CN106984322A - A kind of niobate photochemical catalyst and preparation method thereof - Google Patents
A kind of niobate photochemical catalyst and preparation method thereof Download PDFInfo
- Publication number
- CN106984322A CN106984322A CN201710167780.2A CN201710167780A CN106984322A CN 106984322 A CN106984322 A CN 106984322A CN 201710167780 A CN201710167780 A CN 201710167780A CN 106984322 A CN106984322 A CN 106984322A
- Authority
- CN
- China
- Prior art keywords
- photochemical catalyst
- conb
- compound
- preparation
- niobate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 27
- 150000001875 compounds Chemical class 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 17
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000007790 solid phase Substances 0.000 claims abstract description 7
- PWYYWQHXAPXYMF-UHFFFAOYSA-N strontium(2+) Chemical compound [Sr+2] PWYYWQHXAPXYMF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000001788 irregular Effects 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 4
- 239000012798 spherical particle Substances 0.000 claims abstract description 3
- 239000010955 niobium Substances 0.000 claims description 17
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 11
- 230000001699 photocatalysis Effects 0.000 claims description 10
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 8
- 238000007146 photocatalysis Methods 0.000 claims description 8
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 claims description 7
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 7
- 229910021281 Co3O4In Inorganic materials 0.000 claims description 5
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 5
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 claims description 5
- 229910052712 strontium Inorganic materials 0.000 claims description 5
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 150000002822 niobium compounds Chemical class 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 17
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 11
- 229960000907 methylthioninium chloride Drugs 0.000 description 11
- 230000015556 catabolic process Effects 0.000 description 10
- 238000006731 degradation reaction Methods 0.000 description 10
- 229910002651 NO3 Inorganic materials 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- GQHZBSPNWMRGMM-UHFFFAOYSA-N [Co].[Sr] Chemical compound [Co].[Sr] GQHZBSPNWMRGMM-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 5
- 229910052758 niobium Inorganic materials 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 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 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 description 2
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical group [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000005303 weighing 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 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
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- B01J35/39—
-
- 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
-
- 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
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
A kind of niobate photochemical catalyst and preparation method thereof, belongs to inorganic photochemical catalyst and preparation method thereof.The catalysis material chemical general formula is Sr3CoNb2O9, irregular particle shape or spherical particle are prepared into using solid phase method；Method for preparing solid phase, step is as follows：(1) according to chemical formula Sr3CoNb2O9Metering ratio, weigh respectively containing Sr2+、Co2+/Co3+And Nb5+Compound, be fully ground in mortar, be well mixed；(2) step (1) is weighed and grinds uniform mixture and calcined in air atmosphere, calcining heat is 650~850 DEG C, calcination time is 3~8 hours；(3) after the mixture natural cooling for calcining step (2), grind and be well mixed, calcined in air atmosphere, calcining heat is 1000~1300 DEG C, calcination time is 6~10 hours；Natural cooling obtains niobates catalysis material.Advantage：Preparation process is simple and easy to apply, and production cost is low, simple to equipment requirement；Chemical stability is good, is easy to industrialized production.
Description
Technical field
The present invention relates to a kind of inorganic photochemical catalyst and preparation method thereof, particularly a kind of niobate photochemical catalyst and its
Preparation method.
Background technology
With continuing to develop for industry, the destruction of various natural resources, environmental pollution is increasingly serious, is given birth to as the mankind are threatened
The serious problems deposited.Vast scientific worker expands a series of pollution administrations, the research of environmental protection.Since 1972
Year, Japanese scholars Fujishima and Honda had found TiO2Since can be with light degradation water, photochemical catalyst can solve energy as one kind
A kind of potential key technology of source crisis and environmental pollution and the concern for being increasingly subject to people.In past 20 years, researcher
Except to TiO2Modification outside, be also actively working to the new effective photochemical catalyst of research, such as oxide, sulfide, oxysulfide,
Nitride, nitrogen oxides etc..
Efficient light-catalyzed reaction can utilize the harmful and noxious substance in the direct decomposition water of solar energy, environment.Photocatalysis
Mechanism be exactly semiconductor under the exciting of light, electronics transits to conduction band from valence band, is left in valence band on photohole, conduction band
Form light induced electron；Produced photo-generated carrier reaches the surface of semiconductor under the effect such as diffusion, is inhaled with catalyst surface
Attached oxygen, water or pollutant etc. are acted on.Because reduction and the oxidability of electron-hole pair, they can directly and pollution
Thing is reacted, or hydrone or oxygen can also be made to be excited into the freedom with strong oxidation performance such as hydroxyl and superoxide radical
They are resolved into harmless small molecule, carbon dioxide, water etc., not resulted in secondary by the organic pollution in base, degraded environment
Pollution.At present, most widely used catalysis material belongs to elastic braid n-type semiconductor, such as TiO2, ZnO, ZnS etc., wherein with
TiO2Use it is most extensive.But TiO2The photoelectron produced after light irradiation is easily combined again with hole, so as to lose work
Property, cause its photocatalysis efficiency low, no more than 28%.One of key issue of photocatalysis research is that developmental research has visible ray
The catalysis material of response.Current researcher is by a series of modifications to catalysis material, and the means such as doping, compound are widened can
See the response of light, or find other emerging catalysis materials.
Its immediate element of niobium element (V, Zr, Mo) is more or less the same in terms of electronegativity and ionic radius, but interesting
, the catalysis behavior of niobium compound and the compound of surrounding element are very different.The characteristic of the compound of niobium is that it has rush
Enter agent and the effect of carrier.Niobates and containing niobium compound in the catalytic reaction of acid condition, show well catalysis live
Property, selectivity and stability, can effectively remove the nitrogen oxides in industrial waste gas and vehicle exhaust and organic print of degrading
Contaminate waste water；And under the irradiation of ultraviolet light or visible ray, some niobates can release hydrogen and oxygen by decomposition water completely, so as to give
People's research and development green energy resource technology opens a new way.
The content of the invention
The invention aims to provide a kind of preparation method it is simple, to the visible light photocatalytic degradation of many organic pollutions
Niobate photochemical catalyst of function admirable and preparation method thereof.
The object of the present invention is achieved like this：The present invention includes niobate photochemical catalyst and niobate photochemical catalyst
Preparation method.
Described niobate photochemical catalyst, niobate photochemical catalyst, chemical formula is Sr3CoNb2O9；Wherein, press
Sr3CoNb2O9Stoichiometric proportion, weigh respectively containing Sr2+、Co2+/Co3+And Nb5+Compound；Compound containing strontium is SrCO3
With Sr (NO3)2In one kind；Compound containing cobalt ions is CoCO3、Co(NO3)2·6H2O、Co3O4In one kind；Containing niobium
Compound is Nb2O5With Nb (OH)5In one kind.Sr3CoNb2O9Mass percent be multiplied by for the amount ratio of material of each element
Respective molal weight is obtained.
Niobate photochemical catalyst preparation method is：Solid phase prepares method, is prepared into irregular particle shape or spherical particle.
The method for preparing solid phase of described niobate photocatalyst, step is as follows：
(1) according to chemical formula Sr3CoNb2O9Metering ratio, weigh respectively containing Sr2+、Co2+And Nb5+Compound, compound
Mass percent be multiplied by respective molal weight for the amount ratio of the material of each element and obtain；It is fully ground, mixes in mortar
Close uniform；
(2) step (1) is weighed and grinds uniform mixture and calcined in air atmosphere, calcining heat is 650~850
DEG C, calcination time is 3~8 hours；
(3) after the mixture natural cooling for calcining step (2), grind and be well mixed, calcine, forge in air atmosphere
It is 1000~1300 DEG C to burn temperature, and calcination time is 6~10 hours；Natural cooling obtains a kind of new niobates photocatalysis material
Material.
Wherein, the compound containing strontium is SrCO3With Sr (NO3)2In one kind；Compound containing cobalt ions is CoCO3、
Co(NO3)2·6H2O、Co3O4In one kind；Compound containing niobium is Nb2O5With Nb (OH)5In one kind.
Beneficial effect and advantage：The Sr of the present invention3CoNb2O9Photochemical catalyst, can effectively degrade has under visible light illumination
Organic pollutants, chemical stability is good, reusable edible, non-secondary pollution, with stronger application prospect；Preparation method is simple,
Chemical stability is good, and experimental cost is low, and spectral response range is wide, the organic pollution that can be used in degrading waste water.
1、Sr3CoNb2O9Catalysis material is prepared simply, less demanding to experimental facilities, is easy to operation；
2nd, Sr prepared by the present invention3CoNb2O9Catalysis material has preferable response, the catalysis material in visible region
Material can efficient catalytic degradation methylene blue, be a kind of efficient catalysis material with good photocatalytic activity.
3rd, pollution-free in the catalysis material preparation process, no waste gas and waste liquid discharge, production cost is low, environment-friendly.
Brief description of the drawings：
Fig. 1, the technical scheme of the embodiment of the present invention 1 prepares the X-ray powder diffraction pattern of sample, and XRD test results are shown,
Prepared Sr3CoNb2O9For monophase materialses, mutually exist without any other impurity thing.
Fig. 2, the Sr obtained by the embodiment of the present invention 13CoNb2O9The scanning electron microscope diagram spectrum of sample.
Fig. 3, the Sr obtained by the embodiment of the present invention 13CoNb2O9Sample UV-Vis DRS spectrum.
Fig. 4, the Sr obtained by the embodiment of the present invention 13CoNb2O9Sample is under different visible light application times to there is engine dyeing
Expect the degradation curve of methylene blue.
Embodiment
The present invention includes niobate photochemical catalyst and niobate photochemical catalyst preparation method.
Described niobate photochemical catalyst, chemical formula is Sr3CoNb2O9；Wherein, by Sr3CoNb2O9Stoichiometry
Than weighing respectively containing Sr2+、Co2+/Co3+And Nb5+Compound；Compound containing strontium is SrCO3With Sr (NO3)2In one kind；
Compound containing cobalt ions is CoCO3、Co(NO3)2·6H2O、Co3O4In one kind；Compound containing niobium is Nb2O5And Nb
(OH)5In one kind, Sr3CoNb2O9Mass percent be multiplied by respective molal weight for the amount ratio of the material of each element and obtain
.
Niobate photochemical catalyst preparation method is：Method for preparing solid phase, is prepared into irregular particle shape or spherical
Grain.
The method for preparing solid phase of described niobate photocatalyst, step is as follows：
(1) according to chemical formula Sr3CoNb2O9Metering ratio, weigh respectively containing Sr2+、Co2+And Nb5+Compound, compound
Mass percent be multiplied by respective molal weight for the amount ratio of the material of each element and obtain；It is fully ground, mixes in mortar
Close uniform；
(2) step (1) is weighed and grinds uniform mixture and calcined in air atmosphere, calcining heat is 650~850
DEG C, calcination time is 3~8 hours；
(3) after the mixture natural cooling for calcining step (2), grind and be well mixed, calcine, forge in air atmosphere
It is 1000~1300 DEG C to burn temperature, and calcination time is 6~10 hours；Natural cooling obtains a kind of new niobates photocatalysis material
Material.
The compound containing strontium is SrCO3With Sr (NO3)2In one kind；Compound containing cobalt ions is CoCO3、Co
(NO3)2·6H2O、Co3O4In one kind；Compound containing niobium is Nb2O5With Nb (OH)5In one kind.
1st, in order to obtain the photochemical catalyst used in the present invention, presoma is prepared first by required raw material, i.e., work
Ratio is measured according to target constitutional chemistry for the various metal salts or oxide of raw material, precalcining is first carried out under atmosphere in atmosphere,
Synthesized at ambient pressure in air atmosphere again.
2nd, due to there is the presence of cobalt element, catalyst color of the invention is brown, and this can effectively utilize light, and loose
Porous, specific surface area is larger, and the diffusion velocity in light induced electron and hole is fast, is conducive to the separation of carrier, so as to have preferably
Photocatalysis performance.
3rd, photocatalytic degradation methylene blue activity rating is using self-control photocatalytic reaction device, and illuminator is 500 watts of cylinders
Shape xenon lamp, reactive tank is the cylindrical light catalytic reaction instrument being made using pyrex, and illuminator is inserted into reactive tank
In, filter plate is placed between illuminator and liquid level and filters ultraviolet light and infrared light, and condensed water cooling is passed through, temperature is room during reaction
Temperature.100 milligrams of catalyst amount, 250 milliliters of liquor capacity, the concentration of methylene blue is 10 mg/litres.
Before degradation experiment starts, ready methylene blue solution is first placed in dark place for a period of time, to reach that absorption is flat
Weighing apparatus state.Catalyst is placed in reaction solution, and catalysis time is set as 120 minutes, and illumination is started after opening condensed water, every after illumination
A sample is taken within 15 minutes, centrifuges, takes its supernatant, determines sub- in wavelength 548-552 nanometers with ultraviolet-visible spectrophotometer
The absorbance of methyl blue solution.According to Lambert-Beer's law, the absorbance of solution is directly proportional to concentration, therefore available absorbance
Clearance is calculated instead of concentration, as the clearance of methylene blue solution.
Calculation formula：Degradation rate=(1-C/C0) × 100%=(1-A/A0) × 100%, wherein C0, C be respectively photocatalysis
Concentration before and after degraded, A0, A respectively be degraded before and after absorbance.
Technical solution of the present invention is further described with reference to the accompanying drawings and examples.
Embodiment 1：Sr is prepared using solid sintering technology3CoNb2O9, first, according to chemical formula Sr3CoNb2O9, weigh respectively
Strontium carbonate SrCO3：1.772 grams, cobalt carbonate CoCO3：0.476 gram, niobium pentaoxide Nb2O5：1.063 grams, ground simultaneously in mortar
Well mixed, selection air atmosphere is calcined for the first time, and temperature is 650 DEG C, and calcination time is 6 hours, is then cooled to room temperature, is taken out
Sample.Then, preceding step sample is fully ground again, is well mixed, calcined in air atmosphere, calcining heat is 1200 DEG C,
Calcination time is 8 hours, is cooled to room temperature, takes out sample, that is, obtains niobic acid cobalt strontium Sr3CoNb2O9Powder.
Referring to accompanying drawing 1, the present embodiment 1 prepares the X-ray powder diffraction figure of sample, and XRD test results are shown, prepared
Niobic acid cobalt strontium Sr3CoNb2O9For monophase materialses, exist without any other dephasign, and crystallinity is preferable.
Referring to accompanying drawing 2, the present embodiment 1 prepares the SEM figures of sample, and the material is spherical or irregular powder.Because adopting
High temperature solid-state method, so in the presence of certain agglomeration.
Referring to accompanying drawing 3, it is sample Sr prepared by the present embodiment3CoNb2O9UV-Vis DRS spectrum, from figure
As can be seen that sample is fine to the Absorption of light, absorption is respectively provided with Uv and visible light regional extent；
Referring to accompanying drawing 4, it is sample Sr prepared by the present embodiment3CoNb2O9To organic under the different ultraviolet lighting time
The degradation curve of dyestuff methylene blue.It can be seen that the degradation rate of the sample photocatalytic degradation methylene blue is at 100 points
Clock or so reaches 90%, illustrates the Sr prepared3CoNb2O9Material has certain photocatalytic activity.
Embodiment 2：Sr is prepared using solid phase method3CoNb2O9, first, according to chemical formula Sr3CoNb2O9Stoichiometric proportion,
Strontium nitrate Sr (NO are weighed respectively3)2：2.552 grams, cobaltosic oxide Co3O4：0.324 gram, niobium pentaoxide Nb2O5：1.063 gram.
Taken raw material is put into agate mortar, appropriate absolute ethyl alcohol is added, ground 30~40 minutes, then by well mixed raw material
Corundum crucible is put into, precalcining 5 hours at 700 DEG C obtain presoma after being taken out after Temperature fall.Precursor is placed in again and ground
In alms bowl, continue plus absolute ethyl alcohol is ground 30 minutes, be put into after grinding fully in crucible, it is small in calcining 8 under 1250 DEG C, air atmosphere
When, room temperature is cooled to, sample is taken out, that is, obtains niobic acid cobalt strontium Sr3CoNb2O9Powder.
Its main structure and morphology, absorbance and similar to Example 1 to the degradation rate of methylene blue.
Embodiment 3：Sr is prepared using solid phase method3CoNb2O9, first, according to chemical formula Sr3CoNb2O9Stoichiometric proportion,
Strontium carbonate SrCO is weighed respectively3：1.772 grams, cabaltous nitrate hexahydrate Co (NO3)2·6H2O：1.164 grams, niobium hydroxide Nb (OH)5：
1.424 gram.Taken raw material is put into agate mortar, appropriate absolute ethyl alcohol is added, grinds 30~40 minutes, then will mix equal
Even raw material is put into corundum crucible, precalcining 4 hours at 800 DEG C, and presoma is obtained after being taken out after Temperature fall.Again by preceding body
Body is placed in mortar, continues plus absolute ethyl alcohol is ground 40 minutes, be put into after grinding fully in crucible, in 1280 DEG C, air atmosphere
Lower calcining 6 hours, is cooled to room temperature, takes out sample, that is, obtains niobic acid cobalt strontium Sr3CoNb2O9Powder.
Its main structure and morphology, absorbance and similar to Example 1 to the degradation rate of methylene blue.
Embodiment 4：Sr is prepared using solid sintering technology3CoNb2O9, first, according to chemical formula Sr3CoNb2O9, weigh respectively
Strontium nitrate Sr (NO3)2：2.54 grams, cabaltous nitrate hexahydrate Co (NO3)2·6H2O：1.164 grams, niobium hydroxide Nb (OH)5：1.424
Gram, grind and be well mixed in mortar, selection air atmosphere is calcined for the first time, and temperature is 650 DEG C, and calcination time is 3 hours,
Then it is cooled to room temperature, takes out sample.Then, preceding step sample is fully ground again, is well mixed, calcined in air atmosphere,
Calcining heat is 1300 DEG C, and calcination time is 5 hours, is cooled to room temperature, takes out sample, that is, obtains Sr3CoNb2O9Powder.
It is its main structure and morphology, similar to Example 1 to the degradation rate of methylene blue.
Embodiment 5：Sr is prepared using solid phase method3CoNb2O9, first, according to chemical formula Sr3CoNb2O9Stoichiometric proportion,
Strontium nitrate Sr (NO are weighed respectively3)2：2.54 grams, cobalt carbonate CoCO3：0.476 gram, niobium pentaoxide Nb2O5：1.063 gram.By institute
Take raw material to be put into agate mortar, add appropriate absolute ethyl alcohol, grind 30~40 minutes, be then put into well mixed raw material
Corundum crucible, precalcining 4 hours at 850 DEG C obtain presoma after being taken out after Temperature fall.Precursor is placed in mortar again
In, continue plus absolute ethyl alcohol is ground 40 minutes, be put into after grinding fully in crucible, it is small in calcining 6 under 1250 DEG C, air atmosphere
When, room temperature is cooled to, sample is taken out, that is, obtains niobic acid cobalt strontium Sr3CoNb2O9Powder.
Claims (3)
1. a kind of niobate photochemical catalyst, it is characterized in that：Niobate photochemical catalyst, chemical formula is Sr3CoNb2O9；Wherein,
By Sr3CoNb2O9Metering ratio, weigh respectively containing Sr2+、Co2+/Co3+And Nb5+Compound；Compound containing strontium is SrCO3With
Sr(NO3)2In one kind；Compound containing cobalt ions is CoCO3、Co(NO3)2·6H2O、Co3O4In one kind；Change containing niobium
Compound is Nb2O5With Nb (OH)5In one kind.
2. a kind of preparation method of niobate photochemical catalyst described in claim 1, it is characterized in that：Niobate photochemical catalyst
Preparation method is：Method for preparing solid phase, is prepared into irregular particle shape or spherical particle.
3. a kind of its preparation method of niobate photochemical catalyst according to claim 2, it is characterized in that：Described niobic acid
The method for preparing solid phase of salt photochemical catalyst, step is as follows：
(1) according to chemical formula Sr3CoNb2O9Metering ratio, weigh respectively containing Sr2+、Co2+/Co3+And Nb5+Compound, compound
Mass percent be multiplied by respective molal weight for the amount ratio of the material of each element and obtain；It is fully ground, mixes in mortar
Close uniform；
(2) step (1) is weighed and grinds uniform mixture and calcined in air atmosphere, calcining heat is 650~850 DEG C,
Calcination time is 3~8 hours；
(3) after the mixture natural cooling for calcining step (2), grind and be well mixed, calcined in air atmosphere, calcining temperature
Spend for 1000~1300 DEG C, calcination time is 6~10 hours；Natural cooling, grinding obtains a kind of new niobates photocatalysis
Material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710167780.2A CN106984322A (en) | 2017-03-21 | 2017-03-21 | A kind of niobate photochemical catalyst and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710167780.2A CN106984322A (en) | 2017-03-21 | 2017-03-21 | A kind of niobate photochemical catalyst and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106984322A true CN106984322A (en) | 2017-07-28 |
Family
ID=59411801
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710167780.2A Pending CN106984322A (en) | 2017-03-21 | 2017-03-21 | A kind of niobate photochemical catalyst and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106984322A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935100A (en) * | 2017-11-18 | 2018-04-20 | 桂林电子科技大学 | A kind of method of degraded methylene blue solution under visible ray |
| CN113751025A (en) * | 2021-09-02 | 2021-12-07 | 西安理工大学 | MnNb3S6Preparation method and application of piezoelectric catalytic material |
| CN114314633A (en) * | 2022-01-07 | 2022-04-12 | 北京大学深圳研究生院 | Preparation method of yttrium-barium compound |
| CN115025783A (en) * | 2022-06-15 | 2022-09-09 | 河南大学 | Synthesis method and application of niobium-oxygen-rich cluster/ZIF-67 derivative composite material |
| CN115400794A (en) * | 2022-05-05 | 2022-11-29 | 河南大学 | Preparation method and application of cobaltosic oxide/niobate composite material with p-n junction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134162A (en) * | 2007-10-18 | 2008-03-05 | 桂林工学院 | Perovskite-like structure composite oxides photocatalyst and method of producing the same |
| CN105289577A (en) * | 2015-10-31 | 2016-02-03 | 江苏师范大学 | Vanadium tantalum/niobate photocatalyst and preparation method and application of vanadium tantalum/niobate photocatalyst |
| CN105597729A (en) * | 2016-01-11 | 2016-05-25 | 苏州格瑞惠农膜材料科技有限公司 | Preparing method of niobate photocatalyst Bi3Nb17O47 and application of niobate photocatalyst Bi3Nb17O47 |
-
2017
- 2017-03-21 CN CN201710167780.2A patent/CN106984322A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134162A (en) * | 2007-10-18 | 2008-03-05 | 桂林工学院 | Perovskite-like structure composite oxides photocatalyst and method of producing the same |
| CN100531899C (en) * | 2007-10-18 | 2009-08-26 | 桂林工学院 | Perovskite-like structure composite oxides photocatalyst and method of producing the same |
| CN105289577A (en) * | 2015-10-31 | 2016-02-03 | 江苏师范大学 | Vanadium tantalum/niobate photocatalyst and preparation method and application of vanadium tantalum/niobate photocatalyst |
| CN105597729A (en) * | 2016-01-11 | 2016-05-25 | 苏州格瑞惠农膜材料科技有限公司 | Preparing method of niobate photocatalyst Bi3Nb17O47 and application of niobate photocatalyst Bi3Nb17O47 |
Non-Patent Citations (1)
| Title |
|---|
| V. TING ET AL.: "A structure, conductivity and dielectric properties investigation of A3CoNb2O9 (A=Ca2+, Sr2+, Ba2+) triple perovskites", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935100A (en) * | 2017-11-18 | 2018-04-20 | 桂林电子科技大学 | A kind of method of degraded methylene blue solution under visible ray |
| CN113751025A (en) * | 2021-09-02 | 2021-12-07 | 西安理工大学 | MnNb3S6Preparation method and application of piezoelectric catalytic material |
| CN114314633A (en) * | 2022-01-07 | 2022-04-12 | 北京大学深圳研究生院 | Preparation method of yttrium-barium compound |
| CN114314633B (en) * | 2022-01-07 | 2023-08-25 | 北京大学深圳研究生院 | Preparation method of yttrium barium compound |
| CN115400794A (en) * | 2022-05-05 | 2022-11-29 | 河南大学 | Preparation method and application of cobaltosic oxide/niobate composite material with p-n junction |
| CN115400794B (en) * | 2022-05-05 | 2023-09-15 | 河南大学 | Preparation method and application of cobaltosic oxide/niobate composite material with p-n junction |
| CN115025783A (en) * | 2022-06-15 | 2022-09-09 | 河南大学 | Synthesis method and application of niobium-oxygen-rich cluster/ZIF-67 derivative composite material |
| CN115025783B (en) * | 2022-06-15 | 2023-10-27 | 河南大学 | Synthetic method and application of multi-niobium oxygen cluster/ZIF-67 derivative composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106984322A (en) | A kind of niobate photochemical catalyst and preparation method thereof | |
| CN104174408B (en) | A kind of have visible light-responded ferrochrome vanadate photocatalytic material and its preparation method and application | |
| CN102000584A (en) | Method for preparing cobalt-doped improved beta-bismuth oxide photocatalyst | |
| CN108620113B (en) | Preparation method of nitrogen-doped carbon-cerium composite nanosheet | |
| CN103157459A (en) | Visible-light-responsive vanadate photocatalyst LiMVO4 and preparation method thereof | |
| CN107175099A (en) | A kind of V ion dopings BiNb5O14Photochemical catalyst and its preparation method and application | |
| CN105597729A (en) | Preparing method of niobate photocatalyst Bi3Nb17O47 and application of niobate photocatalyst Bi3Nb17O47 | |
| Sun et al. | Photocatalytic degradation of gaseous o-xylene over M-TiO 2 (M= Ag, Fe, Cu, Co) in different humidity levels under visible-light irradiation: activity and kinetic study | |
| CN104190398A (en) | Visible light responding photocatalyst Bi2Sm4Ti5O19 and preparation method thereof | |
| CN103433049A (en) | Visible-light-responsive photocatalyst CaCuV2O7 and preparation method thereof | |
| CN103521210A (en) | Photocatalyst Bi3Sb3Zn2O14 with visible light response | |
| CN104549222A (en) | Preparation method and application of visible-light-induced photocatalyst chromium chromate | |
| CN106984323A (en) | A kind of barium niobate photochemical catalyst and preparation method thereof | |
| CN105688923A (en) | Preparing method and application of novel visible-light responding photocatalyst Li3Ni2NbO6 | |
| CN103495411A (en) | Visible-light response photocatalyst Sr2Bi3V3O14 and preparation method thereof | |
| CN103521213A (en) | Photocatalyst LiLaV2O7 with visible-light response and preparation method thereof | |
| CN103111281A (en) | Visible-light response vanadium composite oxide photocatalyst M3(VO4)2 and preparation method thereof | |
| CN106622257A (en) | Silicate base photocatalyst and preparation method thereof | |
| CN109772293B (en) | Antimony bismuth indium oxide photocatalytic material and preparation and application thereof | |
| CN104190400A (en) | Visible light responding photocatalyst Ca3La4V2O14 and preparation method thereof | |
| CN104190404B (en) | Visible light-responded photochemical catalyst SmNbMo2O10And preparation method thereof | |
| CN105562039A (en) | Titanium tellurate photocatalyst and preparing method and application thereof | |
| CN104549298B (en) | A kind of preparation method of titanate catalysis material | |
| CN104591267B (en) | The stannic acid neodymium nanometer ball composite oxide material of the single-phase pyrochlore constitution of a kind of multifunctional type | |
| CN103433045A (en) | Visible-light-responsive photocatalyst Sr2CuO3 and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170728 |