CN107649118A - A kind of BiVO4Load multiphase TiO2The preparation method of visible light composite photocatalyst - Google Patents
A kind of BiVO4Load multiphase TiO2The preparation method of visible light composite photocatalyst Download PDFInfo
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- CN107649118A CN107649118A CN201710829743.3A CN201710829743A CN107649118A CN 107649118 A CN107649118 A CN 107649118A CN 201710829743 A CN201710829743 A CN 201710829743A CN 107649118 A CN107649118 A CN 107649118A
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- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000002131 composite material Substances 0.000 title abstract description 8
- 239000011941 photocatalyst Substances 0.000 title abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 20
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 11
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000003643 water by type Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 230000033228 biological regulation Effects 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 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 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims 1
- 239000006227 byproduct Substances 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 239000002105 nanoparticle Substances 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 230000004044 response Effects 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 239000010842 industrial wastewater Substances 0.000 abstract description 2
- 238000007704 wet chemistry method Methods 0.000 abstract description 2
- 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 abstract 1
- 230000009471 action Effects 0.000 abstract 1
- 229960000907 methylthioninium chloride Drugs 0.000 abstract 1
- 230000005012 migration Effects 0.000 abstract 1
- 238000013508 migration Methods 0.000 abstract 1
- 230000009467 reduction Effects 0.000 abstract 1
- 238000001338 self-assembly Methods 0.000 abstract 1
- 239000012798 spherical particle Substances 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 abstract 1
- 239000000725 suspension Substances 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 239000008236 heating water Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910003087 TiOx Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000002243 precursor Substances 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
- 238000006479 redox reaction Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J35/19—Catalysts containing parts with different compositions
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Thermal Sciences (AREA)
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Abstract
TiO2As a kind of common semi-conducting material, quantum efficiency is relatively low, seriously constrains its application in photocatalysis field without the shortcomings of response to visible ray.The present invention is prepared for unformed TiO first using isopropyl titanate as raw material2Micron ball, then it is prepared for by green water-heat process the TiO with anatase/brockite multiphase2Mesoporous Spheres, the structure are made up of nano particle, pass through compound action during nanosizing process reduction charge migration.Secondly by easy wet chemistry method by BiVO4Nano particle loads to TiO2On Mesoporous Spheres, obtained composite heterogenous junction structure has well visible light-responded, has Visible Light Induced Photocatalytic effect to methylene blue.BiVO4/TiO2The micron level spherical particle form that composite photo-catalyst is formed with primary nanoparticle self assembly is present, and is easy to reclaim from sewage, has highly important practical significance in Industrial Wastewater Treatment.
Description
Technical field：
The present invention relates to a kind of BiVO4Load TiO2The preparation method of mesoporous micron ball structure photochemical catalyst, more specifically
Say, the TiO containing anatase/brockite multiphase is prepared using hydro-thermal method2Flower-like nanostructure is carrier, passes through wet-chemical
Method is by BiVO4Nano particle loads to TiO2, preparing has visible light-responded hetero-junctions nano-photocatalyst.This technology belongs to
The preparation field of nano material.
Background technology：
In recent years, as the fast development of social economy, problem of environmental pollution increasingly highlight.Country arranges for industrial wastewater
The high standard put, it is desirable to which a kind of sewage water treatment method efficiently, economic is found by especially medium-sized and small enterprises of each enterprise.
Photocatalitic Technique of Semiconductor is a kind of high efficiency technical that catalytic reaction is carried out using solar energy that recent decades are risen,
It is widely applied to photolysis water hydrogen, photocatalytic degradation organic matter etc..1972, Fujishima et al. used TiO2Photoelectricity
Water is decomposed in pole, has started the upsurge of photocatalysis technology research since then.Titanium dioxide as a kind of semi-conducting material, by
In its cost is cheap, nontoxic, chemical stability is high the characteristics of, the extensive concern of society is received.However, titanium dioxide has
There is the shortcomings that some protrusions, it is restricted in the application of photocatalysis field：
(1) quantum efficiency of titanium dioxide is relatively low, and the recombination rate of photo-generate electron-hole is high, can by nano titaniaization
To improve the transfer of photogenerated charge, but industrially the recovery to catalyst generates certain difficulty；
(2) energy gap of titanium dioxide is 3.2eV, the ultraviolet light that wavelength can only be utilized to be less than 387nm, and ultraviolet light portion
Divide and only about account for the 4% of solar spectrum, greatly limit the utilization to luminous energy.
In order to solve the above problems, generally to TiO2Material is modified processing.On the one hand by self assembling process, two are made
On the basis of TiOx nano, complex nanotube, nanometer rods, 3D nanostructureds are constructed, these structures are by nanometer chi
Very little primary granule constitutes larger-size secondary structure, is advantageous to sedimentation, the recovery of catalyst.On the other hand be by from
The modes such as sub- doping, noble metal loading, semiconductors coupling are modified, and wherein semiconductors coupling is more effective manner.Pucherite
As a kind of narrow band gap (2.4eV) semiconductor, but because it has shorter electron transfer length, it is generally used alone as photocatalysis
Effect is unsatisfactory during agent.It can be used for and TiO2Carry out compound, strengthen the light abstraction width of photochemical catalyst, and pass through hetero-junctions
Structure reach increase the separation of charge life-span purpose, improve photocatalysis efficiency.At present on BiVO4Load TiO2Complex light is urged
The report of agent is less, and most of researchs are concentrated and formerly prepare BiVO4Particle, sol method is recycled by TiO2It is supported on BiVO4
Surface (Yin Hu, Danzhen Li, Yi Zheng, Wei Chen, Yunhui He, Yu Shao, Xianzhi Fu,
Guangcan Xiao,Applied Catalysis B: Environmental 104(2011)30-36Wenjuan Li,Ze
Wang,Defen Kong,Dandan Du,Min Zhou,Yong Du,Tingjiang Yan,Jinmao You,Desheng
Kong Journal of Alloys and Compounds 688(2016)703-711)；And the BiVO prepared4Load TiO2It is more
Exist with scattered small particles form (Xianliang Song, Yingying Li, Zhedong Wei, Shengying Ye,
Dionysios D. Dionysiou,Chemical Engineering Journal 314(2017)443–452,Natda
Wetchakun,Surachai Chainet,Sukon Phanichphant,Khatcharin Wetchakun,Ceramics
International 41 (2015) 5999-6004), it is unfavorable for the recovery after catalytic reaction.It is noted that at present almost
There is no BiVO4Load the TiO of multiphase2The relevant report of ball visible light catalyst.
The content of the invention
It is an object of the invention to provide a kind of BiVO4Load multiphase TiO2The preparation method of visible light catalyst, with gram
The deficiency in prior art is taken, the program can realize semiconductors coupling to improve the catalytic activity of catalyst, while with nanometer
The form for the micron Mesoporous Spheres that particles self assemble forms is present, and is easy to separate from liquid phase, does not easily cause secondary pollution, while
Be advantageous to the recycling of catalyst.
To realize above-mentioned purpose, solve above-mentioned technical problem, using following technical scheme, a kind of BiVO4Load is mixed
Synthetic phase TiO2The preparation method of visible light catalyst, include following step：
(1) make raw material from isopropyl titanate (TTIP), be dissolved in 500mL ethanol, adding a certain amount of concentration is
0.1mol·L-1KCl solution, trigger hydrolysis, occur stopping stirring after white precipitate, stand 12-48h.Centrifugation, water
Wash, dry, obtain white powder.
(2) powder in 0.6g (1) is added to the 0.1molL containing 60mL-1In NaOH solution water heating kettle liner, it is added dropwise
0.9mL mass fraction is 3% hydrogen peroxide, the 140-200 DEG C of reaction 2-20h in air dry oven.After being cooled to room temperature, it will produce
Thing centrifugation, washing, dry, obtain white powder.
(3) powder in 1.0g (2) is added in 250mL 0.1M watery hydrochloric acid, be sufficiently stirred 1 hour, stand 1 hour.Will
Product centrifugation, washing, dry.Obtained white product 400-500 DEG C of calcining 60-120min in Muffle furnace, obtains white powder
End.
(4) by 2.425g Bi (NO3)3·5H2O is added to 100mL 0.4molL-1Dilute nitric acid solution in, fully stir
Mix to obtain bismuth nitrate solution.By 0.5849g NH4VO3It is added in 100mL 80 DEG C of deionized waters, is sufficiently stirred to obtain inclined vanadium
Acid ammonium solution, obtained TiO in the step of adding g (3)2Mesoporous Spheres, it is sufficiently stirred, and above-mentioned pucherite solution is added drop-wise to
In the solution.Using the pH=4 of ammoniacal liquor regulation system, mixture is placed in heating evaporation in 90 DEG C of water-baths, finally given bright orange
Mill base shape product.Washing, centrifugation, dry, obtain glassy yellow powder.
(5) powder obtained in step (4) is calcined in Muffle furnace, 400-500 DEG C is calcined 60-120min, final to obtain
To BiVO4Load multiphase TiO2Visible light catalyst.
The BiVO that this patent is selected4As a kind of important narrow band gap (about 2.4eV) semi-conducting material, generally separately as
A kind of visible light catalyst uses, while can be regarded as a kind of excellent photosensitizer.By BiVO4With TiO2It is compound, Ke Yixian
Work widens TiO2Spectrum respective range.When the energy of incident light is not enough to excite TiO2Photo-generate electron-hole is produced so as to trigger
During redox reaction, BiVO4But it can be excited, improve the utilization rate of solar energy.Secondly, the TiO of multiphase2Itself
Heterojunction structure can be formed, further enhances the separating effect of photogenerated charge.Finally, compared with other patterns, composite photocatalyst
Agent exists in the form of the secondary mesoporous micron ball that nano-particles self assemble forms, and is returned after being advantageous to catalyst use from sewage
Receive and utilize.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) present invention is prepared for BiVO using wet chemistry method4The TiO of load2Mesoporous micron spherical structure, simple equipments, cost
It is relatively low.
(2) narrow gap semiconductor BiVO is used4With TiO2It is compound, spectral response range has been widened, has improved Solar use
Rate.
(3) flower-shaped TiO2Precursor construction causes BiVO4Contact area improve, form good heterojunction structure, enhancing suppression
Light induced electron processed and hole it is compound；TiO simultaneously2Middle anatase/brockite multiphase further enhances separating effect.
(4) composite photo-catalyst exists in the form of the secondary mesoporous micron ball that nano-particles self assemble forms, be easy to from
Recycled in sewage after processing, avoid secondary pollution, be a kind of environmentally friendly photochemical catalyst.
Brief description of the drawings
Fig. 1：Multiphase TiO2The TEM pictures of flower-shaped ball presoma
Fig. 2：BiVO in embodiment 14/TiO2The TEM pictures of mesoporous micron ball
Fig. 3：BiVO in embodiment 14/TiO2The spectral response of mesoporous micron ball
Embodiment
Embodiment 1：
2mL 0.1molL are added into 500mL ethanol-1KCl solution, stir 10min.Add 9mL TTIP, stirring
30 minutes.Stand 24 hours after, white turbid is centrifuged, and with ethanol, washing, drying.0.6g above-mentioned product is added to
60mL 0.1molL-1In NaOH solution, stir 30 minutes, the hydrogen peroxide for then adding 0.9mL mass fractions 3% is molten
Liquid, stir 2 minutes, encapsulation water heating kettle 180 DEG C of reaction 10h in air dry oven.After taking out water heating kettle, room temperature is cooled to, will
Product washing, dry.The above-mentioned products of 1.0g are added to 250 milliliters of 0.1molL-1Watery hydrochloric acid in, persistently stir 1h, afterwards
Stop stirring and stand 1h.Supernatant liquor is outwelled afterwards, washing, desciccate, product is calcined to 450 DEG C of 2h in Muffle furnace.Claim
Take 2.425g Bi (NO3)3It is added to 100mL 0.4molL-1Salpeter solution in, stir 30min, formed solution A.Weigh
0.5849g NH4VO3It is added in 100mL deionized waters, 80 DEG C of heating water baths simultaneously stir, and add 3.9935g TiO2,
10min is stirred, forms suspension B.Solution A is slowly dropped in suspension B, stirs 30min.Ammoniacal liquor adjusts pH value of solution=4,
90 DEG C of water-baths obtain glassy yellow mud.Washing, dry, 450 DEG C of calcining 2h in Muffle furnace.Can obtain mol ratio is Bi：Ti
=1:10 BiVO4The multiphase TiO of load2Composite mesoporous photochemical catalyst.Fig. 2 is BiVO4/TiO2Mesoporous micron ball
TEM pictures, Fig. 3 BiVO4/TiO2The spectral response figure of mesoporous micron ball.
Embodiment 2：
2mL 0.1molL are added into 500mL ethanol-1KCl solution, stir 10min.Add 9mL TTIP, stirring
30 minutes.Stand 24 hours after, white turbid is centrifuged, and with ethanol, washing, drying.0.6g above-mentioned product is added to
60mL 0.1molL-1In NaOH solution, stir 30 minutes, the hydrogen peroxide for then adding 0.9mL mass fractions 3% is molten
Liquid, stir 2 minutes, encapsulation water heating kettle 180 DEG C of reaction 10h in air dry oven.After taking out water heating kettle, room temperature is cooled to, will
Product washing, dry.The above-mentioned products of 1.0g are added to 250 milliliters of 0.1molL-1Watery hydrochloric acid in, persistently stir 1h, afterwards
Stop stirring and stand 1h.Supernatant liquor is outwelled afterwards, washing, desciccate, product is calcined to 450 DEG C of 2h in Muffle furnace.Claim
Take 2.425g Bi (NO3)3It is added to 100mL 0.4molL-1Salpeter solution in, stir 30min, formed solution A.Weigh
0.5849g NH4VO3It is added in 100mL deionized waters, 80 DEG C of heating water baths simultaneously stir, and add 19.9675g TiO2,
10min is stirred, forms suspension B.Solution A is slowly dropped in suspension B, stirs 30min.Ammoniacal liquor adjusts pH value of solution=4,
90 DEG C of water-baths obtain glassy yellow mud.Washing, dry, 450 DEG C of calcining 2h in Muffle furnace.Can obtain mol ratio is Bi：Ti
=1:50 BiVO4The multiphase TiO of load2Composite mesoporous photochemical catalyst.
Claims (4)
- A kind of 1. BiVO4Load multiphase TiO2The preparation method of visible light catalyst, it is characterised in that enter according to the following steps OK：(1) make raw material from isopropyl titanate (TTIP), be dissolved in 500mL ethanol, adding a certain amount of concentration is 0.1mol·L-1KCl solution, trigger hydrolysis, occur stopping stirring after white precipitate, stand 12-48h.Centrifuge, wash, Dry, obtain white powder.(2) powder in (1) is added to the 0.1molL containing 60mL-1In NaOH solution water heating kettle liner, it is added dropwise 0.9mL's Mass fraction is 3% hydrogen peroxide, the 140-200 DEG C of reaction 2-20h in air dry oven.After being cooled to room temperature, product is centrifuged, Washing, dry, obtain white powder.(3) powder in 1.0g (2) is added in 250mL 0.1M watery hydrochloric acid, be sufficiently stirred 1 hour, stand 1 hour.By product Centrifugation, washing, dry.Obtained white product 400-500 DEG C of calcining 120min in Muffle furnace, obtains white powder.(4) by 2.425g Bi (NO3)3·5H2O is added to 100mL 0.4molL-1Dilute nitric acid solution in, be sufficiently stirred To bismuth nitrate solution.By 0.5849g NH4VO3It is added in 100mL 80 DEG C of deionized waters, is sufficiently stirred to obtain ammonium metavanadate Solution, obtained TiO is added in a certain amount of step (3)2Mesoporous Spheres, it is sufficiently stirred, and above-mentioned pucherite solution is added drop-wise to In the solution.Using the pH=4 of ammoniacal liquor regulation system, mixture is placed in heating evaporation in 90 DEG C of water-baths, finally given bright orange Mill base shape product.Washing, centrifugation, dry, obtain glassy yellow powder.(5) powder obtained in step (4) is calcined in Muffle furnace, 400-500 DEG C of calcining 60-120min, finally given BiVO4Load multiphase TiO2Visible light catalyst.
- 2. BiVO as claimed in claim 14Load multiphase TiO2The preparation method of visible light catalyst, it is characterised in that The concentration that powder is added in step (2) is 10g/L, and optimal hydro-thermal scheme is 180 DEG C of reaction 10h.
- 3. BiVO as claimed in claim 14Load multiphase TiO2The preparation method of visible light catalyst, it is characterised in that Step (3) powder optimal calcining scheme in Muffle furnace is 450 DEG C of calcining 120min.
- 4. BiVO as claimed in claim 14Load multiphase TiO2The preparation method of visible light catalyst, it is characterised in that Step (4) TiO2The addition of Mesoporous Spheres is 0.3994-19.968g, optimal case 3.994g.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479752A (en) * | 2018-04-26 | 2018-09-04 | 青岛科技大学 | A kind of BiVO of two dimension carbon-coating load4/TiO2The preparation method of heterogeneous visible light catalyst |
| CN109603809A (en) * | 2019-01-25 | 2019-04-12 | 泉州师范学院 | A kind of preparation and application of pucherite quantum dot and titanium dioxide nano-belts composite photo-catalyst |
| CN110026170A (en) * | 2019-05-23 | 2019-07-19 | 乐山师范学院 | A kind of TiO of photocatalytic degradation rhodamine B2Photochemical catalyst and preparation method thereof |
| CN111229206A (en) * | 2020-02-25 | 2020-06-05 | 南开大学 | Preparation method and application of heterojunction visible-light-driven photocatalyst |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6592842B2 (en) * | 1999-10-01 | 2003-07-15 | Battelle Memorial Institute | Nanocrystalline heterojunction materials |
| CN1638868A (en) * | 2002-06-03 | 2005-07-13 | 旭化成株式会社 | Photocatalyst composition |
| CN1935362A (en) * | 2006-09-22 | 2007-03-28 | 中国海洋大学 | Method for preparing nano powder photocatalyst |
| CN101698506A (en) * | 2009-11-23 | 2010-04-28 | 江苏河海纳米科技股份有限公司 | Preparation method of mixed crystal type nanometer titanium dioxide |
| WO2011012935A2 (en) * | 2009-07-29 | 2011-02-03 | Universidade Do Minho | Photocatalytic coating for the controlled release of volatile agents |
| CN102580721A (en) * | 2011-12-19 | 2012-07-18 | 陕西科技大学 | Method for preparing TiO2/BiVO4 composite photocatalyst by MH method |
| CN103506110A (en) * | 2013-10-10 | 2014-01-15 | 青岛科技大学 | Preparation method of TiO2/WO3 double-layer composite nanotubes using TiO2 for coating WO3 |
| CN104549199A (en) * | 2014-11-05 | 2015-04-29 | 华文蔚 | Preparation method of visible light responsible TiO2 catalyst taking kaolin as matrix |
| CN105540656A (en) * | 2015-12-28 | 2016-05-04 | 南昌航空大学 | Anatase/brookite titanium dioxide heterojunction nano composite material |
| US20160288091A1 (en) * | 2015-03-31 | 2016-10-06 | Toto Ltd. | Photocatalytic coating composition |
| CN106031869A (en) * | 2015-03-12 | 2016-10-19 | 大连民族学院 | A BiVO4/TiO2 composite nanorod having visible light activity, and preparation and applications thereof |
-
2017
- 2017-09-15 CN CN201710829743.3A patent/CN107649118B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6592842B2 (en) * | 1999-10-01 | 2003-07-15 | Battelle Memorial Institute | Nanocrystalline heterojunction materials |
| CN1638868A (en) * | 2002-06-03 | 2005-07-13 | 旭化成株式会社 | Photocatalyst composition |
| CN1935362A (en) * | 2006-09-22 | 2007-03-28 | 中国海洋大学 | Method for preparing nano powder photocatalyst |
| WO2011012935A2 (en) * | 2009-07-29 | 2011-02-03 | Universidade Do Minho | Photocatalytic coating for the controlled release of volatile agents |
| CN101698506A (en) * | 2009-11-23 | 2010-04-28 | 江苏河海纳米科技股份有限公司 | Preparation method of mixed crystal type nanometer titanium dioxide |
| CN102580721A (en) * | 2011-12-19 | 2012-07-18 | 陕西科技大学 | Method for preparing TiO2/BiVO4 composite photocatalyst by MH method |
| CN103506110A (en) * | 2013-10-10 | 2014-01-15 | 青岛科技大学 | Preparation method of TiO2/WO3 double-layer composite nanotubes using TiO2 for coating WO3 |
| CN104549199A (en) * | 2014-11-05 | 2015-04-29 | 华文蔚 | Preparation method of visible light responsible TiO2 catalyst taking kaolin as matrix |
| CN106031869A (en) * | 2015-03-12 | 2016-10-19 | 大连民族学院 | A BiVO4/TiO2 composite nanorod having visible light activity, and preparation and applications thereof |
| US20160288091A1 (en) * | 2015-03-31 | 2016-10-06 | Toto Ltd. | Photocatalytic coating composition |
| CN105540656A (en) * | 2015-12-28 | 2016-05-04 | 南昌航空大学 | Anatase/brookite titanium dioxide heterojunction nano composite material |
Non-Patent Citations (4)
| Title |
|---|
| BIN ZHAO ET AL.: ""Phase and morphological transitions of titania/titanate nanostructures from an acid to an alkali hydrothermal environment"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| LIANG SHI ET AL.: ""Facile fabrication of hierarchical BiVO4/TiO2 heterostructures for enhanced photocatalytic activities under visible-light irradiation"", 《JOURNAL OF MATERIALS SCIENCE》 * |
| SHUYUN WANG ET AL.: ""Visible Light-Driven BiVO4/TiO2 Composite Photocatalysts: Preparation Methods and Photocatalytic Performance"", 《AUSTRALIAN JOURNAL OF CHEMISTRY》 * |
| 焦艳超等: "" 板钛矿与锐钛矿混晶及其光催化性能"", 《 第六届全国环境化学大会暨环境科学仪器与分析仪器展览会摘要集》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479752A (en) * | 2018-04-26 | 2018-09-04 | 青岛科技大学 | A kind of BiVO of two dimension carbon-coating load4/TiO2The preparation method of heterogeneous visible light catalyst |
| CN108479752B (en) * | 2018-04-26 | 2021-04-06 | 青岛科技大学 | BiVO loaded by two-dimensional carbon layer4/TiO2Preparation method of heterogeneous visible light catalyst |
| CN109603809A (en) * | 2019-01-25 | 2019-04-12 | 泉州师范学院 | A kind of preparation and application of pucherite quantum dot and titanium dioxide nano-belts composite photo-catalyst |
| CN110026170A (en) * | 2019-05-23 | 2019-07-19 | 乐山师范学院 | A kind of TiO of photocatalytic degradation rhodamine B2Photochemical catalyst and preparation method thereof |
| CN110026170B (en) * | 2019-05-23 | 2022-07-08 | 乐山师范学院 | TiO for degrading rhodamine B through photocatalysis2Photocatalyst and preparation method thereof |
| CN111229206A (en) * | 2020-02-25 | 2020-06-05 | 南开大学 | Preparation method and application of heterojunction visible-light-driven photocatalyst |
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