CN109289887A - A kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method and application - Google Patents
A kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method and application Download PDFInfo
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- CN109289887A CN109289887A CN201811049348.4A CN201811049348A CN109289887A CN 109289887 A CN109289887 A CN 109289887A CN 201811049348 A CN201811049348 A CN 201811049348A CN 109289887 A CN109289887 A CN 109289887A
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- titanium dioxide
- dispersion liquid
- tao
- nitrogen
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 156
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 30
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 28
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 36
- 239000006185 dispersion Substances 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 11
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 10
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims abstract description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 19
- 238000010992 reflux Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000006731 degradation reaction Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 230000015556 catabolic process Effects 0.000 claims description 6
- 230000004044 response Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 5
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000011218 binary composite Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000005303 weighing Methods 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
- B01J27/24—Nitrogen compounds
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
A kind of nitrogen of the invention, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method, comprising the following steps: butyl titanate is slowly dropped into aqueous isopropanol, is stirred evenly, dispersion liquid A is obtained；Ammonium metavanadate is added to absolute ethanol, is stirred evenly, dispersion liquid B is obtained；The dispersion liquid B is slowly dropped into dispersion liquid A, is stirred evenly and cooled to room temperature after heated reflow treatment, product V-TiO is obtained2；By the V-TiO2It is placed in high-temperature calcination under ammonia atmosphere, obtains nanometer bulk N/V-TiO2Photochemical catalyst；By above-mentioned N/V-TiO2Photochemical catalyst is scattered in dehydrated alcohol, and five water bismuth nitrates are added, and after five water bismuth nitrates are completely dissolved, tantalic chloride is added and is completely dissolved to it, then is adjusted and obtained Bi through hydrothermal synthesis after pH to 9~113TaO7/N/V‑TiO2Composite material.Pass through N, V codope TiO in the present invention2With Bi3TaO7Synergistic effect caused by coupling is to improve the service life in light induced electron and hole, and the stability of compound rear catalyst is effectively promoted.
Description
Technical field
The invention belongs to nano material synthesis technical field more particularly to a kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate
The preparation method and application of Z-type heterojunction photocatalyst.
Background technique
Titanium dioxide (TiO2) due to its with chemical inertness, good bio-compatibility, stronger oxidability and
The ability of resist chemical, and cheap, energy conversion, wastewater treatment, the depollution of environment, sensor, coating, cosmetics,
The numerous areas such as catalyst, filler all cause the highest attention of domestic and foreign scholars.Especially as a kind of N-type of function admirable
Semiconductor material can make full use of solar energy, energy-saving and environment-friendly, be a kind of nanometer of the most wide function of current application prospect
It can material.Although titanium dioxide is a kind of photochemical catalyst being potential, (anatase is about 3.2eV to broad-band gap, and rutile is about
For 3.0eV) make TiO2 can only occupied sunlight 5% wavelength it is shorter ultraviolet light (λ ﹤ 387nm) excitation, meanwhile, light excitation
The electrons and holes of generation are easily compound, cause light absorbing quantum yield very low, this hinders this light of titanium dioxide significantly
The application of catalyst.
In order to solve this problem, domestic and international scientist has carried out a large amount of research, and the method applied at present specifically includes that
It is coupled with low-gap semiconductor, dyestuff or metallic compound surface sensitizing and noble metal loading etc..Wherein metal/non-metal
Ion doping is widely used as wherein relatively simple and efficient method, but finds metallic element in the course of the study
Having some limitations property of doping, for example doped samples can usually have thermal instability, and easily become in Carrier recombination
Heart etc., and these problems will limit the large-scale application of doping vario-property.So in recent years for utilizing nonmetalloid to two
The research that titanium oxide is doped and is modified becomes a hot spot of photocatalysis field research.Up to the present, nonmetallic ion
Doping is concentrated mainly on nitrogen, carbon, sulphur, boron and halogen etc..
The cardinal principle of nonmetal doping, which refers to nonmetalloid, replaces nano-TiO2In O2-Either will
Nonmetalloid is filled into TiO2 interstitial void the chemical constituent and structure for changing TiO2, and then changes its optical property,
Currently used preparation method specifically includes that solution combustion method, hydro-thermal method, colloidal sol-microwave-hydrothermal method combination ultrasonic technique etc.,
The nano-titanium dioxide of the wherein C of solution combustion method preparation, N doping is mainly Detitanium-ore-type, and crystallite dimension is in 9~15nm, grain
Diameter is distributed in 30~180nm, but this method process time is longer, and cost of manufacture is high, and the material of formation is easy to reunite, utilization efficiency
It is low, it is unfavorable for promoting the use of in practical applications；TiO2 is adulterated by colloidal sol-microwave-hydrothermal method combination ultrasonic technique preparation N
Microballoon does not have to destroy the pattern of microballoon before and after hydro-thermal reaction, but apparent nanocrystalline assembling phenomenon occurs in surface, and with
There is the tightly packed and agglomeration of nanocrystal, seriously affect in the increase of the additional amount of ammonium hydroxide, partial sample surface
Photocatalysis efficiency.
In addition to this, novel Z-type photochemical catalyst can effectively promote the separation and transfer of electron hole, be further to mention
Rise the active effective way of its photocatalysis performance.Pass through bismuth tantalate (Bi3TaO7) nano dot is carried on nitrogen (N), vanadium (V) codope
TiO2Nanometer blocks can make up defect existing for monomeric substance effectively to construct Z-type heterojunction photocatalysis system and solve above-mentioned
The problem of.Therefore, the present invention provides a kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate heterojunction photocatalyst preparation side
Method, it is intended in utilize Bi3TaO7With N/V-TiO2The two it is compound caused by synergistic effect come reinforced composite stability and
The quick separating of light induced electron and hole is promoted to promote its photocatalytic activity to inhibit the compound of photo-generated carrier.
Summary of the invention
A kind of nitrogen, vanadium codope dioxy are provided the purpose of the invention is to overcome the problems of the above-mentioned prior art
Change titanium/bismuth tantalate Z-type heterojunction photocatalyst preparation method and application.
In order to achieve the above objectives, the present invention is achieved through the following technical solutions:
A kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method, which is characterized in that
The following steps are included:
Butyl titanate is slowly dropped into aqueous isopropanol by step 1, is stirred evenly, and dispersion liquid A, the metatitanic acid are obtained
The volume of four butyl esters is 0.1~0.3mL, and the volume of aqueous isopropanol is 5~20mL；
Ammonium metavanadate is added to absolute ethanol by step 2, is stirred evenly, and dispersion liquid B, the matter of the ammonium metavanadate are obtained
Amount is 0.2~0.6g, and the volume of dehydrated alcohol is 50~80mL；
Step 3: the dispersion liquid B being slowly dropped into dispersion liquid A, is stirred evenly and naturally cold after heated reflow treatment
But it to room temperature, is centrifugated, washing obtains product V-TiO2；
Step 4: by the V-TiO2It is placed in high-temperature calcination under ammonia atmosphere, obtains nanometer bulk N/V-TiO2Photochemical catalyst；
Step 5: by above-mentioned N/V-TiO2Photochemical catalyst is scattered in dehydrated alcohol, five water bismuth nitrates is added, to five water nitre
After sour bismuth is completely dissolved, tantalic chloride is added and is completely dissolved to it, then adjusts pH to 9~11 and is placed on 180~240 DEG C of environment
In, constant temperature thermal response 12~for 24 hours, centrifugation, washing are dried to get Bi is arrived3TaO7/N/V-TiO2Composite material.
Preferably, in step 3, the reflux temperature for being heated to reflux processing is 60~80 DEG C, and return time is 4~6h.
Preferably, step 4 high temperature calcining specific method includes: by V-TiO2It is placed in the tube furnace of ammonia atmosphere, with 3
The heating rate of~5 DEG C/min is warming up to 500~800 DEG C, then 4~8h of constant temperature is down to room with the rate of temperature fall of 5 DEG C/min
Temperature obtains nanometer bulk N/V-TiO2Photochemical catalyst；More preferably, 650 DEG C are warming up to the heating rate of 4 DEG C/min, constant temperature 6h.
Preferably, in step 5, the bismuth nitrate, tantalic chloride, N/V-TiO2And the amount ratio of dehydrated alcohol be 0.1~
0.3g:0.05~0.2g:0.2~0.4g:20~40mL.
Preferably, in step 5, the NaOH solution concentration is 0.5~1.0mol/L；More preferably, the NaOH solution is dense
Degree is 1.0mol/L.
Preferably, in step 5, the washing refers to alternately is washed 3 times with ultrapure water and dehydrated alcohol, and the drying, which refers to, to be placed in
50~60 DEG C of vacuum drying environment, dry 5~10h.
The second object of the present invention is, provides a kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type hetero-junctions light is urged
The application of agent catalytic degradation organic pollutants under ultraviolet light or radiation of visible light.
Beneficial effects of the present invention:
(1) nitrogen prepared by the present invention, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction material, preparation process green
Simply, at low cost, environmental protection is easy to large-scale industrial production, which has excellent environmental stability, is solving
There is potential application prospect in terms of solar energy conversion and environmental pollution.
(2) nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction material improve visible light absorption capacity, urge in light
The suspension characteristic changed in degradation process effectively raises the utilization rate to light source.
(3)0D/3D Bi3TaO7Nano dot/N/V-TiO2Nanometer blocks composite material can be used as the visible light light of function admirable
Catalyst.N, V codope TiO2On the basis of again with Bi3TaO7Synergistic effect caused by coupling, which not only improves, improves photoproduction
In the service life of electrons and holes, promote the transmission of photogenerated charge, and the stability of compound rear catalyst is effectively promoted.Therefore,
Bi3TaO7Nano dot/N/V-TiO2Nanometer blocks composite material improves catalyst to the degradation effect of organic dyestuff significantly,
Photocatalysis practical application area has broad prospects.
Detailed description of the invention
Fig. 1 is Bi obtained by the present embodiment3TaO7/N/V-TiO2The X ray diffracting spectrum (XRD) of heterojunction material；
Fig. 2 is the present embodiment institute Bi3TaO7/N/V-TiO2The atomic force microscope and transmission electron microscope picture of heterojunction material,
In (A) be N/V-TiO2Atomic force microscope, (B) is N/V-TiO2Thickness；(C) figure is N/V-TiO2Transmission electron microscope；(D,
E) figure is Bi3TaO7/N/V-TiO2Transmission electron microscope, (F) figure is Bi3TaO7/N/V-TiO2The diffraction pattern of transmission electron microscope.
Fig. 3 is ultraviolet-visible absorption spectra of prepared heterojunction material；
Fig. 4 is binary composite photo-catalyst Bi3TaO7/N/V-TiO2Photoelectric current (a) and impedance diagram (b)；
Fig. 5 be prepared sample under visible light illumination to concentration be 20mg/L occrycetin photocatalytic degradation and follow
Ring stabilizing effect figure.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
A kind of preparation method of nitrogen, vanadium codope titanium dioxide, method includes the following steps:
1. 0.25mL butyl titanate is taken to be slowly dropped into 10mL isopropanol, it is thoroughly mixed uniformly, obtains dispersion liquid
A；
2. taking 0.5g ammonium metavanadate to be scattered in 70mL dehydrated alcohol and the ultrapure water mixed solution of 0.15mL, ultrasonic disperse
0.5h obtains dispersion liquid B；
3. dispersion liquid A is slowly dropped into dispersion liquid B, flow back 5h at 80 DEG C, products therefrom V-TiO2It is washed through 3 alcohol,
It is dry under vacuum condition.Then, by ground V-TiO2It is put into porcelain crucible, is placed in tube furnace under ammonia atmosphere and heats up
To 600 DEG C of calcining 4h, it is cooled to room temperature to the end of being calcined to get nanometer bulk N/V-TiO is arrived2Photochemical catalyst.
By the N/V-TiO2Photochemical catalyst carries out X ray diffracting spectrum, as shown in Figure 1, it can be found that compared to discovery
TiO2, N/V-TiO2Peak position apparent offset has occurred, this shows N/V-TiO2N and V element in composite material have succeeded
Doping, and without other impurity.
By the N/V-TiO2Photochemical catalyst carries out atomic force microscope and transmission electron microscope picture, as shown in Fig. 2, wherein (A) is
N/V-TiO2Atomic force microscope, (B) is N/V-TiO2Thickness, N/V-TiO as we know from the figure2Thickness be about 9nm；(C)
Figure is N/V-TiO2Transmission electron microscope, structure are that nanometer is blocky, are uniformly dispersed, permeability is good.
Embodiment 2
A kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method, this method include
Following steps:
0.1mL butyl titanate is slowly dropped into 5mL aqueous isopropanol by step 1, is stirred evenly, is obtained dispersion liquid A；
0.2g ammonium metavanadate is added in 50mL dehydrated alcohol step 2, stirs evenly, obtains dispersion liquid B；
Step 3: the dispersion liquid B being slowly dropped into dispersion liquid A, is stirred evenly and naturally cold after heated reflow treatment
But it to room temperature, is centrifugated, washing obtains product V-TiO2, the reflux temperature for being heated to reflux processing is 70 DEG C, when reflux
Between be 5h；
Step 4: by step V-TiO2It is placed in the tube furnace of ammonia atmosphere, is warming up to 650 with the heating rate of 3 DEG C/min
DEG C, then constant temperature 6h is down to room temperature with the rate of temperature fall of 5 DEG C/min, obtain nanometer bulk N/V-TiO2Photochemical catalyst；
Step 5: by above-mentioned 0.3g N/V-TiO2Photochemical catalyst is scattered in 30mL dehydrated alcohol, and five water nitre of 0.2g is added
Sour bismuth is added 0.1g tantalic chloride and is completely dissolved to it after five water bismuth nitrates are completely dissolved, then with concentration is 1.0mol/L's
Sodium hydroxide solution adjusts pH to 10 and is placed in 200 DEG C of environment, constant temperature thermal response 16h, centrifugation, with deionized water and anhydrous second
Alcohol alternately washing three times, it is dry to get arriving Bi3TaO7The Bi that mass fraction is 10%3TaO7/N/V-TiO2Composite material, i.e.,
10%Bi3TaO7/N/V-TiO2。
By the 10%Bi3TaO7/N/V-TiO2Composite material carries out X ray diffracting spectrum, as shown in Figure 1, Bi3TaO7/N/
V-TiO2There is Bi in the X ray diffracting spectrum of composite material3TaO7Diffraction maximum, also have N/V-TiO2Diffraction maximum, this shows
Bi3TaO7/N/V-TiO2Successful preparation.
By the 10%Bi3TaO7/N/V-TiO2Composite material carries out atomic force microscope and transmission electron microscope picture, as Fig. 2 (D,
E) described in figure, Bi as we know from the figure3TaO7It is evenly distributed on N/V-TiO2Nanometer blocks surface, soilless sticking phenomenon；Fig. 2 (F) figure is
Bi3TaO7/N/V-TiO2The diffraction pattern of transmission electron microscope, shows Bi3TaO7/N/V-TiO2Purity is high, good crystallinity.
By the Bi3TaO7/N/V-TiO2Composite material carries out ultraviolet-visible absorption spectra test, as shown in figure 3, comparing
Pure Bi3TaO7And N/V-TiO2, Bi3TaO7/N/V-TiO2The visible absorption of composite material is remarkably reinforced.
By the 10%Bi3TaO7/N/V-TiO2Composite material carries out photoelectric current and testing impedance, by Fig. 4 test result table
It is bright, the sequence of photoelectric current from high to low are as follows: IBi3TaO7/N/V-TiO2> IN/V-TiO2> IBi3TaO7> ITiO2, and impedance magnitude and photoelectricity
Stream sequence completely on the contrary, itself the result shows that, binary composite Bi3TaO7/N/V-TiO2With best photo-generate electron-hole point
From efficiency, electron lifetime is best, has more preferably photocatalytic degradation efficiency.
By the 10%Bi3TaO7/N/V-TiO2Composite material and Bi3TaO7And N/V-TiO2It is real that photocatalytic degradation is carried out respectively
Test, each sample under visible light illumination to concentration be 20mg/L occrycetin photocatalytic degradation and cyclical stability effect such as
Shown in Fig. 5, the result shows that 10%Bi3TaO7/N/V-TiO2It is imitated with good recycling and optimal photocatalytic degradation
Rate, result are consistent with the photochemistry test result of Fig. 4.
Embodiment 3
A kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method, this method include
Following steps:
0.3mL butyl titanate is slowly dropped into 20mL aqueous isopropanol by step 1, is stirred evenly, is obtained dispersion liquid A；
0.6g ammonium metavanadate is added in 80mL dehydrated alcohol step 2, stirs evenly, obtains dispersion liquid B；
Step 3: the dispersion liquid B being slowly dropped into dispersion liquid A, is stirred evenly and naturally cold after heated reflow treatment
But it to room temperature, is centrifugated, washing obtains product V-TiO2, the reflux temperature for being heated to reflux processing is 60 DEG C, when reflux
Between be 6h；
Step 4: by step V-TiO2It is placed in the tube furnace of ammonia atmosphere, is warming up to 800 with the heating rate of 5 DEG C/min
DEG C, then constant temperature 4h is down to room temperature with the rate of temperature fall of 5 DEG C/min, obtain nanometer bulk N/V-TiO2Photochemical catalyst；
Step 5: by above-mentioned N/V-TiO2Photochemical catalyst is scattered in 20mL dehydrated alcohol, and five water bismuth nitrate of 0.3g is added,
After five water bismuth nitrates are completely dissolved, 0.2g tantalic chloride is added and is completely dissolved to it, then adjusts pH to 9 and is placed on 180 DEG C of rings
In border, constant temperature thermal response 12h, centrifugation, with deionized water and dehydrated alcohol alternately washing three times, it is dry to get arriving Bi3TaO7Matter
Measure the Bi that score is 20%3TaO7/N/V-TiO2Composite material, i.e. 20%Bi3TaO7/N/V-TiO2。
As shown in Fig. 5 (a), 20%Bi that the present embodiment obtains3TaO7/N/V-TiO2Composite material has efficient degradation
Efficiency, and as shown in Fig. 5 (b), the 20%Bi3TaO7/N/V-TiO2It is a kind of ideal with good photocatalysis stability
Photochemical catalyst form.
Embodiment 4
A kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method, this method include
Following steps:
0.2mL butyl titanate is slowly dropped into 15mL aqueous isopropanol by step 1, is stirred evenly, is obtained dispersion liquid A；
0.4g ammonium metavanadate is added in 60mL dehydrated alcohol step 2, stirs evenly, obtains dispersion liquid B；
Step 3: the dispersion liquid B being slowly dropped into dispersion liquid A, is stirred evenly and naturally cold after heated reflow treatment
But it to room temperature, is centrifugated, washing obtains product V-TiO2, the reflux temperature for being heated to reflux processing is 80 DEG C, when reflux
Between be 4h；
Step 4: by step V-TiO2It is placed in the tube furnace of ammonia atmosphere, is warming up to 500 with the heating rate of 3 DEG C/min
DEG C, then constant temperature 4h is down to room temperature with the rate of temperature fall of 5 DEG C/min, obtain nanometer bulk N/V-TiO2Photochemical catalyst；
Step 5: by above-mentioned 0.3g N/V-TiO2Photochemical catalyst is scattered in 30mL dehydrated alcohol, and five water nitre of 0.2g is added
Sour bismuth is added 0.1g tantalic chloride and is completely dissolved to it, then adjust pH to 9 and be placed on 180 after five water bismuth nitrates are completely dissolved
In DEG C environment, constant temperature thermal response 12h, centrifugation, with deionized water and dehydrated alcohol alternately washing three times, it is dry to get arriving
Bi3TaO7The Bi that mass fraction is 15%3TaO7/N/V-TiO2Composite material, i.e. 15%Bi3TaO7/N/V-TiO2。
As shown in Fig. 5 (a), 15%Bi that the present embodiment obtains3TaO7/N/V-TiO2Composite material has efficient degradation
Efficiency is a kind of ideal photochemical catalyst form.
Embodiment 5
A kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method, this method include
Following steps:
0.3mL butyl titanate is slowly dropped into 10mL aqueous isopropanol by step 1, is stirred evenly, is obtained dispersion liquid A；
0.4g ammonium metavanadate is added in 60mL dehydrated alcohol step 2, stirs evenly, obtains dispersion liquid B；
Step 3: the dispersion liquid B being slowly dropped into dispersion liquid A, is stirred evenly and naturally cold after heated reflow treatment
But it to room temperature, is centrifugated, washing obtains product V-TiO2, the reflux temperature for being heated to reflux processing is 80 DEG C, when reflux
Between be 4h；
Step 4, by step V-TiO2It is placed in the tube furnace of ammonia atmosphere, is warming up to 500 with the heating rate of 3 DEG C/min
DEG C, then constant temperature 4h is down to room temperature with the rate of temperature fall of 5 DEG C/min, obtain nanometer bulk N/V-TiO2Photochemical catalyst；
Step 5, by above-mentioned 0.4g N/V-TiO2Photochemical catalyst is scattered in 40mL dehydrated alcohol, and five water nitre of 0.1g is added
Sour bismuth is added 0.05g tantalic chloride and is completely dissolved to it, reuse the hydrogen-oxygen of 1mol/L after five water bismuth nitrates are completely dissolved
Change sodium solution adjusting pH to 9 to be placed in 180 DEG C of environment, constant temperature thermal response 12h, centrifugation is handed over deionized water and dehydrated alcohol
For washing three times, it is dry to get arriving Bi3TaO7The Bi that mass fraction is 5%3TaO7/N/V-TiO2Composite material, i.e., 5%
Bi3TaO7/N/V-TiO2。
As shown in Fig. 5 (a), 5%Bi that the present embodiment obtains3TaO7/N/V-TiO2Composite material has efficient degradation effect
Rate is a kind of ideal photochemical catalyst form.
Comparative example 1
A kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate photochemical catalyst preparation method, method includes the following steps:
0.2mL butyl titanate is slowly dropped into 15mL aqueous isopropanol by step 1, is stirred evenly, is obtained dispersion liquid A；
0.4g ammonium metavanadate is added in 60mL dehydrated alcohol step 2, stirs evenly, obtains dispersion liquid B；
Step 3: the dispersion liquid B being slowly dropped into dispersion liquid A, is stirred evenly and naturally cold after heated reflow treatment
But it to room temperature, is centrifugated, washing obtains product V-TiO2, the reflux temperature for being heated to reflux processing is 80 DEG C, when reflux
Between be 4h；
Step 4: by step V-TiO2It is placed in the tube furnace of ammonia atmosphere, is warming up to 500 with the heating rate of 3 DEG C/min
DEG C, then constant temperature 4h is down to room temperature with the rate of temperature fall of 5 DEG C/min, obtain nanometer bulk N/V-TiO2Photochemical catalyst；
Step 5: in 40mL dehydrated alcohol, five water bismuth nitrate of 0.2g is added, after five water bismuth nitrates are completely dissolved, is added
0.1g tantalic chloride is completely dissolved to it, then is adjusted pH to 9 with sodium hydroxide solution and be placed in 180 DEG C of environment, and constant temperature heating is anti-
Answer 12h, centrifugation, with deionized water and dehydrated alcohol alternately washing three times, it is dry to get arriving Bi3TaO7Photochemical catalyst.
Step 6: weighing 0.27g nanometers of bulk N/V-TiO2Photochemical catalyst and 0.03gBi3TaO7Photochemical catalyst physical mixed
Uniformly, the Bi of physical mixed is obtained3TaO7/N/V-TiO2, i.e. B/NVTi-PM.
As shown in Fig. 5 (a), the B/NVTi-PM composite material that the present embodiment obtains is relatively and described in above-described embodiment 2-5
Composite material, photocatalysis effect are substantially reduced.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of nitrogen, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst preparation method, which is characterized in that packet
Include following steps:
Butyl titanate is slowly dropped into aqueous isopropanol by step 1, is stirred evenly, and dispersion liquid A, four fourth of metatitanic acid are obtained
The volume of ester is 0.1~0.3mL, and the volume of aqueous isopropanol is 5~20mL；
Ammonium metavanadate is added to absolute ethanol by step 2, is stirred evenly, and dispersion liquid B is obtained, and the quality of the ammonium metavanadate is
0.2~0.6g, the volume of dehydrated alcohol are 50~80mL；
Step 3: the dispersion liquid B being slowly dropped into dispersion liquid A, stirs evenly and is naturally cooled to after heated reflow treatment
Room temperature is centrifugated, and washing obtains product V-TiO2；
Step 4: by the V-TiO2It is placed in high-temperature calcination under ammonia atmosphere, obtains nanometer bulk N/V-TiO2Photochemical catalyst；
Step 5: by above-mentioned N/V-TiO2Photochemical catalyst is scattered in dehydrated alcohol, and five water bismuth nitrates are added, complete to five water bismuth nitrates
After fully dissolved, tantalic chloride is added and is completely dissolved to it, then is placed on 180~240 DEG C by NaOH solution adjusting pH to 9~11
In environment, constant temperature thermal response 12~for 24 hours, centrifugation, washing are dried to get Bi is arrived3TaO7/N/V-TiO2Composite material.
2. a kind of nitrogen according to claim 1, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst system
Preparation Method, it is characterised in that: in step 3, the reflux temperature for being heated to reflux processing be 60~80 DEG C, return time be 4~
6h。
3. a kind of nitrogen according to claim 1, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst system
Preparation Method, which is characterized in that it includes: by V-TiO that step 4 high temperature, which calcines specific method,2It is placed in the tube furnace of ammonia atmosphere,
500~800 DEG C are warming up to the heating rate of 3~5 DEG C/min, then 4~8h of constant temperature is down to the rate of temperature fall of 5 DEG C/min
Room temperature obtains nanometer bulk N/V-TiO2Photochemical catalyst.
4. a kind of nitrogen according to claim 1, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst system
Preparation Method, it is characterised in that: in step 5, the bismuth nitrate, tantalic chloride, N/V-TiO2And the amount ratio of dehydrated alcohol is 0.1
~0.3g:0.05~0.2g:0.2~0.4g:20~40mL.
5. a kind of nitrogen according to claim 1, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst system
Preparation Method, it is characterised in that: in step 5, the washing refers to alternately is washed 3 times with ultrapure water and dehydrated alcohol, and the drying refers to
It is placed in 50~60 DEG C of vacuum drying environment, dry 5~10h.
6. a kind of nitrogen according to claim 1, vanadium codope titanium dioxide/bismuth tantalate Z-type heterojunction photocatalyst system
Preparation Method, it is characterised in that: in step 5, the NaOH solution concentration is 0.5~1.0mol/L.
7. one kind is according to claim 1 to nitrogen described in 5 any one, vanadium codope titanium dioxide/bismuth tantalate Z-type hetero-junctions light
The application of catalyst occrycetin in catalytic degradation water under ultraviolet light or radiation of visible light.
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