of novel visible-light responding photocatalyst Li3Ni2NbO6 - Google Patents
Preparing method and application of novel visible-light responding photocatalyst Li3Ni2NbO6 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000011941 photocatalyst Substances 0.000 title abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000000126 substance Substances 0.000 claims abstract description 20
- 230000001699 photocatalysis Effects 0.000 claims abstract description 19
- 238000009826 distribution Methods 0.000 claims abstract description 3
- 238000003836 solid-state method Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 92
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 53
- 239000002994 raw material Substances 0.000 claims description 30
- 150000001875 compounds Chemical class 0.000 claims description 25
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- 238000006555 catalytic reaction Methods 0.000 claims description 22
- 239000010955 niobium Substances 0.000 claims description 22
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 20
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 17
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 claims description 17
- 229910001416 lithium ion Inorganic materials 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 14
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 12
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 12
- 239000002738 chelating agent Substances 0.000 claims description 10
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 10
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 8
- 229910001453 nickel ion Inorganic materials 0.000 claims description 8
- 229910052758 niobium Inorganic materials 0.000 claims description 8
- -1 niobium ion Chemical class 0.000 claims description 8
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 8
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- HFLAMWCKUFHSAZ-UHFFFAOYSA-N niobium dioxide Inorganic materials O=[Nb]=O HFLAMWCKUFHSAZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910019804 NbCl5 Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 6
- AMDUMQZTBRMNMG-UHFFFAOYSA-N nickel nitric acid Chemical compound [Ni].O[N+]([O-])=O AMDUMQZTBRMNMG-UHFFFAOYSA-N 0.000 claims description 6
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 6
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 6
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 claims description 6
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 5
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 4
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 29
- 229960000907 methylthioninium chloride Drugs 0.000 description 29
- 230000015556 catabolic process Effects 0.000 description 24
- 238000006731 degradation reaction Methods 0.000 description 24
- 238000007146 photocatalysis Methods 0.000 description 10
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 7
- 239000000975 dye Substances 0.000 description 5
- 238000005286 illumination Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
- 238000010668 complexation reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910013553 LiNO Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- GRZXREUFTYRRJH-UHFFFAOYSA-N 10-oxatetracyclo[6.5.0.02,7.09,11]trideca-1,3,5,7,12-pentaene Chemical compound C12=CC=CC=C2C2=C1C1OC1C=C2 GRZXREUFTYRRJH-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 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
- 239000011701 zinc Substances 0.000 description 1
- 229960001296 zinc oxide Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8474—Niobium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical Kinetics & Catalysis (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a preparing method and application of a novel nickel-lithium-niobate photocatalyst Li3Ni2NbO6, and belongs to the field of inorganic photocatalytic materials. According to the preparing method and application, the high temperature solid state method and the chemical solution method are adopted for preparing, the preparing method is simple and easy to carry out, prepared materials are even in granularity distribution and good in chemical stability, the good photocatalytic performance is achieved, organic pollutants can be effectively degraded under visible light radiation, and the good application prospects are achieved.
Description
Technical field
The present invention relates to the preparation method of a kind of novel inorganic photocatalyst material and application thereof, particularly to the photocatalyst Li for degradable organic pollutant3Ni2NbO6And preparation method thereof。
Background technology
Photocatalysis subject is the emerging research field of the multi-crossed disciplines such as catalytic chemistry, Optical Electro-Chemistry, Semiconductor Physics, material science and environmental science。Photocatalysis technology is the basic nanotechnology being born at 20 century 70s。Photocatalyst is exactly the general designation of the chemical substance that can play catalytic action under the exciting of photon。1972, Fujishma and Honda delivered on Nature magazine and has carried out UV Light decomposing H with nano titanium oxide as light anode2O is H2And O2Research opinion。U.S. Carey in 1976 is about the report of photocatalysis Decomposition biphenyl and biphenylene oxide, it is believed that be the photocatalysis initiative research work in eliminating environmental contaminants。Along with the appearance of the outburst and ecological deterioration problem etc. of energy crisis in world wide, in this context, environmental friendliness photocatalysis technology is as new green technology, and its practical research and development are paid attention to widely。
Typical natural light catalyst is exactly our common chlorophyll, promotes that the carbon dioxide in air and hydration become oxygen and carbohydrate in the photosynthesis of plant。Early stage titanium dioxide (TiO2) as photocatalyst, there is anatase (Anatase), rutile (Rutile) and three kinds of crystal structures of brockite (Brookite), wherein only anatase structured and rutile structure has photocatalysis characteristic, owing to its oxidability is strong, stable chemical nature is nontoxic, but it is only used for ultraviolet light photocatalysis, and therefore its application is restricted。Also once more use zinc oxide (ZnO) and cadmium sulfide (CdS) as catalysis material, but the unstable chemcial property due to both, light being occurred to dissolve light-catalysed, the metal ion that dissolution is harmful to has certain bio-toxicity simultaneously。Although photocatalysis research has been carried out the several years, but at present the photocatalyst of report still suffer from that light conversion efficiency is low, poor stability and the problem such as spectrum respective range is narrow, be therefore badly in need of research and development novel photocatalyst。The great vital conjuncture that can make environment and energy the two 21st century facing mankind, once obtain and breaking through, is addressed by the research application of photocatalyst。
Chinese patent CN103191715A reports a kind of visible light-responded niobate photocatalyst K3MNb7O21And preparation method thereof, wherein M is the one in Ti, Sn and Zr；Chinese patent CN103212403A reports a kind of niobate photocatalyst Ba6MNb4O18And preparation method thereof, wherein M is the one in Ti, Sn and Zr。Both photocatalysts of preparation all have excellent catalytic performance, have the effect decomposing harmful chemical and good stability under visible light illumination, have a good application prospect。Chinese patent CN103657662A reports a kind of nickel doping zinc-oxide hierarchical structure photocatalytic nano material with visible light catalysis activity and preparation method thereof simultaneously, and this material component is Zn1-x Ni x O, whereinx=0.5 10mol%, hence it is evident that improve visible light photocatalytic degradation organic dyestuff activity, it is possible to the photocatalytic degradation being widely used in dying industrial wastewater processes。On the basis of these reports, it has been found that for Li3Ni2NbO6Photocatalytic Performance Study have not yet seen report, therefore we are to Li3Ni2NbO6Photocatalysis performance studied, found that this compound have excellence visible light-responded photocatalysis performance。
Summary of the invention
Meaning of the present invention is in that to provide niobic acid nickel lithium photocatalyst that a kind of preparation method is simple, photocatalytic activity good, have a extensive future and preparation method thereof。
For reaching object above, the technical solution used in the present invention is:
A kind of novel niobic acid nickel lithium catalysis material, its chemical formula is Li3Ni2NbO6。The sample thing of preparation is mutually pure, and its pattern presents spherical or ellipticity, even size distribution, and grain diameter is 0.1-0.2 micron。
The preparation method of the first novel niobic acid nickel lithium catalysis material as above, adopts high temperature solid-state method, is made up of following steps:
(1) with containing lithium ion Li+Compound, containing nickel ion Ni2+Compound, containing niobium ion Nb5+Compound be raw material, by formula Li3Ni2NbO6In the stoichiometric proportion of each element weigh raw material, grind and mix homogeneously；
(2) mixture precalcining precalcining 1 ~ 2 time in air atmosphere step (1) obtained, calcining heat is 300～900 DEG C, and calcination time is 3～15 hours, after natural cooling, grinds and makes its mix homogeneously；
(3) being calcined in air atmosphere by the mixture that step (2) obtains, calcining heat is 900～1300 DEG C, and calcination time is 8～16 hours, natural cooling, grinds after uniformly and namely obtains a kind of novel niobic acid nickel lithium catalysis material。
Described in above step containing lithium ion Li+Compound be lithium oxide Li2O, lithium carbonate Li2CO3, lithium nitrate LiNO3, one in Lithium hydrate LiOH and lithium chloride LiCl；Described containing nickel ion Ni2+Compound be nickel oxide NiO, nickelous carbonate NiCO3, hydroxide nickel (OH)2, nitric acid nickel (NO3)2·6H2One in O；Described contains niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, columbium dioxide NbO2, niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one。
Calcining heat described in above step (2) is 350～900 DEG C, and calcination time is 4～12 hours；Calcining heat described in step (3) is 900～1250 DEG C, and calcination time is 8～15 hours。
The preparation method of the second niobic acid as above nickel lithium catalysis material, adopts chemical solution method, is made up of following steps:
(1) by chemical formula Li3Ni2NbO6In the stoichiometric proportion of each element, weigh respectively containing lithium ion Li+Compound, containing nickel ion Ni2+Compound, containing niobium ion Nb5+Compound, the raw material weighed is dissolved separately in deionized water or nitric acid, then adds chelating agent respectively by 0.5～2.0wt% of reactant quality in each raw material, obtain the mixed liquor of each raw material；Described chelating agent is the one in citric acid, oxalic acid；
(2) mixed liquor of each raw material is slowly mixed together, stirs 1～2 hour when temperature is 50～100 DEG C, after standing, drying, obtain fluffy presoma；
(3) being calcined in air atmosphere by presoma, calcining heat is 200～500 DEG C, and calcination time is 2～12 hours, repeats this step twice；Grind and uniformly namely obtain a kind of niobic acid nickel lithium photocatalytic powder material。
(4) after natural cooling, grinding and mix homogeneously, calcine in air atmosphere, calcining heat is 500～900 DEG C, and calcination time is 5～16 hours, obtains a kind of novel molybdate catalysis material。
Described in above step containing lithium ion Li+Compound be lithium oxide Li2O, lithium carbonate Li2CO3, lithium nitrate LiNO3, one in Lithium hydrate LiOH and lithium chloride LiCl；Described containing nickel ion Ni2+Compound be nickel oxide NiO, nickelous carbonate NiCO3, hydroxide nickel (OH)2, nitric acid nickel (NO3)2·6H2One in O；Described contains niobium ion Nb5+Compound be niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one；Described chelating agent is the one in citric acid or oxalic acid。
Calcining heat described in above step (3) is 300～500 DEG C, and calcination time is 3～10 hours。Calcining heat described in step (4) is 500～850 DEG C, and calcination time is 5～12 hours。
Above-described novel niobic acid nickel lithium catalysis material, preparation method is simple, photocatalytic activity good, can as excellent inorganic catalysis material。
Compared with prior art, technical solution of the present invention advantage is in that:
(1) Li prepared3Ni2NbO6Photocatalyst thing is mutually pure, and granule is tiny and is evenly distributed, and photocatalytic activity is good, and the degradation rate of 240 minutes photocatalytic degradation methylene blues can reach 96%, it is possible to photocatalytic degradation methylene blue efficiently。
(2) Li prepared3Ni2NbO6The raw material sources of photocatalyst is extensive, cheap, and preparation method is simple, and energy consumption is low, and cost is low。
(3) present invention is prone to industrialized production, discharges without waste gas and waste liquid, environmentally friendly, Li3Ni2NbO6Photocatalyst is the inorganic catalysis material of a kind of green safety。
Accompanying drawing explanation
Fig. 1 is the Li obtained by the embodiment of the present invention 13Ni2NbO6The X-ray powder diffraction pattern of sample；
Fig. 2 is the Li obtained by the embodiment of the present invention 13Ni2NbO6The UV-Vis DRS spectrogram of sample；
Fig. 3 is the Li obtained by the embodiment of the present invention 13Ni2NbO6The SEM figure of sample；
Fig. 4 is the Li obtained by the embodiment of the present invention 13Ni2NbO6Sample degradation curve to organic dyestuff methylene blue when illumination；
Fig. 5 is the Li obtained by the embodiment of the present invention 13Ni2NbO6The kinetic curve figure of sample degradation methylene blue；
Fig. 6 is the Li obtained by the embodiment of the present invention 53Ni2NbO6The X-ray powder diffraction pattern of sample；
Fig. 7 is the Li obtained by the embodiment of the present invention 53Ni2NbO6The UV-Vis DRS spectrogram of sample；
Fig. 8 is the Li obtained by the embodiment of the present invention 53Ni2NbO6The SEM figure of sample；
Fig. 9 is the Li obtained by the embodiment of the present invention 53Ni2NbO6Sample degradation curve to organic dyestuff methylene blue when illumination；
Figure 10 is the Li obtained by the embodiment of the present invention 53Ni2NbO6The kinetic curve figure of sample degradation methylene blue。
Detailed description of the invention
Below in conjunction with drawings and Examples, technical solution of the present invention is further described。
1, in order to obtain the composite oxides used in the present invention, prepare powder first by solid-phase synthesis, namely raw material is measured ratio according to target constitutional chemistry and mix, then synthesize in air atmosphere at ambient pressure。
2 in order to effectively utilize light, and the size of the photocatalyst in the present invention is preferably in micron level, or even nanoparticle, and specific surface area is bigger。The oxide powder prepared with solid-phase synthesis, its particle is relatively big and surface area is less, but can be by using instead chemical solution method and prepare photocatalyst and make particle diameter diminish。
3, photocatalytic degradation methylene blue activity rating adopts self-control photocatalytic reaction device, illuminator is 500 watts of cylindrical shape xenon lamps, reactive tank uses the cylindrical light catalytic reaction instrument that pyrex is made, illuminator is inserted in reactive tank, and passing into condensed water cooling, during reaction, temperature is room temperature。Catalyst amount 100 milligrams, liquor capacity 250 milliliters, the concentration of methylene blue is 10 mg/litre。Catalyst is placed in reactant liquor, and catalysis time is set as 240 minutes, starts illumination after opening condensed water, a sample is taken at set intervals after illumination, centrifugal, take its supernatant, measure the absorbance of methylene blue solution with ultraviolet-visible spectrophotometer in wavelength 664-666 nanometers。According to Lambert-Beer's law, the absorbance of solution is directly proportional to concentration, therefore concentration can be replaced to calculate clearance with absorbance, as the clearance of methylene blue solution。Computing formula: degradation rate=(1-C/C0) × 100%=(1-A/A0) × 100%, wherein C0, concentration before and after C respectively photocatalytic degradation, A0, A respectively be degraded before and after absorbance。
Embodiment 1:
According to chemical formula Li3Ni2NbO6, weigh lithium oxide Li respectively2O:0.45 gram, nickel oxide NiO:1.50 gram, niobium pentaoxide Nb2O5: 1.33 grams, grinding and after mix homogeneously in agate mortar, select air atmosphere to carry out precalcining, precalcining temperature is 350 DEG C, calcination time 4 hours, is subsequently cooled to room temperature, takes out sample；The raw material of first time calcining is sufficiently mixed grinding uniformly again, air atmosphere carries out second time calcining, calcining heat 900 DEG C, calcination time 12 hours, is then cooled to room temperature, take out sample；Being placed on after finally it being again fully ground in Muffle furnace, calcine in air atmosphere, calcining heat is 1250 DEG C, and calcination time is 15 hours, grinds and obtain Li after cooling3Ni2NbO6Photocatalyst。
Referring to accompanying drawing 1, it is the X-ray powder diffraction pattern by sample prepared by the present embodiment technical scheme, and XRD test result shows, prepared Li3Ni2NbO6Crystallization is better, without other dephasigns；
Referring to accompanying drawing 2, it is the UV-Vis DRS spectrogram by sample prepared by the present embodiment technical scheme, it can be seen that this sample has absorption in visible region；
Referring to accompanying drawing 3, it is the SEM(scanning electron microscope by sample prepared by the present embodiment technical scheme) collection of illustrative plates, it can be seen that gained sample particle exists some agglomerations, its mean diameter is 1.5 microns;
Referring to accompanying drawing 4, it is by the sample degradation curve to organic dyestuff methylene blue prepared by the present embodiment technical scheme。It can be seen that the degradation rate of this sample photocatalytic degradation methylene blue reaches 75% in 240 minutes, the Li prepared is described3Ni2NbO6Material has good photocatalytic activity；
Referring to accompanying drawing 5, it is the kinetic curve figure by sample degradation methylene blue prepared by the present embodiment technical scheme, it can be seen that the apparent kinetics speed constant of this sample photocatalytic degradation methylene blue is 0.00504 minute-1。
Embodiment 2:
According to chemical formula Li3Ni2NbO6, weigh lithium carbonate Li respectively2CO3: 1.11 grams, nickelous carbonate NiCO3: 2.38 grams, columbium dioxide NbO2: 2.50 grams, grinding and after mix homogeneously in agate mortar, select air atmosphere to carry out precalcining, precalcining temperature is 400 DEG C, calcination time 5 hours, is subsequently cooled to room temperature, takes out sample；The raw material of first time calcining is sufficiently mixed grinding uniformly again, air atmosphere carries out second time calcining, calcining heat 800 DEG C, calcination time 6 hours, is then cooled to room temperature, take out sample；Being placed on after finally it being again fully ground in Muffle furnace, calcine in air atmosphere, calcining heat is 900 DEG C, and calcination time is 8 hours, grinds and obtain Li after cooling3Ni2NbO6Photocatalyst。
Its main structure and morphology, UV-Vis DRS spectrum, SEM collection of illustrative plates, the degradation rate of methylene blue is similar to embodiment 1 with the kinetic curve of degradation of methylene blue。
Embodiment 3:
According to chemical formula Li3Ni2NbO6, weigh lithium carbonate Li respectively2CO3: 1.11 grams, nickelous carbonate NiCO3: 2.38 grams, niobium pentaoxide Nb2O5: 1.33 grams, grinding and after mix homogeneously in agate mortar, select air atmosphere to carry out precalcining, precalcining temperature is 350 DEG C, calcination time 6 hours, is subsequently cooled to room temperature, takes out sample；The raw material of first time calcining is sufficiently mixed grinding uniformly again, air atmosphere carries out second time calcining, calcining heat 850 DEG C, calcination time 8 hours, is then cooled to room temperature, take out sample；Being placed on after finally it being again fully ground in Muffle furnace, calcine in air atmosphere, calcining heat is 1200 DEG C, and calcination time is 12 hours, grinds and obtain Li after cooling3Ni2NbO6Photocatalyst。
Its main structure and morphology, UV-Vis DRS spectrum, SEM collection of illustrative plates, the degradation rate of methylene blue is similar to embodiment 1 with the kinetic curve of degradation of methylene blue。
Embodiment 4:
According to chemical formula Li3Ni2NbO6, weigh lithium chloride LiCl:1.28 gram, nickel oxide NiO:1.50 gram, columbium dioxide NbO respectively2: 2.50 grams, grinding and after mix homogeneously in agate mortar, select air atmosphere to carry out precalcining, precalcining temperature is 500 DEG C, calcination time 7 hours, is subsequently cooled to room temperature, takes out sample；The raw material of first time calcining is sufficiently mixed grinding uniformly again, air atmosphere carries out second time calcining, calcining heat 900 DEG C, calcination time 11 hours, is then cooled to room temperature, take out sample；Being placed on after finally it being again fully ground in Muffle furnace, calcine in air atmosphere, calcining heat is 1100 DEG C, and calcination time is 13 hours, grinds and obtain Li after cooling3Ni2NbO6Photocatalyst。
Its main structure and morphology, UV-Vis DRS spectrum, SEM collection of illustrative plates, the degradation rate of methylene blue is similar to embodiment 1 with the kinetic curve of degradation of methylene blue。
Embodiment 5:
According to chemical formula Li3Ni2NbO6, weigh Lithium hydrate LiOH:0.72 gram, hydroxide nickel (OH) respectively2: 1.86 grams, niobium hydroxide Nb (OH)5: 1.78 grams, dissolving them in and add appropriate citric acid in deionized water as chelating agent, stirring complexation obtains the mixed liquor of each raw material；The mixed liquor of each raw material is slowly mixed together, stirs 1～2 hour when temperature is 50～100 DEG C, after standing, drying, obtain fluffy presoma；Being calcined in air atmosphere by presoma, calcining heat is 300 DEG C, and calcination time is 3 hours, is subsequently cooled to room temperature, takes out sample；Raw material after first time calcining being sufficiently mixed grinding again uniformly, carries out second time calcining in air atmosphere, calcining heat 500 DEG C, calcination time is 10 hours, is then cooled to room temperature；After natural cooling, again being ground and mix homogeneously by sample, calcine in air atmosphere, calcining heat is 850 DEG C, and calcination time is 12 hours, grinds and obtain Li after cooling3Ni2NbO6Photocatalyst。
Referring to accompanying drawing 6, it is the X-ray powder diffraction pattern by sample prepared by the present embodiment technical scheme, and XRD test result shows, prepared Li3Ni2NbO6Also being monophase materials, degree of crystallinity is good；
Referring to accompanying drawing 7, it is the UV-Vis DRS spectrogram by sample prepared by the present embodiment technical scheme, it can be seen that this sample has absorption in visible region；
Referring to accompanying drawing 8, it is the SEM(scanning electron microscope by sample prepared by the present embodiment technical scheme) collection of illustrative plates, it can be seen that gained sample particle is uniformly dispersed, granularity is less, and grain diameter is 0.1-0.2 micron；
Referring to accompanying drawing 9, it is by the sample degradation curve to organic dyestuff methylene blue prepared by the present embodiment technical scheme。It can be seen that the degradation rate of this sample photocatalytic degradation methylene blue can reach 96% in 240 minutes, the Li prepared is described3Ni2NbO6Material has extraordinary photocatalytic activity；
Referring to accompanying drawing 10, it is the kinetic curve figure by sample degradation methylene blue prepared by the present embodiment technical scheme, it can be seen that the apparent kinetics speed constant of this sample photocatalytic degradation methylene blue is 0.01032 minute-1。
Embodiment 6:
According to chemical formula Li3Ni2NbO6, weigh Lithium hydrate LiOH:0.36 gram, nitric acid nickel (NO respectively3)2·6H2O:2.91 gram, niobium hydroxide Nb (OH)5: 0.89 gram, dissolving them in and add appropriate citric acid in deionized water as chelating agent, stirring complexation obtains the mixed liquor of each raw material；The mixed liquor of each raw material is slowly mixed together, stirs 1～2 hour when temperature is 50～100 DEG C, after standing, drying, obtain fluffy presoma；Being calcined in air atmosphere by presoma, calcining heat is 350 DEG C, and calcination time is 3 hours, is subsequently cooled to room temperature, takes out sample；Raw material after first time calcining being sufficiently mixed grinding again uniformly, carries out second time calcining in air atmosphere, calcining heat 400 DEG C, calcination time is 4 hours, is then cooled to room temperature；After natural cooling, again being ground and mix homogeneously by sample, calcine in air atmosphere, calcining heat is 500 DEG C, and calcination time is 5 hours, grinds and obtain Li after cooling3Ni2NbO6Photocatalyst。
Its main structure and morphology, UV-Vis DRS spectrum, SEM collection of illustrative plates, the degradation rate of methylene blue is similar to embodiment 5 with the kinetic curve of degradation of methylene blue。
Embodiment 7:
According to chemical formula Li3Ni2NbO6, weigh lithium nitrate LiNO respectively3: 2.07 grams, hydroxide nickel (OH)2: 1.86 grams, niobium chloride NbCl5: 2.71 grams, dissolving them in and add appropriate citric acid in deionized water as chelating agent, stirring complexation obtains the mixed liquor of each raw material；The mixed liquor of each raw material is slowly mixed together, stirs 1～2 hour when temperature is 50～100 DEG C, after standing, drying, obtain fluffy presoma；Being calcined in air atmosphere by presoma, calcining heat is 350 DEG C, and calcination time is 5 hours, is subsequently cooled to room temperature, takes out sample；Raw material after first time calcining being sufficiently mixed grinding again uniformly, carries out second time calcining in air atmosphere, calcining heat 450 DEG C, calcination time is 8 hours, is then cooled to room temperature；After natural cooling, again being ground and mix homogeneously by sample, calcine in air atmosphere, calcining heat is 650 DEG C, and calcination time is 10 hours, grinds and obtain Li after cooling3Ni2NbO6Photocatalyst。
Its main structure and morphology, UV-Vis DRS spectrum, SEM collection of illustrative plates, the degradation rate of methylene blue is similar to embodiment 5 with the kinetic curve of degradation of methylene blue。
Embodiment 8:
According to chemical formula Li3Ni2NbO6, weigh lithium nitrate LiNO respectively3: 1.04 grams, nitric acid nickel (NO3)2·6H2O:2.91 gram, niobium chloride NbCl5: 1.36 grams, dissolving them in and add appropriate citric acid in deionized water as chelating agent, stirring complexation obtains the mixed liquor of each raw material；The mixed liquor of each raw material is slowly mixed together, stirs 1～2 hour when temperature is 50～100 DEG C, after standing, drying, obtain fluffy presoma；Being calcined in air atmosphere by presoma, calcining heat is 300 DEG C, and calcination time is 6 hours, is subsequently cooled to room temperature, takes out sample；Raw material after first time calcining being sufficiently mixed grinding again uniformly, carries out second time calcining in air atmosphere, calcining heat 500 DEG C, calcination time is 8 hours, is then cooled to room temperature；After natural cooling, again being ground and mix homogeneously by sample, calcine in air atmosphere, calcining heat is 750 DEG C, and calcination time is 11 hours, grinds and obtain Li after cooling3Ni2NbO6Photocatalyst。
Its main structure and morphology, UV-Vis DRS spectrum, SEM collection of illustrative plates, the degradation rate of methylene blue is similar to embodiment 5 with the kinetic curve of degradation of methylene blue。
Claims (8)
1. niobic acid nickel lithium catalysis material one kind novel, it is characterised in that: its chemical formula is Li3Ni2NbO6。
2. novel niobic acid nickel lithium catalysis material according to claim 1, it is characterised in that: the sample thing of preparation is mutually pure, and its pattern presents spherical or ellipticity, even size distribution, and grain diameter is 0.1-0.2 micron。
3. a preparation method for novel niobic acid nickel lithium catalysis material as claimed in claim 1, adopts high temperature solid-state method, it is characterised in that comprise the steps:
(1) with containing lithium ion Li+Compound, containing nickel ion Ni2+Compound, containing niobium ion Nb5+Compound be raw material, by formula Li3Ni2NbO6In the stoichiometric proportion of each element weigh raw material, grind and mix homogeneously；
(2) mixture precalcining precalcining 1 ~ 2 time in air atmosphere step (1) obtained, calcining heat is 300～900 DEG C, and calcination time is 3～15 hours, after natural cooling, grinds and makes its mix homogeneously；
(3) being calcined in air atmosphere by the mixture that step (2) obtains, calcining heat is 900～1300 DEG C, and calcination time is 8～16 hours, natural cooling, grinds after uniformly and namely obtains a kind of novel niobic acid nickel lithium catalysis material。
4. the preparation method of a kind of novel niobic acid nickel lithium catalysis material according to claim 3, it is characterised in that: described contains lithium ion Li+Compound be lithium oxide Li2O, lithium carbonate Li2CO3, lithium nitrate LiNO3, one in Lithium hydrate LiOH and lithium chloride LiCl；Described containing nickel ion Ni2+Compound be nickel oxide NiO, nickelous carbonate NiCO3, hydroxide nickel (OH)2, nitric acid nickel (NO3)2·6H2One in O；Described contains niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, columbium dioxide NbO2, niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one。
5. the preparation method of a kind of novel niobic acid nickel lithium catalysis material according to claim 3, it is characterised in that: the calcining heat described in step (2) is 350～900 DEG C, and calcination time is 4～12 hours；Calcining heat described in step (3) is 900～1250 DEG C, and calcination time is 8～15 hours。
6. a preparation method for niobic acid nickel lithium catalysis material as claimed in claim 1, adopts chemical solution method, it is characterised in that comprise the following steps:
(1) by chemical formula Li3Ni2NbO6In the stoichiometric proportion of each element, weigh respectively containing lithium ion Li+Compound, containing nickel ion Ni2+Compound, containing niobium ion Nb5+Compound, the raw material weighed is dissolved separately in deionized water or nitric acid, then adds chelating agent respectively by 0.5～2.0wt% of reactant quality in each raw material, obtain the mixed liquor of each raw material；Described chelating agent is the one in citric acid, oxalic acid；
(2) mixed liquor of each raw material is slowly mixed together, stirs 1～2 hour when temperature is 50～100 DEG C, after standing, drying, obtain fluffy presoma；
(3) being calcined in air atmosphere by presoma, calcining heat is 200～500 DEG C, and calcination time is 2～12 hours, repeats this step twice；Grind and uniformly namely obtain a kind of niobic acid nickel lithium photocatalytic powder material；
(4) after natural cooling, grinding and mix homogeneously, calcine in air atmosphere, calcining heat is 500～900 DEG C, and calcination time is 5～16 hours, obtains a kind of novel molybdate catalysis material。
7. the preparation method of a kind of novel niobic acid nickel lithium catalysis material according to claim 6, it is characterised in that: described contains lithium ion Li+Compound be lithium oxide Li2O, lithium carbonate Li2CO3, lithium nitrate LiNO3, one in Lithium hydrate LiOH and lithium chloride LiCl；Described containing nickel ion Ni2+Compound be nickel oxide NiO, nickelous carbonate NiCO3, hydroxide nickel (OH)2, nitric acid nickel (NO3)2·6H2One in O；Described contains niobium ion Nb5+Compound be niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one；Described chelating agent is the one in citric acid or oxalic acid。
8. the preparation method of a kind of novel niobic acid nickel lithium catalysis material according to claim 6, it is characterised in that: the calcining heat described in step (3) is 300～500 DEG C, and calcination time is 3～10 hours；Calcining heat described in step (4) is 500～850 DEG C, and calcination time is 5～12 hours。
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Application publication date: 20160622 |