CN108745390A - A kind of visible-light photocatalyst and its preparation and application - Google Patents
A kind of visible-light photocatalyst and its preparation and application Download PDFInfo
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- CN108745390A CN108745390A CN201810581586.3A CN201810581586A CN108745390A CN 108745390 A CN108745390 A CN 108745390A CN 201810581586 A CN201810581586 A CN 201810581586A CN 108745390 A CN108745390 A CN 108745390A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000008139 complexing agent Substances 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 31
- 150000001875 compounds Chemical class 0.000 claims description 17
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 15
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 230000015556 catabolic process Effects 0.000 claims description 10
- 238000006731 degradation reaction Methods 0.000 claims description 10
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 8
- -1 phosphonium ion Chemical class 0.000 claims description 8
- 239000000428 dust Substances 0.000 claims description 7
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 7
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 claims description 6
- 229910001456 vanadium ion Inorganic materials 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910017677 NH4H2 Inorganic materials 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 5
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 14
- 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 10
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 10
- 150000002500 ions Chemical class 0.000 description 10
- 229960000907 methylthioninium chloride Drugs 0.000 description 10
- 238000000634 powder X-ray diffraction Methods 0.000 description 8
- 239000000975 dye Substances 0.000 description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- 238000000643 oven drying Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- 235000005979 Citrus limon Nutrition 0.000 description 3
- 244000131522 Citrus pyriformis Species 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000000985 reflectance spectrum Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 241001062009 Indigofera Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000005056 cell body Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- 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
-
- 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
- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
It is prepared the present invention relates to a kind of visible-light photocatalyst and its application, the chemical formula of feature is：AlV6+xP1‑xO19(0.01<x<0.65), belong to inorganic field of photocatalytic material.Photochemical catalyst of the present invention is chemical solution method using preparation method, and the raw material of the whole ratio of chemistry is prepared into transparent solution, polymeric complexing agent is added so that the Al among raw material3+Ion, V5+Ion and P3+Ion is fully complexed, and drying is prepared into presoma xerogel, high-temperature calcination, and organic components volatilization obtains the AlV of pure object phase6+xP1‑xO19(0.01<x<0.65)；Material prepared by the present invention can absorb the ultraviolet light to 580nm；There is photocatalytic effect under the irradiation of visible light；And operation is simple for preparation process, sintering temperature is low, does not need complicated sintering atmosphere, obtained uniform granularity, chemical stability are good.
Description
Technical field
The invention belongs to inorganic field of photocatalytic material, it is related to the photocatalysis for degradating organic dye and other pollutants
Agent, more particularly to a kind of visible-light photocatalyst and its preparation and application.
Background technology
With the development of industry and society, worldwide environmental pollution is increasingly severe, becomes among social development
One of focal issue of strong interest.For example, since industrial wastewater and people's lives sewage add the continuous of environmental pollution
Play causes serious ecological environment destruction, and the existence of the whole mankind is constituted and is seriously threatened.It is dirty in order to solve many environment
Dye problem, people are being dedicated to always controlling and curbing environmental pollution by various methods.Wherein, it is dropped using light-catalyzed reaction
Pollutant is solved, is a kind of one of means of green, has obtained more and more attention.
So-called light-catalyzed reaction is exactly photochemical catalyst under the irradiation of light, its own does not change, and can but promote chemistry
The substance of reaction can utilize luminous energy existing for nature to be converted into the energy needed for chemical reaction, to generate catalytic action,
The oxygen of surrounding and hydrone is set to be excited into the free anion of great oxidizing force.Almost separable solution is all human body and environment
Harmful organic substance and part inorganic substances, can not only accelerate to react, and can also use nature determines Lu, does not result in waste of resources
It is formed with additional pollution.Classical photochemical catalyst such as TiO2It needs to realize light-catalyzed reaction under ultraviolet light, still
The ratio that ultraviolet light accounts in sunlight is about 5 percent less than the visible light model that most solar energy is concentrated mainly on
Enclose (400-700 nanometers), therefore, TiO2In visible-range and do not have catalytic activity, while therefore current photocatalysis skill
Art cannot still make full use of sunlight.So researcher is widened by doping, the means such as compound, its is visible light-responded, or transfers
Find other novel photocatalysis materials.But the TiO of these modifications2Material still has among preparing complicated, application process not
Stablize, the excessively high different disadvantage of cost.
Invention content
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of visible-light photocatalyst and its
It prepares and applies, which is a kind of vanadium aluminate, is based on AlV6PO19Matrix, by the V for realizing part among lattice5+It takes
For P5+Element realizes the photochemical catalyst AlV that auto-dope obtains6+xP1-xO19, which is oneself realized among the same lattice
Doping prepares and uses chemical solution synthetic method, and as mild as a dove, calcination temperature is very low for preparation condition, simple process and low cost
Honest and clean, experimental technique is with good stability and repeatable, stably-doped, efficient, substantially increases in visible region
Between efficiency of light absorption, realize preferable photocatalysis efficiency.Research finds that such compound has good photocatalysis performance.
To achieve the goals above, the technical solution adopted by the present invention is：
A kind of visible-light photocatalyst, chemical general formula are：AlV6+xP1-xO19, x is V in lattice5+Auto-dope replaces P5+Member
Molar ratio 0.01≤x≤0.65 of element.
The present invention also provides the preparation methods of the visible-light photocatalyst, include the following steps：
(1) chemical general formula AlV is pressed6+xP1-xO19The stoichiometric ratio of middle each element is weighed respectively containing aluminium ion Al3+'s
Compound contains vanadium ion V5+Compound and contain phosphonium ion P5+Compound, they are dissolved completely in dust technology respectively
In, and appropriate amount of deionized water dilution is added；
(2) complexing agent is added respectively in step (1) each raw material, under magnetic stirring to being completely dissolved, obtain completely molten
The solution of each raw material of solution；
(3) solution for each raw material that step (2) obtains is slowly mixed together, stirs to being mixed thoroughly, stands, dries,
Obtain fluffy presoma；
(4) step (3) presoma is placed in Muffle furnace, is sintered in air atmosphere, after natural cooling, ground and mix
Uniformly to get powdered visible-light photocatalyst.
In the step (1), contain aluminium ion Al3+Compound can be Al (NO3)3·9H2O or Al (OH)3Deng containing
There is vanadium ion V5+Compound can be NH4VO3Deng containing phosphonium ion P5+Compound can be NH4H2PO4Or P2O5Deng.
In the step (2), complexing agent can be citric acid or oxalic acid, and the additive amount of each raw material complexing agent is in raw material
The 10-20wt% of reactive material.Reactive material herein " is referred to containing aluminium ion Al3+Compound, contain vanadium ion V5+
Compound and contain phosphonium ion P5+Compound
In the step (3), it can be stirred under conditions of temperature is 70~90 DEG C after mixing.
In the step (4), sintering temperature is preferably 500~650 DEG C, and sintering time is 3~10 hours,
The degradation to dye solution can be achieved in visible-light photocatalyst of the present invention under the irradiation of visible light.
Compared with prior art, the beneficial effects of the invention are as follows：
1、AlV6+xP1-xO19(0.01<x<0.65) chemical composition can be adjusted by changing the amount of V, obtained light
Catalyst has good visible light light absorption.
2, preparation method is simple, and as mild as a dove, calcination temperature is very low for preparation condition.
3 and the irradiation of visible light under, photochemical catalyst can efficient catalytic degradation methylene blue, there is good light to urge
Change activity.
Description of the drawings
Attached drawing 1：1 technical solution of the embodiment of the present invention prepares the X-ray powder diffraction figure of sample.
Attached drawing 2：The electron microscope picture of sample prepared by the embodiment of the present invention.
Attached drawing 3：The uv-visible absorption spectroscopy figure of sample prepared by the embodiment of the present invention 1.
Attached drawing 4：Sample prepared by the embodiment of the present invention 1 is under different light application times to the drop of organic dyestuff methylene blue
Solution.
Attached drawing 5：4 technical solution of the embodiment of the present invention prepares the X-ray powder diffraction figure of sample.
Attached drawing 6：The ultraviolet-visible diffuse reflectance spectrum figure of sample prepared by the embodiment of the present invention 4.
Attached drawing 7：Sample prepared by the embodiment of the present invention 4 is under different light application times to the drop of organic dyestuff methylene blue
Solution.
Specific implementation mode
The embodiment that the present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment 1
According to chemical formula AlV6.2P0.8O19Middle Al3+Ion, V5+And P5+Stoichiometric ratio, weigh aluminium hydroxide Al respectively
(OH)3：0.78 gram, ammonium metavanadate NH4VO3：7.254 grams, ammonium di-hydrogen phosphate NH4H2PO4：0.92 gram, three kinds of reagents are dissolved in respectively
In dust technology；Contain Al above-mentioned3+Ion, V5+And P5+0.16 gram, 1.45 grams and 0.18 gram of citric acid is added in solution respectively
It is complexed；Three of the above solution is mixed, is stirred at 90 DEG C to being mixed thoroughly, stands, be put into baking oven drying, obtain
Fluffy presoma；Presoma is taken out, is calcined in air atmosphere, calcination temperature is 650 DEG C, and calcination time is 3 hours, is taken out
Afterwards and it is fully ground and obtains AlV6.2P0.8O19Photocatalyst powder.
Referring to attached drawing 1, it is the X-ray powder diffraction figure that sample is prepared by 1 technical solution of the present embodiment, is shown prepared
Sample be monophase materials, without other dephasigns.
Referring to attached drawing 2, it is the electron microscope picture by sample prepared by the present embodiment, it can be seen that grain size number is thin
Small highly uniform, particle is loose, it is easy to scatter in mortar or water；
Referring to attached drawing 3, it be by the ultraviolet-visible diffuse reflectance spectrum figure of sample prepared by the present embodiment 1, can be with from figure
Find out, which can absorb ultraviolet-visible light.
Referring to attached drawing 4, it be sample prepared by the present embodiment 1 under different visible light application times to organic dyestuff methylene
The degradation curve of base indigo plant.As can be seen that the sample has visible light catalysis activity.
Embodiment 2
According to chemical formula AlV6.1P0.9O19Middle element al3+、V5+And P5+Stoichiometric ratio, weigh aluminum nitrate Al respectively
(NO3)3：3.75 grams, ammonium metavanadate NH4VO3：7.13 grams, phosphorus pentoxide P2O5：1.28 grams, three kinds of reagents are dissolved in dilute nitre respectively
In acid；Contain Al above-mentioned3+Ion, V5+And P5+0.675 gram, 1.28 grams and 0.23 gram of oxalic acid is added in solution respectively to carry out
Complexing；Three of the above solution is mixed, is stirred at 70 DEG C to being mixed thoroughly, stands, be put into baking oven drying, obtain fluffy
Presoma；Presoma is taken out, is calcined in air atmosphere, calcination temperature is 500 DEG C, and calcination time is 10 hours, after taking-up
And it is fully ground and obtains AlV6.1P0.9O19Photocatalyst powder.
The X-ray powder diffraction figure for the photochemical catalyst that embodiment 2 obtains is same as in figure 1, has pure object phase；Its is main
It is microscopic appearance, similar to Example 1 to the degradation of methylene blue.
Embodiment 3
According to chemical formula AlV6.01P0.99O19Middle element al3+、V5+And P5+Stoichiometric ratio, weigh aluminum nitrate Al respectively
(NO3)3：3.75 grams, ammonium metavanadate NH4VO3：7.032 grams, ammonium di-hydrogen phosphate NH4H2PO4：：1.138 grams, three kinds of reagent difference are molten
In dust technology；Contain Al above-mentioned3+Ion, V5+And P5+0.375 gram, 0.7 gram and 0.114 gram of lemon is added in solution respectively
Lemon acid is complexed；Three of the above solution is mixed, is stirred at 80 DEG C to being mixed thoroughly, stands, be put into baking oven drying,
Obtain fluffy presoma；Presoma to be taken out, is calcined in air atmosphere, calcination temperature is 550 DEG C, and calcination time is 8 hours,
After taking-up and it is fully ground and obtains AlV6.01P0.99O19Photocatalyst powder.
The X-ray powder diffraction figure for the photochemical catalyst that embodiment 3 obtains is same as in figure 1, has pure object phase；Its is main
It is microscopic appearance, similar to Example 1 to the degradation of methylene blue.
Embodiment 4
According to chemical formula AlV6.65P0.35O19The stoichiometric ratio of middle element al, V and P weighs aluminum nitrate Al respectively
(NO3)3：3.75 grams, ammonium metavanadate NH4VO3：7.78 grams, ammonium di-hydrogen phosphate NH4H2PO4：0.405 gram, three kinds of reagents are dissolved in respectively
In dust technology；Contain Al above-mentioned3+Ion, V5+And P5+0.75 gram, 1.556 grams and 0.08 gram of lemon is added in solution respectively
Acid is complexed；Three of the above solution is mixed, is stirred at 80 DEG C to being mixed thoroughly, stands, be put into baking oven drying, obtain
To fluffy presoma；Presoma is taken out, is calcined in air atmosphere, calcination temperature is 600 DEG C, and calcination time is 5 hours, is taken
Go out afterwards and be fully ground and obtains AlV6.65P0.35O19Photocatalyst powder.
It is the X-ray powder diffraction figure for preparing sample by 4 technical solution of the present embodiment referring to attached drawing 5, shows prepared
Material is monophase materials, without other dephasigns.
Referring to attached drawing 6, be by the ultraviolet-visible diffuse reflectance spectrum figure of sample prepared by the present embodiment 4, can from figure
Go out, which can absorb ultraviolet to 600 nanometers of visible light.
Referring to attached drawing 7, be sample prepared by the present embodiment 4 under different light application times to the drop of organic dyestuff methylene blue
Solution curve.As can be seen that the sample has visible light catalysis activity.
Embodiment 5
According to chemical formula AlV6.5P0.5O19The stoichiometric ratio of middle element al, V and P weighs aluminum nitrate Al (NO respectively3)3：
3.75 grams, ammonium metavanadate NH4VO3：7.605 grams, ammonium di-hydrogen phosphate NH4H2PO4：0.575 gram, three kinds of reagents are dissolved in dust technology respectively
In；Contain Al above-mentioned3+Ion, V5+And P5+0.56 gram, 1.14 grams and 0.08 gram of citric acid is added in solution respectively and carries out network
It closes；Three of the above solution is mixed, is stirred at 80 DEG C to being mixed thoroughly, stands, be put into baking oven drying, obtain fluffy
Presoma；Presoma is taken out, is calcined in air atmosphere, calcination temperature is 630 DEG C, and calcination time is 4 hours, after taking-up and is filled
Grinding is divided to obtain AlV6.5P0.5O19Photocatalyst powder.
The AlV that embodiment 5 obtains6.5P0.5O19Photochemical catalyst has pure object phase, and X-ray powder diffraction figure is in embodiment 4
As obtaining；Its light absorption and to the degradation rate of methylene blue and the kinetic curve of degradation of methylene blue and 4 phase of embodiment
Seemingly.
Embodiment 6
According to chemical formula AlV6.3P0.3O19The stoichiometric ratio of middle element al, V and P weighs aluminum nitrate Al (NO respectively3)3：
3.75 grams, ammonium metavanadate NH4VO3：7.371 grams, ammonium di-hydrogen phosphate NH4H2PO4：0.081 gram, three kinds of reagents are dissolved in dust technology respectively
In；Contain Al above-mentioned3+Ion, V5+And P5+0.563 gram, 1.105 grams and 0.121 gram of oxalic acid is added in solution respectively to carry out
Complexing；Three of the above solution is mixed, is stirred at 80 DEG C to being mixed thoroughly, stands, be put into baking oven drying, obtain fluffy
Presoma；Presoma is taken out, is calcined in air atmosphere, calcination temperature is 600 DEG C, and calcination time is 6 hours, after taking-up simultaneously
It is fully ground and obtains AlV6.3P0.3O19Photocatalyst powder.
The AlV that embodiment 5 obtains6.3P0.3O19Photochemical catalyst has pure object phase, and X-ray powder diffraction figure is in embodiment 4
As obtaining；Its light absorption and to the degradation rate of methylene blue and the kinetic curve of degradation of methylene blue and 4 phase of embodiment
Seemingly.
To sum up, the present invention is prepared using chemical solution method, and the raw material of the whole ratio of chemistry is prepared into transparent solution, and high score is added
Sub- complexing agent so that the Al among raw material3+Ion, V5+Ion and P3+Ion is fully complexed, and the dry forerunner's soma that is prepared into coagulates
Glue, high-temperature calcination, organic components volatilization obtain the AlV of pure object phase6+xP1-xO19；Resulting materials, which can absorb, ultraviolet arrives 580nm's
Light；There is photocatalytic effect under the irradiation of visible light；And operation is simple for preparation process, sintering temperature is low, need not answer
Miscellaneous sintering atmosphere, obtained uniform granularity, chemical stability are good.
Claims (9)
1. a kind of visible-light photocatalyst, chemical general formula are：AlV6+xP1-xO19, x is V in lattice5+Auto-dope replaces P5+Element
Molar ratio, 0.01≤x≤0.65.
2. visible-light photocatalyst according to claim 1, which is characterized in that its chemical formula is AlV6.2P0.8O19、
AlV6.1P0.9O19、AlV6.01P0.99O19、AlV6.65P0.35O19、AlV6.5P0.5O19Or AlV6.3P0.3O19。
3. the preparation method of visible-light photocatalyst described in claim 1, which is characterized in that include the following steps：
(1) chemical general formula AlV is pressed6+xP1-xO19The stoichiometric ratio of middle each element is weighed respectively containing aluminium ion Al3+Chemical combination
Object contains vanadium ion V5+Compound and contain phosphonium ion P5+Compound, they are dissolved completely in dust technology respectively,
And appropriate amount of deionized water dilution is added；
(2) complexing agent is added respectively in step (1) each raw material, under magnetic stirring to being completely dissolved, be completely dissolved
The solution of each raw material；
(3) solution for each raw material that step (2) obtains is slowly mixed together, stirs to being mixed thoroughly, stands, dries, obtain
Fluffy presoma；
(4) step (3) presoma is placed in Muffle furnace, is sintered in air atmosphere, after natural cooling, ground and mix
It is even to get powdered visible-light photocatalyst.
4. the preparation method of visible-light photocatalyst according to claim 3, which is characterized in that in the step (1), contain
Aluminium ion Al3+Compound be Al (NO3)3·9H2O or Al (OH)3, contain vanadium ion V5+Compound be NH4VO3, contain phosphorus
Ion P5+Compound be NH4H2PO4Or P2O5。
5. the preparation method of visible-light photocatalyst according to claim 3, which is characterized in that in the step (2), each original
Expect that the additive amount of complexing agent is the 10-20wt% of reactive material total amount in raw material, reactive material refers to containing aluminium ion Al3+Change
It closes object, contain vanadium ion V5+Compound and contain phosphonium ion P5+Compound.
6. according to the preparation method of the visible-light photocatalyst of claim 3 or 5, which is characterized in that in the step (2),
Complexing agent is citric acid or oxalic acid.
7. the preparation method of visible-light photocatalyst according to claim 3, which is characterized in that in the step (3), mixing
It is stirred under conditions of temperature is 70~90 DEG C afterwards.
8. the preparation method of visible-light photocatalyst according to claim 3, which is characterized in that in the step (4), sintering
Temperature is 500~650 DEG C, and sintering time is 3~10 hours.
9. visible-light photocatalyst described in claim 1 realizes the application of the degradation to dye solution under the irradiation of visible light.
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