CN107308960A - A kind of niobic acid tellurium catalysis material and its preparation method and application - Google Patents
A kind of niobic acid tellurium catalysis material and its preparation method and application Download PDFInfo
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- CN107308960A CN107308960A CN201710598951.7A CN201710598951A CN107308960A CN 107308960 A CN107308960 A CN 107308960A CN 201710598951 A CN201710598951 A CN 201710598951A CN 107308960 A CN107308960 A CN 107308960A
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- tellurium
- niobium
- catalysis material
- acid
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- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 39
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 30
- 239000002253 acid Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006555 catalytic reaction Methods 0.000 title claims description 27
- 239000000126 substance Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000000975 co-precipitation Methods 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims description 57
- 239000002994 raw material Substances 0.000 claims description 25
- 239000010955 niobium Substances 0.000 claims description 22
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 19
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- SWLJJEFSPJCUBD-UHFFFAOYSA-N tellurium tetrachloride Chemical compound Cl[Te](Cl)(Cl)Cl SWLJJEFSPJCUBD-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 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 12
- 229910052758 niobium Inorganic materials 0.000 claims description 10
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims description 10
- -1 tellurium ion Chemical class 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 229910003069 TeO2 Inorganic materials 0.000 claims description 8
- 239000008139 complexing agent Substances 0.000 claims description 8
- 239000007788 liquid Substances 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
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 6
- 238000009938 salting Methods 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910019804 NbCl5 Inorganic materials 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 150000002821 niobium Chemical class 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 22
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract 1
- 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 29
- 229960000907 methylthioninium chloride Drugs 0.000 description 29
- 230000015556 catabolic process Effects 0.000 description 22
- 238000006731 degradation reaction Methods 0.000 description 22
- 238000001228 spectrum Methods 0.000 description 10
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000536 complexating effect Effects 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 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
- 241000196324 Embryophyta Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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
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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0576—Tellurium; Compounds thereof
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
Abstract
The invention discloses a kind of niobic acid tellurium TeNb4O12The preparation method and application of photochemical catalyst, belongs to inorganic field of photocatalytic material.The present invention is prepared using sol-gal process and coprecipitation, preparation method is simple and easy to apply, and the material granule degree prepared is evenly distributed, chemical stability is good, has preferable light absorpting ability in ultraviolet region, can effectively degradable organic pollutant, have a good application prospect.
Description
Technical field
It is more particularly to organic for degrading the present invention relates to a kind of preparation method and applications of inorganic photocatalyst material
The photochemical catalyst TeNb of pollutant4O12And preparation method thereof.
Background technology
The huge advance of human civilization brings the fast development of industry, and many cities all turn into the heat of commercial development
Soil, large-size chemical factory and high pollution enterprise gradually increase, and are also brought while economy is rapidly developed inevitably
Environmental pollution and problem of energy crisis, they have become a major challenge that the whole mankind needs to face jointly.
Photocatalysis technology is with the chemical conversion of solar energy and is stored as core, converts solar energy into the photocatalytic water of Hydrogen Energy
Technology and photocatalytic degradation eliminate toxic organic pollutant technology and progressively moved to maturity, they will for solve environmental problem and
Energy crisis provides a kind of preferable method.
1972, Honda and Fujishima find on monocrystalline TiO2 electrodes can photochemical catalyzing, started and partly led
The New Times of body Heterogeneous photocatalysis, in the past few decades in, photocatalysis is obtained for extensively in theoretical and engineering practice
Development.
Photocatalysis degradation organic contaminant is to utilize band structure special in semiconductor, i.e., deposited between valence band and conduction band
In a forbidden band.
When photon energy is the light irradiation semiconductor of semiconductor absorber threshold value higher than energy gap, the valence band electricity of semiconductor
Son transits to conduction band from valence band, so as to produce light induced electron (e-) and hole (h+).
The dissolved oxygen capture now adsorbed in catalyst particle surface electronically forms superoxide anion, and hole will be adsorbed
Hydroxide ion and water oxygen the chemical conversion hydroxyl free radical of catalyst surface.
And superoxide anion and hydroxyl free radical have very strong oxidisability, most of oxidation operation can be formed
CO2 and H2O.
The top of valence band of one preferable photochemical catalyst（VBT）More just, the oxidability in hole is stronger, conduction band bottom（CBB）More
Negative, the reducing power of electronics is stronger.
Photochemical catalyst with this characteristic has wider band gap, has preferable light absorpting ability in ultraviolet region, from
And improve degradation efficiency of the photochemical catalyst in ultraviolet region.
In the application, we report a kind of for the photochemical catalyst TeNb4O12 of degradable organic pollutant and its preparation side
Method, such a photochemical catalyst are there is not yet the report of related fields, this patent result shows, the compound has good in ultraviolet region
Good light absorpting ability, has a extensive future.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention is provided, a kind of preparation method is simple, photocatalytic activity is good, should
With niobic acid tellurium photochemical catalyst having a extensive future and preparation method thereof.
A kind of niobic acid tellurium catalysis material, its chemical formula is TeNb4O12；
The preparation method of described niobic acid tellurium catalysis material, prepares powder using sol-gal process, comprises the following steps：
（1）By the stoichiometric proportion of each element in chemical formula TeNb4O12, the compound containing tellurium ion Te4+ is weighed respectively, will
The dissolution of raw material weighed is in hydrofluoric acid or nitric acid, then weighs the compound containing niobium ion Nb5+, by the dissolution of raw material weighed
Complexing agent is added respectively in nitric acid or absolute ethyl alcohol, then by 0.5~2.0wt% of reactant quality in each raw material, obtains uniform
Mixed liquor, described complexing agent is one kind in citric acid, oxalic acid；
（2）The mixed liquor of each raw material is slowly mixed together, stirred 1~2 hour under conditions of temperature is 50~100 DEG C, stands, dry
Fluffy presoma is obtained after dry；
（3）Presoma is calcined in air atmosphere, calcining heat is 200~500 DEG C, calcination time is after 2~12 hours, certainly
So cooling；
（4）By step（3）Obtained mixture takes out, after grinding is uniform, is calcined in air atmosphere, and calcining heat is 500~
900 DEG C, calcination time is 5~16 hours, and it is to obtain a kind of niobic acid tellurium catalysis material powder to be ground after natural cooling uniform.
The described compound containing niobium ion Nb5+ is niobium pentaoxide Nb2O5, niobium hydroxide Nb (OH) 5 and niobium chloride
One kind in NbCl5, the compound containing tellurium ion Te4+ is tellurium dioxide TeO2 and telluric chloride TeCl4.
Step（3）Described calcining heat is 300~500 DEG C, and calcination time is 3~10 hours.
Step（4）Described calcining heat is 500~850 DEG C, and calcination time is 5~12 hours.
A kind of preparation method of niobic acid tellurium catalysis material as claimed in claim 1, is prepared using coprecipitation
Powder, comprises the following steps：
（1）The raw material of the element containing niobium is weighed by the stoichiometric proportion of corresponding element in formula TeNb4O12, hydrofluoric acid is dissolved in
Or in nitric acid, obtain soluble niobium salting liquid；
（2）Weigh the raw material containing tellurium element by the stoichiometric proportion of corresponding element in formula TeNb4O12, be dissolved in nitric acid or
In absolute ethyl alcohol, soluble tellurium salting liquid is obtained；
（3）Niobium salt and tellurium salting liquid are mixed, after stirring, the ammonia spirit that volume fraction is 20% is slowly added dropwise, regulation pH=
8-9, obtains sediment, after centrifugation, washing, drying, obtains presoma；
（4）Presoma is put into Muffle furnace and calcined, calcining heat is 550~950 DEG C, calcination time is 5~18 hours, natural
After cooling, grinding is uniform to obtain a kind of niobic acid tellurium catalysis material powder.
The compound of the described element containing niobium is niobium pentaoxide Nb2O5, niobium hydroxide Nb (OH) 5 and niobium chloride NbCl5
In one kind, the compound containing tellurium element be tellurium dioxide TeO2 and telluric chloride TeCl4 in one kind.
Step（4）Described calcining heat is preferably 550~900 DEG C, and calcination time is preferably 6~17 hours.
Application of the above-mentioned niobic acid tellurium catalysis material on inorganic catalysis material, has good light in ultraviolet region
Absorbability, has a extensive future.
Compared with prior art, technical solution of the present invention advantage is：
（1）The TeNb of preparation4O12Photochemical catalyst thing is mutually pure, and particle is tiny and is evenly distributed, and photocatalytic activity is good, 120 minutes light
The degradation rate of catalytic degradation methylene blue can reach 86%, being capable of efficiently photocatalytic degradation methylene blue.
（2）The TeNb of preparation4O12The raw material sources of photochemical catalyst are extensively, cheap, and preparation method is simple, energy consumption
Low, cost is low.
（3）The present invention is easy to industrialized production, no waste gas and waste liquid discharge, environmentally friendly, TeNb4O12Photochemical catalyst is one
Plant the inorganic catalysis material of green safety.
Brief description of the drawings
Fig. 1 is the TeNb obtained by the embodiment of the present invention 14O12The X-ray powder diffraction pattern of sample；
Fig. 2 is the TeNb obtained by the embodiment of the present invention 14O12The SEM figures of sample；
Fig. 3 is the TeNb obtained by the embodiment of the present invention 14O12The UV-visible absorption spectrum of sample；
Fig. 4 is the TeNb obtained by the embodiment of the present invention 14O12Degraded of the sample in illumination to organic dyestuff methylene blue is bent
Line；
Fig. 5 is the TeNb obtained by the embodiment of the present invention 14O12The dynamic curve diagram of sample degradation methylene blue；
Fig. 6 is the TeNb obtained by the embodiment of the present invention 54O12The X-ray powder diffraction pattern of sample；
Fig. 7 is the TeNb obtained by the embodiment of the present invention 54O12The SEM figures of sample；
Fig. 8 is the TeNb obtained by the embodiment of the present invention 54O12The UV-visible absorption spectrum of sample；
Fig. 9 is the TeNb obtained by the embodiment of the present invention 54O12Degraded of the sample in illumination to organic dyestuff methylene blue is bent
Line；
Figure 10 is the TeNb obtained by the embodiment of the present invention 54O12The dynamic curve diagram of sample degradation methylene blue.
Embodiment
In order to obtain the niobic acid tellurium photochemical catalyst used in the present invention, powder is prepared using sol-gal process and coprecipitation
End, preparation method is simple and easy to apply.
2nd, even received preferably in micron level in order to effective size for utilizing the photochemical catalyst in light, the present invention
Rice corpuscles, and specific surface area is larger.
The photocatalyst particles diameter prepared by sol-gal process and coprecipitation is small and even particle size distribution.
3rd, photocatalytic degradation methylene blue activity rating is using self-control photocatalytic reaction device, and illuminator is 500 watts of cylinders
Shape shape xenon lamp, the cylindrical light catalytic reaction instrument that reactive tank is made using pyrex, reactive tank is inserted into by illuminator
In, and condensed water cooling is passed through, temperature is room temperature during reaction.
100 milligrams of catalyst amount, 250 milliliters of liquor capacity, the concentration of methylene blue is 10 mg/litres.
Catalyst is placed in reaction solution, and catalysis time is set as 240 minutes, starts illumination after opening condensed water, after illumination
A sample is taken at regular intervals, is centrifuged, its supernatant is taken, with ultraviolet-visible spectrophotometer in wavelength 664-666 nanometers
Determine the absorbance of methylene blue solution.
According to Lambert-Beer's law, the absorbance of solution is directly proportional to concentration, therefore available absorbance is calculated instead of concentration
Clearance, 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 drop
Concentration before and after solution, A0, A respectively be degraded before and after absorbance.
Embodiment 1：
According to chemical formula TeNb4O12, niobium pentaoxide Nb is weighed respectively2O5：2.658 grams, tellurium dioxide TeO2：0.798 gram, will
Niobium pentaoxide is dissolved in hydrofluoric acid, and tellurium dioxide is dissolved in nitric acid, is added appropriate citric acid as complexing agent, is stirred
Mix the mixed liquor that complexing obtains each raw material；The mixed liquor of each raw material is slowly mixed together, stirred under conditions of temperature is 50~100 DEG C
Mix 1~2 hour, fluffy presoma is obtained after standing, drying；Presoma is calcined in air atmosphere, calcining heat is 300
DEG C, calcination time is 3 hours, is subsequently cooled to room temperature, takes out sample；Raw material after first time is calcined is sufficiently mixed again to be ground
Mill is uniform, and second is carried out in air atmosphere and is calcined, 500 DEG C of calcining heat, calcination time is 10 hours, is then cooled to room
Temperature；After natural cooling, sample is ground and is well mixed again, calcined in air atmosphere, calcining heat is 850 DEG C, calcining
Time is 12 hours, and grinding obtains TeNb after cooling4O12Photochemical catalyst.
Referring to accompanying drawing 1, it is the X-ray powder diffraction pattern of the sample as prepared by the present embodiment technical scheme, XRD tests
As a result show, prepared TeNb4O12Also it is monophase materialses, crystallinity is good；
Referring to accompanying drawing 2, it is the UV-Vis DRS spectrogram of the sample as prepared by the present embodiment technical scheme, from figure
As can be seen that the sample has good light absorpting ability in ultraviolet region；
Referring to accompanying drawing 3, it is the SEM of the sample as prepared by the present embodiment technical scheme（SEM）Collection of illustrative plates, from figure
In as can be seen that gained sample particle be uniformly dispersed, granularity is smaller；
Referring to accompanying drawing 4, it is degradation curve of the sample to organic dyestuff methylene blue as prepared by the present embodiment technical scheme.
It can be seen that the degradation rate of the sample photocatalytic degradation methylene blue can reach 80% in 120 minutes, say
The bright TeNb prepared4O12Material has preferable photocatalytic activity；
Referring to accompanying drawing 5, it is the dynamic curve diagram of the sample degradation methylene blue as prepared by the present embodiment technical scheme, from figure
In as can be seen that the sample photocatalytic degradation methylene blue apparent kinetics speed constant be 0.01275 minute-1。
Embodiment 2：
According to chemical formula TeNb4O12, niobium pentaoxide Nb is weighed respectively2O5：2.658 grams, telluric chloride TeCl4:1.347 gram, will
Niobium pentaoxide is dissolved in hydrofluoric acid, and telluric chloride is dissolved in absolute ethyl alcohol, adds appropriate citric acid as complexing
Agent, stirring complexing obtains the mixed liquor of each raw material；The mixed liquor of each raw material is slowly mixed together, in the bar that temperature is 50~100 DEG C
Stirred 1~2 hour under part, fluffy presoma is obtained after standing, drying；Presoma is calcined in air atmosphere, calcining temperature
Spend for 350 DEG C, calcination time is 3 hours, be subsequently cooled to room temperature, take out sample；Raw material after first time is calcined fills again
Divide mixed grinding uniform, second is carried out in air atmosphere and is calcined, 400 DEG C of calcining heat, calcination time is 4 hours, then
It is cooled to room temperature；After natural cooling, sample is ground and is well mixed again, calcined in air atmosphere, calcining heat is 500
DEG C, calcination time is 5 hours, and grinding obtains TeNb after cooling4O12Photochemical catalyst.
Its main structure and morphology, UV-Vis DRS spectrum, SEM spectrum, the degradation rate to methylene blue and degraded
The kinetic curve of methylene blue is similar to Example 1.
Embodiment 3：
According to chemical formula TeNb4O12, niobium hydroxide Nb (OH) is weighed respectively5：3.558 grams, telluric chloride TeCl4：1.347 gram,
Niobium hydroxide is dissolved in hydrofluoric acid, telluric chloride is dissolved in absolute ethyl alcohol, adds appropriate citric acid as complexing
Agent, stirring complexing obtains the mixed liquor of each raw material；The mixed liquor of each raw material is slowly mixed together, in the bar that temperature is 50~100 DEG C
Stirred 1~2 hour under part, fluffy presoma is obtained after standing, drying；Presoma is calcined in air atmosphere, calcining temperature
Spend for 350 DEG C, calcination time is 5 hours, be subsequently cooled to room temperature, take out sample；Raw material after first time is calcined fills again
Divide mixed grinding uniform, second is carried out in air atmosphere and is calcined, 450 DEG C of calcining heat, calcination time is 8 hours, then
It is cooled to room temperature；After natural cooling, sample is ground and is well mixed again, calcined in air atmosphere, calcining heat is 650
DEG C, calcination time is 10 hours, and grinding obtains TeNb after cooling4O12Photochemical catalyst.
Its main structure and morphology, UV-Vis DRS spectrum, SEM spectrum, the degradation rate to methylene blue and degraded
The kinetic curve of methylene blue is similar to Example 1.
Embodiment 4：
According to chemical formula TeNb4O12, columbium pentachloride NbCl is weighed respectively5：3.602 grams, tellurium dioxide TeO2：0.898 gram, by five
Niobium chloride is dissolved in nitric acid, and tellurium dioxide is dissolved in nitric acid, adds appropriate citric acid as complexing agent, stirring complexing
Obtain the mixed liquor of each raw material；The mixed liquor of each raw material is slowly mixed together, 1~2 is stirred under conditions of temperature is 50~100 DEG C
Hour, obtain fluffy presoma after standing, drying；Presoma is calcined in air atmosphere, calcining heat is 300 DEG C, is forged
The burning time is 6 hours, is subsequently cooled to room temperature, takes out sample；It is equal that raw material after first time is calcined is sufficiently mixed grinding again
It is even, second of calcining is carried out in air atmosphere, 500 DEG C of calcining heat, calcination time is 8 hours, is then cooled to room temperature；It is natural
After cooling, sample is ground and is well mixed again, calcined in air atmosphere, calcining heat is 750 DEG C, and calcination time is 11
Hour, grinding obtains TeNb after cooling4O12Photochemical catalyst.
Its main structure and morphology, UV-Vis DRS spectrum, SEM spectrum, degradation rate and degraded to methylene blue
The kinetic curve of methylene blue is similar to Example 1.
Embodiment 5：
According to chemical formula TeNb4O12, niobium pentaoxide Nb is weighed respectively2O5：3.544 grams, tellurium dioxide TeO2：1.064 gram, will
Niobium pentaoxide is dissolved in hydrofluoric acid, and tellurium dioxide is dissolved in nitric acid, mixes two kinds of solution, after stirring, slow drop
Plus the ammonia spirit that volume fraction is 20%, adjust pH=8, obtain sediment, centrifugation, washing, dry after, obtain presoma；Will
Presoma is put into Muffle furnace and calcined, and calcining heat is 550 DEG C, and calcination time is 16 hours, after natural cooling, and grinding is uniform i.e.
Obtain a kind of niobic acid tellurium catalysis material powder.
Referring to accompanying drawing 6, it is the X-ray powder diffraction pattern of the sample as prepared by the present embodiment technical scheme, XRD tests
As a result show, prepared photochemical catalyst niobic acid tellurium TeNb4O12For monophase materialses, and crystallinity is preferable；
Referring to accompanying drawing 7, it is the SEM of the sample as prepared by the present embodiment technical scheme（SEM）Collection of illustrative plates, from figure
In as can be seen that gained powder particle disperse more uniform；
Referring to accompanying drawing 8, it is the UV-Vis DRS spectrum of the sample as prepared by the present embodiment technical scheme, can from figure
To find out, the sample has good light absorpting ability in ultraviolet region；
Referring to accompanying drawing 9, it is that sample is sub- to organic dyestuff under different light application times as prepared by the present embodiment technical scheme
The degradation curve of methyl blue.
It can be seen that the degradation rate of the sample photocatalytic degradation methylene blue reaches 86% in 120 minutes, illustrate system
For the niobic acid tellurium TeNb gone out4O12Material has excellent photocatalytic activity.
Referring to accompanying drawing 10, it is the kinetic curve of the sample degradation methylene blue as prepared by the present embodiment technical scheme
Figure, it can be seen that the apparent kinetics speed constant of the sample photocatalytic degradation methylene blue is 0.02081 minute-1。
Embodiment 6：
According to chemical formula TeNb4O12, niobium pentaoxide Nb is weighed respectively2O5：3.544 grams, telluric chloride TeCl4：1.796 gram, will
Niobium pentaoxide is dissolved in hydrofluoric acid, and telluric chloride is dissolved in absolute ethyl alcohol, mixes two kinds of solution, after stirring, and is delayed
It is slow that the ammonia spirit that volume fraction is 20% is added dropwise, adjust pH=9, obtain sediment, centrifugation, washing, dry after, obtain forerunner
Body；Presoma is put into Muffle furnace and calcined, calcining heat is 900 DEG C, and calcination time is 7 hours, after natural cooling, and grinding is equal
It is even to obtain a kind of niobic acid tellurium catalysis material powder.
Its main structure and morphology, UV-Vis DRS spectrum, degradation rate and degradation of methylene blue to methylene blue
Kinetic curve it is similar to Example 5.
Embodiment 7：
According to chemical formula TeNb4O12, niobium hydroxide Nb (OH) is weighed respectively5：4.744 grams, tellurium dioxide TeO2：1.064 gram, will
Niobium hydroxide is dissolved in hydrofluoric acid, and tellurium dioxide is dissolved in nitric acid, is mixed two kinds of solution, after stirring, is slowly added dropwise
Volume fraction is 20% ammonia spirit, adjusts pH=9, obtains sediment, centrifugation, washing, dry after, obtain presoma；By before
Drive body and be put into calcining in Muffle furnace, calcining heat is 700 DEG C, and calcination time is 10 hours, after natural cooling, and grinding is uniformly produced
To a kind of niobic acid tellurium catalysis material powder.
Its main structure and morphology, UV-Vis DRS spectrum, degradation rate and degradation of methylene blue to methylene blue
Kinetic curve it is similar to Example 5.
Embodiment 8：
According to chemical formula TeNb4O12, columbium pentachloride NbCl is weighed respectively5：4.323 grams, telluric chloride TeCl4：1.078 gram, will
Columbium pentachloride is dissolved in nitric acid, and tellurium dioxide is dissolved in nitric acid, mixes two kinds of solution, after stirring, body is slowly added dropwise
Fraction is 20% ammonia spirit, adjusts pH=8, obtains sediment, centrifugation, washing, dry after, obtain presoma；By forerunner
Body is put into Muffle furnace and calcined, and calcining heat is 600 DEG C, and calcination time is 12 hours, after natural cooling, and grinding is uniform to be obtained
A kind of niobic acid tellurium catalysis material powder.
Its main structure and morphology, UV-Vis DRS spectrum, degradation rate and degradation of methylene blue to methylene blue
Kinetic curve it is similar to Example 5.
Claims (8)
1. a kind of niobic acid tellurium catalysis material, it is characterised in that：Its chemical formula is TeNb4O12。
2. a kind of preparation method of niobic acid tellurium catalysis material as claimed in claim 1, is prepared using sol-gal process
Powder, it is characterised in that comprise the following steps：
（1）By chemical formula TeNb4O12The stoichiometric proportion of middle each element, is weighed containing tellurium ion Te respectively4+Compound, will claim
The dissolution of raw material taken is in hydrofluoric acid or nitric acid, then weighs containing niobium ion Nb5+Compound, by the dissolution of raw material weighed in nitre
In acid or absolute ethyl alcohol, then by 0.5~2.0wt% of reactant quality in each raw material complexing agent is added respectively, uniformly mixed
Liquid is closed, described complexing agent is one kind in citric acid, oxalic acid；
（2）The mixed liquor of each raw material is slowly mixed together, stirred 1~2 hour under conditions of temperature is 50~100 DEG C, stands, dry
Fluffy presoma is obtained after dry；
（3）Presoma is calcined in air atmosphere, calcining heat is 200~500 DEG C, calcination time is after 2~12 hours, certainly
So cooling；
（4）By step（3）Obtained mixture takes out, after grinding is uniform, is calcined in air atmosphere, and calcining heat is 500~
900 DEG C, calcination time is 5~16 hours, and it is to obtain a kind of niobic acid tellurium catalysis material powder to be ground after natural cooling uniform.
3. a kind of preparation method of niobic acid tellurium catalysis material according to claim 2, it is characterised in that：Described contains
Niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one kind, it is described
Contain tellurium ion Te4+Compound be tellurium dioxide TeO2With telluric chloride TeCl4。
4. a kind of preparation method of niobic acid tellurium catalysis material according to claim 2, it is characterised in that：Step（3）Institute
The calcining heat stated is 300~500 DEG C, and calcination time is 3~10 hours, step（4）Described calcining heat is 500~850
DEG C, calcination time is 5~12 hours.
5. a kind of preparation method of niobic acid tellurium catalysis material as claimed in claim 1, it is characterised in that use coprecipitation
Powder is prepared, is comprised the following steps：
（1）By formula TeNb4O12The stoichiometric proportion of middle corresponding element weighs the raw material of the element containing niobium, be dissolved in hydrofluoric acid or
In nitric acid, soluble niobium salting liquid is obtained；
（2）By formula TeNb4O12The stoichiometric proportion of middle corresponding element weighs the raw material containing tellurium element, is dissolved in nitric acid or nothing
In water-ethanol, soluble tellurium salting liquid is obtained；
（3）Niobium salt and tellurium salting liquid are mixed, after stirring, the ammonia spirit that volume fraction is 20% is slowly added dropwise, regulation pH=
8-9, obtains sediment, after centrifugation, washing, drying, obtains presoma；
（4）Presoma is put into Muffle furnace and calcined, calcining heat is 550~950 DEG C, calcination time is 5~18 hours, natural
After cooling, grinding is uniform to obtain a kind of niobic acid tellurium catalysis material powder.
6. a kind of preparation method of niobic acid tellurium catalysis material according to claim 5, it is characterised in that：Described contains niobium
The compound of element is niobium pentaoxide Nb2O5, niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one kind, described contains
The compound of tellurium element is tellurium dioxide TeO2With telluric chloride TeCl4In one kind.
7. a kind of preparation method of new niobic acid tellurium catalysis material according to claim 5, it is characterised in that：Step
（4）Described calcining heat is preferably 550~900 DEG C, and calcination time is preferably 6~17 hours.
8. application of a kind of niobic acid tellurium catalysis material as claimed in claim 1 on inorganic catalysis material, in ultraviolet light
Area has good light absorpting ability.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109772293A (en) * | 2019-03-27 | 2019-05-21 | 江苏师范大学 | A kind of indium acid antimony bismuth catalysis material and its preparation and application |
| WO2021107868A1 (en) * | 2019-11-28 | 2021-06-03 | National University Of Singapore | A multiferroic material and a method of preparing the same |
| CN115069248A (en) * | 2022-07-12 | 2022-09-20 | 西南交通大学 | Silver niobate nano material and preparation method and application thereof |
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| 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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109772293A (en) * | 2019-03-27 | 2019-05-21 | 江苏师范大学 | A kind of indium acid antimony bismuth catalysis material and its preparation and application |
| WO2021107868A1 (en) * | 2019-11-28 | 2021-06-03 | National University Of Singapore | A multiferroic material and a method of preparing the same |
| CN115069248A (en) * | 2022-07-12 | 2022-09-20 | 西南交通大学 | Silver niobate nano material and preparation method and application thereof |
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