CN106994349A - A kind of Preparation method and use of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy - Google Patents
A kind of Preparation method and use of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy Download PDFInfo
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- CN106994349A CN106994349A CN201710329556.9A CN201710329556A CN106994349A CN 106994349 A CN106994349 A CN 106994349A CN 201710329556 A CN201710329556 A CN 201710329556A CN 106994349 A CN106994349 A CN 106994349A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 11
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 11
- JCDAAXRCMMPNBO-UHFFFAOYSA-N iron(3+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Ti+4].[Fe+3].[Fe+3] JCDAAXRCMMPNBO-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 12
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 61
- 238000003756 stirring Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 18
- 238000013019 agitation Methods 0.000 claims description 16
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- RDQSSKKUSGYZQB-UHFFFAOYSA-N bismuthanylidyneiron Chemical compound [Fe].[Bi] RDQSSKKUSGYZQB-UHFFFAOYSA-N 0.000 claims description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 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 description 8
- 238000001035 drying Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- 238000007710 freezing Methods 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 230000003115 biocidal effect Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 230000003111 delayed effect Effects 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 238000009415 formwork Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000002835 absorbance Methods 0.000 abstract description 2
- 239000002585 base Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 230000001052 transient effect Effects 0.000 abstract 1
- 239000002057 nanoflower Substances 0.000 description 12
- 239000000523 sample Substances 0.000 description 8
- 229910052738 indium Inorganic materials 0.000 description 7
- 239000004098 Tetracycline Substances 0.000 description 6
- 238000001338 self-assembly Methods 0.000 description 6
- 229960002180 tetracycline Drugs 0.000 description 6
- 229930101283 tetracycline Natural products 0.000 description 6
- 235000019364 tetracycline Nutrition 0.000 description 6
- 150000003522 tetracyclines Chemical class 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 229910003256 NaTaO3 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- -1 load cocatalyst Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- 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)
- Catalysts (AREA)
- Compounds Of Iron (AREA)
Abstract
The present invention relates to a kind of Preparation method and use of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy, this method utilizes a step hydrothermal synthesis method, the regulation and control of material dimension and band gap are carried out by finely tuning reaction acid or alkali environment in synthesis, with it is common prepare the preparation method of visible light activity material of hierarchy compared with, present invention gained Bi5FeTi3O15Catalyst is without cumbersome grinding, addition organic formwork agent, high-temperature calcination and without in the case of transient metal doped, only realize that the dimension of material regulates and controls, obtains the excellent pattern of the fine setting imparting material of reaction environment in even size distribution, building-up process by simply finely tuning reaction acid-base value, it is to avoid the introducing for the magazine that organic formwork is brought.The material Bi of hierarchy obtained by the present invention5FeTi3O15Show high-end visible light photocatalysis.The method of the invention operating procedure is simple, mild condition, cost are low, and without organic plank is introduced, gained photochemical catalyst has dimension adjustable, it is seen that the advantages of absorbance is strong.
Description
Technical field
The invention belongs to photocatalysis nano material preparing technical field, and in particular to the visible light photocatalysis material of hierarchy
Expect Bi5FeTi3O15Preparation method and use.
Background technology
Energy and environment problem is two huge challenges that the world today is faced, and effectively solves the two issue concerns and arrives
Can the whole mankind realize sustainable development.Therefore, development cleaning effective as selective depollution of environment technology turns into current international ring
Border field most hot issue in the urgent need to address.With the development of solar utilization technique, with Driven by Solar Energy organic synthesis
Process, will be expected to substitute traditional thermocatalytic technology, so as to realize the Chemical Manufacture of low energy consumption., will too in the technological approaches
Sun, which can be converted, saves as chemical energy, and a kind of new thinking is provided for the current energy dilemmas of alleviation.From Fujishima in 1972
Deng discovery monocrystalline TiO first2Can be after photochemical catalyzing on electrode, conductor photocatalysis is rapidly by various countries' environment and the energy
The common concern of researcher.But pass through and extensively and profoundly study for more than 30 years, photocatalysis technology is with being still difficult to high efficiency low cost
Convert and utilize solar energy.Main cause is a series of wide band gap semiconducter photochemical catalyst such as TiO of people's exploitation2、NaTaO3
Deng only having response in ultraviolet light range.Compared with noble metal catalyst, metal oxide has the advantages that low cost, and can open up
Reveal photocatalytic activity, be the preferable solar energy catalysis material of a class.
Researcher can be by many means (such as building heterojunction semiconductor, load cocatalyst, semiconductor doping
Deng) utilization of photo-generated carrier is improved, and then improve its utilization ratio to solar energy.However, conductor photocatalysis molecule
Activation need consider two problems：1) level-density parameter problem；2) problem of transmission of carrier.When photocatalysis is oxygen activating
Consider the conduction band and O of semiconductor2Match condition between reduction potential；Also to consider simultaneously, whether carrier can be from half
Conductor is delivered to O2Molecule gets on.In order to break through this limitation, it is necessary to can be systematic same to develop a kind of new strategy
When modification band gap and valence band conduction band energy level.Meanwhile, the microstructure of material is regulated and controled to increase and utilize its surface and interface
Characteristic, so that the application for increasing sunshine is also an effective way for being effectively increased efficiency.
In the recent period, control synthesis condition and method to synthesize by adding organic plank and surfactant and carry out material dimension
Regulation and control, as an effective method reduce possible environmental problem in visible light catalytic reaction.These synthesis techniques
Synthesis condition is cumbersome, and high energy consumption, multi-step, equipment are expensive, and the template used in these synthetic methods is easily introduced impurity,
It is easy to oxidizing in practical application, hardly results in the stable and uniform grading structure material of fractions distribution, therefore at these
Method receives certain limitation in actual applications.
The content of the invention
Present invention aims at there is provided a kind of preparation method of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy
And purposes, this method utilizes a step hydrothermal synthesis method, by finely tuning reaction acid or alkali environment progress material dimension and band in synthesis
The regulation and control of gap, with it is common prepare the preparation method of visible light activity material of hierarchy compared with, present invention gained
Bi5FeTi3O15Catalyst without cumbersome grinding, add organic formwork agent, high-temperature calcination and mixed without transition metal
In the case of miscellaneous, only realize that the dimension of material regulates and controls by simply finely tuning reaction acid-base value, obtain even size distribution, synthesis
During the fine setting of reaction environment assign material excellent pattern, it is to avoid the introducing for the magazine that organic formwork is brought.Institute of the present invention
The material Bi of the hierarchy obtained5FeTi3O15Show high-end visible light photocatalysis.The letter of the method for the invention operating procedure
List, mild condition, cost are low, and without organic plank is introduced, gained photochemical catalyst has dimension adjustable, it is seen that absorbance is strong etc.
Advantage.
A kind of preparation method of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy of the present invention, this method
Using a step hydrothermal synthesis method, the regulation and control of material dimension and band gap are carried out by finely tuning reaction acid or alkali environment in synthesis, specifically
Operation follows these steps to carry out：
A, according to mol ratio by 0.005mol bismuth nitrates, 1.0mmoL ferric nitrate and 0.003mol butyl titanate essence
Really weigh and be dissolved in the water containing 5mL nitric acid, magnetic agitation 30min, the mixture for being uniformly mixed and being completely dissolved；
0.1mol/L sodium hydrate aqueous solution, and strong agitation 10min are added in b, the mixture for obtaining step a,
Sodium hydroxide solution is slowly dropped into, continues to stir 40min, obtains uniform yellow suspension, it is accurate with hydrochloric acid or sodium hydroxide
Its pH value is adjusted to 7.0-14.0, continuing stirring 5h ensures that reaction is uniform；
C, the suspension for obtaining step b are slowly moved into the 23mL interior kettle lining of tetrafluoroethene reaction, are placed on baking oven
In, in 160 DEG C of temperature, 15h is reacted, then 100 DEG C of temperature is down to 5 DEG C/min of temperature, then it is down to room temperature with 3 DEG C/min of temperature；
D, the reacted products of step c are centrifuged, take sample to stir 1h in the beaker of 400mL water in filling, stand 30min
Particle is all sunk, slowly outwell supernatant, continue to stir with 100mL absolute ethyl alcohols and 400mL water, repeat 7-
8 times, then cleaned 3 times with deionized water, it is placed in vacuum freezing drying oven and dries 10h, it is finely ground, that is, obtain metatitanic acid containing target product
Iron bismuth Bi5FeTi3O15。
The visible light catalyst iron titanate bismuth Bi that the preparation method is obtained5FeTi3O15Degraded in the case where preparing visible ray anti-
Purposes in raw element.
A kind of Preparation method and use of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy of the present invention,
It this method propose a kind of simple, method for efficiently synthesizing photochemical catalyst.Bi when finely tuning pH value5FeTi3O15Show by nanometer
To nanometer sheet, nanometer rods ultimately form the forming process of the self assembly of nano flower, and material has strong visible absorption.This
Invention methods described can not only realize that material morphology regulates and controls, it is often more important that, the surface characteristic of material can be changed, can band knot
Structure.Under visible light can efficiently, quickly be used for antibiotic degraded, degradation efficiency be better than P25.It is special based on material layer structure
Levy, the photochemical catalyst characteristic of the regulation and control of dimension and efficient stable, method proposed by the present invention is explores the active material of novel visible
Effectively and easily method and thinking are found in material offer, and open up a Tiao Xin roads for the synthesis of other perovskite nano materials,
It can be promoted in environment, the development of Material Field simultaneously.
The stratiform of the hierarchy for the visible light activity that described the inventive method is obtained is evaluated by probe molecule of antibiotic
Perovskite photochemical catalyst iron titanate bismuth Bi5FeTi3O15Under visible light degrade drug contamination thing purposes.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of the present invention, wherein (a) is granule-morphology, (b) is nanometer rods and particle
The mixing pattern of composition, (c) is nanometer rods pattern, and (d) is nanometer sheet pattern, and (e) is nano flower pattern, and (f) is hierarchy
Nano flower pattern photochemical catalyst Bi5FeTi3O15Scanning electron microscope (SEM) photograph；Material morphology controlledly synthesis is realized, passes through scanning
Electron microscope picture can be seen that synthetic material is shown by nanometer to nanometer sheet, nanometer rods ultimately form nano flower from group
The forming process of dress；
Fig. 2 a be sem test of the present invention in observe microstructure change, wherein (a) be nano particle pattern,
(b) it is nanometer rods and a little nano particle pattern, (c) is nanometer sheet pattern, and (d) is the chain that nanometer sheet is constituted, (e) nanometer sheet
Self assembly, the nanometer sheet surface of (f) self assembly, the nano flower pattern of (g) self assembly composition, flower of (h) nano flower surface from volume
Valve, (i) is the nano flower pattern of hierarchy；
Fig. 2 b are the forming process schematic diagram of the present invention, realize material by fine setting reaction acid or alkali environment and show by receiving
Rice arrives nanometer sheet, and nanometer rods ultimately form the forming process of the self assembly of nano flower；
Fig. 3 is the level structure schematic diagram of synthetic material of the present invention, wherein (1) is nano particle pattern, (2) are nanometer rods
With a little nano particle pattern, (3) be nanometer sheet pattern, (4) self assembly composition nano flower pattern, (5) nano flower surface from
The petal of volume, (6) are the band gap diagram of the nano flower of hierarchy；
Fig. 4 is final degraded effect of the antibiotic of the present invention (tetracycline) under different-shape catalyst and xenon lamp irradiation
Rate comparison diagram, wherein (1) is without catalyst, (2) are no illumination, and (3) are commercialized titanium dioxide P25, and (4) are nanometer rods
The photochemical catalyst of pattern, the photochemical catalyst of (5) nano particle pattern, the photochemical catalyst of (6) nanometer sheet pattern and (7) classification knot
Degraded change in concentration under the photochemical catalyst catalytic action of the nano flower pattern of structure, wherein catalyst amount are 40mg, tetracycline
Concentration 1 × 10-5mol/L。
Embodiment
The present embodiment is lower premised on technical solution of the present invention to be implemented, and gives detailed embodiment and specific
Operating process, but the present invention is not limited only to following embodiments：
Embodiment 1
A, in molar ratio by 0.005mol bismuth nitrates 2.3298g, 1.0mmoL ferric nitrate 0.1596g and 0.003mol
Butyl titanate accurate weighing is simultaneously dissolved in the water containing 5mL nitric acid, and magnetic agitation about 30min is uniformly mixed and complete
The mixture of fully dissolved；
0.1mol/L sodium hydrate aqueous solution, and strong agitation 10min are added in b, the mixture for obtaining step a,
Sodium hydroxide solution is slowly dropped into again, is continued to stir 40min, is obtained uniform yellow suspension, its pH value is accurately adjusted with hydrochloric acid
To 7.0, continuing stirring 5h ensures that reaction is uniform；
C, the suspension for obtaining step b are slowly moved into the 23mL interior kettle lining of tetrafluoroethene reaction, are placed on baking oven
In, in 160 DEG C of temperature, 15h is reacted, 100 DEG C of temperature is down to 5 DEG C/min of temperature, then room temperature is down to 3 DEG C/min of temperature；
D, the reacted products of step c are centrifuged, take sample to stir 1h in the beaker of 400mL water in filling, stand 30min
Particle is all sunk, slowly outwell supernatant, continue to stir with 100mL absolute ethyl alcohols and 400mL water, repeat 7-
8 times, then cleaned 3 times with deionized water, it is placed in vacuum freezing drying oven and dries 10h, it is finely ground, that is, obtain metatitanic acid containing target product
Iron bismuth Bi5FeTi3O15。
Embodiment 2
A, in molar ratio by 0.005mol bismuth nitrates 2.3298g, 1.0mmoL ferric nitrate 0.1596g and 0.003mol
Butyl titanate accurate weighing is simultaneously dissolved in the water containing 5mL nitric acid, and magnetic agitation about 30min is uniformly mixed and complete
The mixture of fully dissolved；
0.1mol/L sodium hydrate aqueous solution, and strong agitation 10min are added in b, the mixture for obtaining step a,
Sodium hydroxide solution is slowly dropped into again, is continued to stir 40min, is obtained uniform yellow suspension, it is accurately adjusted with sodium hydroxide
PH value is to 9.0, and continuing stirring 5h ensures that reaction is uniform；
C, the suspension for obtaining step b are slowly moved into the 23mL interior kettle lining of tetrafluoroethene reaction, are placed on baking oven
In, in 160 DEG C of temperature, 15h is reacted, 100 DEG C of temperature is down to 5 DEG C/min of temperature, then room temperature is down to 3 DEG C/min of temperature；
D, the reacted products of step c are centrifuged, take sample to stir 1h in the beaker of 400mL water in filling, stand 30min
Particle is all sunk, slowly outwell supernatant, continue to stir with 100mL absolute ethyl alcohols and 400mL water, repeat 7-
8 times, then cleaned 3 times with deionized water, it is placed in vacuum freezing drying oven and dries 10h, it is finely ground, that is, obtain metatitanic acid containing target product
Iron bismuth Bi5FeTi3O15。
Embodiment 3
A, in molar ratio by 0.005mol bismuth nitrates 2.3298g, 1.0mmoL ferric nitrate 0.1596g and 0.003mol
Butyl titanate accurate weighing is simultaneously dissolved in the water containing 5mL nitric acid, and magnetic agitation about 30min is uniformly mixed and complete
The mixture of fully dissolved；
0.1mol/L sodium hydrate aqueous solution, and strong agitation 10min are added in b, the mixture for obtaining step a,
Sodium hydroxide solution is slowly dropped into, continues to stir 40min, obtains uniform yellow suspension；Its pH is accurately adjusted with sodium hydroxide
Value is to 10.0, and continuing stirring 5h ensures that reaction is uniform；
C, the suspension for obtaining step b are slowly moved into the 23mL interior kettle lining of tetrafluoroethene reaction, are placed on baking oven
In, in 160 DEG C of temperature, 15h is reacted, then 100 DEG C of temperature is down to 5 DEG C/min of temperature, then it is down to room temperature with 3 DEG C/min of temperature；
D, the reacted products of step c are centrifuged, take sample to stir 1h in the beaker of 400mL water in filling, stand 30min
Particle is all sunk, slowly outwell supernatant, continue to stir with 100mL absolute ethyl alcohols and 400mL water, repeat 7-
8 times, then cleaned 3 times with deionized water, it is placed in vacuum freezing drying oven and dries 10h, it is finely ground, that is, obtain metatitanic acid containing target product
Iron bismuth Bi5FeTi3O15。
Embodiment 4
A, in molar ratio by 0.005mol bismuth nitrates 2.3298g, 1.0mmoL ferric nitrate 0.1596g and 0.003mol
Butyl titanate accurate weighing is simultaneously dissolved in the water containing 5mL nitric acid, and magnetic agitation about 30min is uniformly mixed and complete
The mixture of fully dissolved；
0.1mol/L sodium hydrate aqueous solution, and strong agitation 10min are added in b, the mixture for obtaining step a,
Sodium hydroxide solution is slowly dropped into, continues to stir 40min, obtains uniform yellow suspension；Its pH is accurately adjusted with sodium hydroxide
Value is to 11.0, and continuing stirring 5h ensures that reaction is uniform；
C, the suspension for obtaining step b are slowly moved into the 23mL interior kettle lining of tetrafluoroethene reaction, are placed on baking oven
In, in 160 DEG C of temperature, 15h is reacted, then 100 DEG C of temperature is down to 5 DEG C/min of temperature, then be down to 3 DEG C/min of temperature to room
Temperature；
D, the reacted products of step c are centrifuged, take sample to stir 1h in the beaker of 400mL water in filling, stand 30min
Particle is all sunk, slowly outwell supernatant, continue to stir with 100mL absolute ethyl alcohols and 400mL water, repeat 7-
8 times, then cleaned 3 times with deionized water, it is placed in vacuum freezing drying oven and dries 10h, it is finely ground, that is, obtain metatitanic acid containing target product
Iron bismuth Bi5FeTi3O15。
Embodiment 5
A, in molar ratio by 0.005mol bismuth nitrates 2.3298g, 1.0mmoL ferric nitrate 0.1596g and 0.003mol
Butyl titanate accurate weighing is simultaneously dissolved in the water containing 5mL nitric acid, and magnetic agitation about 30min is uniformly mixed and complete
The mixture of fully dissolved；
0.1mol/L sodium hydrate aqueous solution, and strong agitation 10min are added in b, the mixture for obtaining step a,
Sodium hydroxide solution is slowly dropped into, continues to stir 40min, obtains uniform yellow suspension, its pH is accurately adjusted with sodium hydroxide
Value is to 12.0, and continuing stirring 5h ensures that reaction is uniform；
C, the suspension for obtaining step b are slowly moved into the 23mL interior kettle lining of tetrafluoroethene reaction, are placed on baking oven
In, in 160 DEG C of temperature, 15h is reacted, then 100 DEG C of temperature is down to 5 DEG C/min of temperature, then it is down to room temperature with 3 DEG C/min of temperature；
D, the reacted products of step c are centrifuged, take sample to stir 1h in the beaker of 400mL water in filling, stand 30min
Particle is all sunk, slowly outwell supernatant, continue to stir with 100mL absolute ethyl alcohols and 400mL water, repeat 7-
8 times, then cleaned 3 times with deionized water, it is placed in vacuum freezing drying oven and dries 10h, it is finely ground to obtain metatitanic acid containing target product
Iron bismuth Bi5FeTi3O15。
Embodiment 6
A, in molar ratio by 0.005mol bismuth nitrates 2.3298g, 1.0mmoL ferric nitrate 0.1596g and 0.003mol
Butyl titanate accurate weighing is simultaneously dissolved in the water containing 5mL nitric acid, and magnetic agitation about 30min is uniformly mixed and complete
The mixture of fully dissolved；
0.1mol/L sodium hydrate aqueous solution, and strong agitation 10min are added in b, the mixture for obtaining step a,
Sodium hydroxide solution is slowly dropped into again, is continued to stir 40min, is obtained uniform yellow suspension, it is accurately adjusted with sodium hydroxide
PH value is to 14.0, and continuing stirring 5h ensures that reaction is uniform；
C, the suspension for obtaining step b are slowly moved into the 23mL interior kettle lining of tetrafluoroethene reaction, are placed on baking oven
In, in 160 DEG C of temperature, 15h is reacted, then 100 DEG C of temperature is down to 5 DEG C/min of temperature, then it is down to room temperature with 3 DEG C/min of temperature；
D, the reacted products of step c are centrifuged, take sample to stir 1h in the beaker of 400mL water in filling, stand 30min
Particle is all sunk, slowly outwell supernatant, continue to stir with 100mL absolute ethyl alcohols and 400mL water, repeat 7-
8 times, then cleaned 3 times with deionized water, it is placed in vacuum freezing drying oven and dries 10h, it is finely ground to obtain metatitanic acid containing target product
Iron bismuth Bi5FeTi3O15。
Embodiment 7
The target product iron titanate bismuth Bi for taking commercialized titanium dioxide P25 and embodiment 1-6 to prepare5FeTi3O15Respectively
40mg, it is 1 × 10 that 100mL concentration is dispersed in respectively-5In mol/L tetracycline, masking foil is wrapped, lucifuge absorption
30min, the 300W xenon lamps for being 420nm with wavelength carry out radiation of visible light, carry out Visible Light Induced Photocatalytic, every equal time interval
3mL is sampled, is filtered after centrifugation with 0.45 μm of filter membrane, by its clear liquid in high performance liquid chromatography, the concentration of tetracycline is detected
Change, test result shows that target product is significantly higher than P25 pairs to the degradation rate of tetracycline almost close to 98% in 30min
The degradation efficiency of tetracycline is shown in Fig. 4.
Claims (2)
1. the preparation method of the laminated perovskite photochemical catalyst iron titanate bismuth of a kind of hierarchy, it is characterised in that this method is utilized
One step hydrothermal synthesis method, carries out the regulation and control of material dimension and band gap, concrete operations in synthesis by finely tuning reaction acid or alkali environment
Follow these steps to carry out：
A, in molar ratio by 0.005 mol bismuth nitrates, 1.0 mmoL ferric nitrate and 0.003 mol butyl titanate accurately claim
Measure and be dissolved in the aqueous solution containing 5 mL nitric acid, the min of magnetic agitation 30, the mixing for being uniformly mixed and being completely dissolved
Thing；
0.1 mol/L sodium hydrate aqueous solution, and the min of strong agitation 10 are added in b, the mixture for obtaining step a, is delayed
It is slow to instill sodium hydroxide solution, continue to stir 40 min, obtain uniform yellow suspension, accurately adjusted with hydrochloric acid or sodium hydroxide
Its pH value is to 7.0 14.0, and continuing 5 h of stirring ensures that reaction is uniform；
C. suspension step b obtained is slowly moved into the 23 mL interior kettle lining of tetrafluoroethene reaction, is placed in baking oven,
In 160 DEG C of temperature, 15 h are reacted, then 100 DEG C of temperature is down to 5 DEG C/min of temperature, then room temperature is down to 3 DEG C/min of temperature；
D. the reacted products of step c are centrifuged, takes sample to stir 1 h in the beaker of 400 mL water in filling, stand 30 min
Particle is all sunk, slowly outwell supernatant, continue to stir with 100 mL absolute ethyl alcohols and 400 mL water, repeat
7-8 times, then cleaned 3 times with deionized water, it is placed in vacuum freezing drying oven and dries 10 h, it is finely ground, that is, obtain target product titanium
Sour iron bismuth Bi5FeTi3O15。
2. the visible light catalyst iron titanate bismuth that preparation method according to claim 1 is obtained is degraded in the case where preparing visible ray
Purposes in antibiotic.
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| CN109331831A (en) * | 2018-11-27 | 2019-02-15 | 青岛大学 | Efficient visible light catalyst single crystal nanoplate and preparation method thereof |
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