CN109331831A - Efficient visible light catalyst single crystal nanoplate and preparation method thereof - Google Patents
Efficient visible light catalyst single crystal nanoplate and preparation method thereof Download PDFInfo
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- CN109331831A CN109331831A CN201811422028.9A CN201811422028A CN109331831A CN 109331831 A CN109331831 A CN 109331831A CN 201811422028 A CN201811422028 A CN 201811422028A CN 109331831 A CN109331831 A CN 109331831A
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- 239000013078 crystal Substances 0.000 title claims abstract description 30
- 239000002055 nanoplate Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 86
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 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 abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 20
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000015556 catabolic process Effects 0.000 claims abstract description 18
- 238000006731 degradation reaction Methods 0.000 claims abstract description 18
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 230000001376 precipitating effect Effects 0.000 claims abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 18
- 239000012265 solid product Substances 0.000 claims description 18
- 229960004756 ethanol Drugs 0.000 claims description 17
- 238000013019 agitation Methods 0.000 claims description 12
- 239000002159 nanocrystal Substances 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 2
- 239000007850 fluorescent dye Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 24
- 238000005286 illumination Methods 0.000 abstract description 3
- 239000010936 titanium Substances 0.000 description 37
- 239000000463 material Substances 0.000 description 15
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 230000005621 ferroelectricity Effects 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 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 description 4
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000004847 absorption spectroscopy Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 229910002321 LaFeO3 Inorganic materials 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 241001198704 Aurivillius Species 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J23/8437—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
- 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
-
- B01J35/39—
-
- B01J35/40—
-
- 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
- C02F2101/308—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
Abstract
The invention discloses a kind of preparation methods of efficient visible light catalyst single crystal nanoplate, method includes the following steps: pressing Bi4Ti3O12‑BiCoO3The stoichiometric ratio of middle Bi, Co and Ti weigh bismuth nitrate, cobalt nitrate and butyl titanate；The weighed bismuth nitrate of step and cobalt nitrate are mixed into solution soluble in water, are added the ethanol solution of the weighed butyl titanate of step into acquired solution, stirring is allowed to uniformly mixed solution A；Using NaOH as precipitating reagent and water environment regulator, NaOH is soluble in water that solution A is added in solution B, solution B, and stirring obtains the suspension presoma of celadon after complete reaction；Suspension presoma is transferred in hydrothermal reaction kettle, by reaction kettle it is closed after be put into baking oven, 48~72h of hydro-thermal reaction at 200 DEG C, product obtains target product through subsequent processing after reaction.This method preparation process is simple, environmental-friendly, at low cost, it can be achieved that scale is synthetically produced, which being capable of rapidly and efficiently rhodamine B degradation under visible light illumination.
Description
Technical field
The present invention relates to photocatalysis technology fields, and in particular to efficient visible light catalyst single crystal nanoplate and its preparation side
Method.
Background technique
Visible light catalytic technology is received significant attention because of the great potential in terms of solar energy conversion and the depollution of environment.From
From discovery TiO2It can be applied to contaminant degradation with potential photocatalytic, researchers have attempted various methods to improve it
Photocatalysis performance.However, being limited to two main disadvantages: visible light utilization efficiency is low and photo-generate electron-hole recombination rate is high,
TiO2Still the efficient utilization difficult to realize to visible light.Therefore, researcher, which is absorbed in seek, other has more preferable photocatalysis
Active semiconductor.
Ferroelectric material has the characteristics such as excellent ferroelectricity, photoelectricity in non-volatile ferroelectric memory, photocatalysis and photoelectric conversion
Etc. have tempting application prospect.Relative to traditional semiconductor material, there are natural built in field inside ferroelectric material,
Photoinduced electron-hole pair, photocatalytic pollutant degradation ability with higher and sun light conversion efficiency, and light can be efficiently separated
Open-circuit voltage is caused to be apparently higher than traditional semiconductor material, by material in terms of photocatalytic pollutant degradation, solar energy
Expect the very big concern of scientist.The sections electric material of laminated perovskite containing Bi is a kind of important functional material, has Curie temperature
The advantages that height, spontaneous polarization is big.Wherein, Bi4Ti3O12It is a kind of typical bismuth system laminated perovskite ferroelectric material, structure is
By pseudo- calcium titanium ore bed and (Bi2O2)2+Along c-axis direction, alternating stacking is formed.Bi4Ti3O12Curie temperature be 675 DEG C, be in ferroelectricity
Its spontaneous polarization value is up to 50 μ C/cm when phase2, information storage, the depollution of environment, in terms of have wide application before
Scape.Bi4Ti3O12It is a kind of typical Aurivillius oxide semiconductor, optical band gap (Eg=2.8eV) compare TiO2It is low
(Eg=3.2eV).Since there are TiO in its structure4Octahedra and three-dimensional active Bi3+Ion, it is as a kind of new and effective
Photochemical catalyst is widely studied in recent years.Related Bi at present4Ti3O12The research of based solid solution material is also seldom, and report
Photocatalytic degradation speed is slower, and the required time is longer.In addition, existing Bi4Ti3O12The preparation process of base single crystal nanoplate is more multiple
Miscellaneous, synthesis condition is harsher, is not suitable for industrial scale production, and the test-material yardstick of existing synthetic method preparation is big, pattern is not
Rule causes its photocatalysis performance to be affected.
Summary of the invention
The technical problem to be solved by the present invention is overcoming the shortage of prior art, efficient visible light catalyst monocrystalline is provided and is received
Rice piece and preparation method thereof.The preparation process of this method is simple, environmental-friendly, synthesis cost is low, and the scale of can be realized is combined to
Produce Bi4Ti3O12-BiCoO3Single crystal nanoplate, and single crystal nanoplate obtained by this method is with vis-absorbing well
Can, it can rapidly and efficiently rhodamine B degradation under visible light illumination.
To solve the above-mentioned problems, the present invention provides a kind of preparation sides of efficient visible light catalyst single crystal nanoplate
Method, comprising the following steps:
(1) Bi is pressed4Ti3O12-BiCoO3The stoichiometric ratio of middle Bi, Co and Ti weigh bismuth nitrate, cobalt nitrate and metatitanic acid fourth
Ester；
(2) the weighed bismuth nitrate of step (1) and cobalt nitrate are mixed into solution soluble in water, step is added into acquired solution
Suddenly the ethanol solution of (1) weighed butyl titanate, stirring are allowed to uniformly mixed solution A；
(3) using NaOH as precipitating reagent and water environment regulator, NaOH is soluble in water that solution B, solution B are added solution A, stir
Mix the suspension presoma for obtaining celadon after complete reaction；
(4) suspension presoma is transferred in hydrothermal reaction kettle, by reaction kettle it is closed after be put into baking oven, at 200 DEG C
48~72h of lower hydro-thermal reaction, cleans to obtain solid product with deionized water after product is filtered, separated after reaction；
(5) step (4) obtained solid product drying obtains target product.
Preferably, step (2) are as follows: step (1) weighed butyl titanate is dissolved in dehydrated alcohol and obtains the anhydrous second of butyl titanate
The weighed bismuth nitrate of step (1), cobalt nitrate mixing are dissolved in distilled water and obtain solution, slowly dripped into acquired solution by alcoholic solution
Add butyl titanate ethanol solution, stirring 30min obtains solution A.
Preferably, step (3) are as follows: weigh suitable NaOH, NaOH is dissolved in deionized water and obtains solution B, solution B is slow
It is added dropwise in solution A and obtains mixed solution, stirring 2h obtains the suspension presoma of celadon, and it is heavy that the total amount of the NaOH of addition meets
Forming sediment after being precipitated completely, NaOH concentration is 1mol/L in mixed solution.
Preferably, step (5) are as follows: step (4) obtained solid product obtains target product through 80 DEG C of dry 12h.
Preferably, the preparation method the following steps are included:
(1) Bi is pressed4Ti3O12-BiCoO3The stoichiometric ratio of middle Bi, Co and Ti weigh 2.4499g bismuth nitrate, 0.2954g nitre
Sour cobalt and 1.0314g butyl titanate；
(2) step (1) weighed butyl titanate is dissolved in 10mL dehydrated alcohol and obtains butyl titanate ethanol solution, will walk
Suddenly (1) weighed bismuth nitrate and cobalt nitrate, which mix to be dissolved in 20mL deionized water at room temperature, obtains solution, dropwise into acquired solution
Butyl titanate ethanol solution is added, magnetic agitation 30min obtains solution A at room temperature；
(3) NaOH 2.0000g is weighed, is dissolved in 10mL deionized water, obtains solution B, solution B is slowly dropped to molten
In liquid A, magnetic agitation 2h obtains the suspension presoma of celadon；
(4) 30ml suspension presoma is taken to be transferred in hydrothermal reaction kettle, by reaction kettle it is closed after be put into baking oven,
Hydro-thermal reaction 72h at 200 DEG C is cleaned 5 times after solid product is filtered, separated after reaction with deionized water；
(5) step (4) obtained solid product obtains target product through 80 DEG C of dry 12h.
The invention also discloses the efficient visible light catalyst single crystal nanoplates as made from above-mentioned preparation method, and described receives
Rice single-chip is Bi4Ti3O12-BiCoO3Nanometer chip, the single crystal nanoplate can irradiate lower degradation rhodamine under visible light
B fluorescent dye.
Preferably, under the nano crystal piece irradiates under visible light, to the degradation rate of rhodamine B up to needed for 95%
Time is 15min.
The beneficial effects of the present invention are: providing efficient visible light catalyst single crystal nanoplate and preparation method thereof.The system
The preparation process of Preparation Method is simple, environmental-friendly, synthesis cost is low, can be realized scale and is synthetically produced Bi4Ti3O12-BiCoO3
Single crystal nanoplate, and single crystal nanoplate obtained by this method has good visible absorption performance, it can be in radiation of visible light
Under rapidly and efficiently rhodamine B degradation.Specifically:
Bi4Ti3O12It is a kind of ideal basis material, in Bi4Ti3O12Lattice in be inserted into narrow band gap BiCoO3Unit
Afterwards, it can get new and effective Bi4Ti3O12-BiCoO3Visible light catalytic material.Bi4Ti3O12-BiCoO3It shows excellent visible
The inherent mechanism of photocatalytic activity is: on the one hand, Bi4Ti3O12Middle Bi6s track and O2p have strong interaction, to drop
The low symmetry of system, and then relevant dipole is generated, these dipoles facilitate photoinduced electron-hole point in system
From making it have higher oxidation activity；On the other hand, Bi4Ti3O12-BiCoO3In introduce Co3d track, increase light swash
Generate electricity subnumber, reduces the forbidden bandwidth of system, enhances its visible light absorption capacity, improves its visible light catalysis activity.
In field of material preparation or Industrial Catalysis field, stablized with simple method composite structure, the catalysis material of function admirable
The always target pursued of scientists.The synthesis of single crystal nanoplate is there are many method, including solid phase method, sol-gal process, has
Machine coprecipitation, microwave method, method of electrostatic spinning etc., most of these methods need hot environment, pollute environment, some methods
It is very high to equipment requirement, it is difficult to realize industrialization large-scale production.On the other hand, the single crystal nanoplate ruler prepared by these methods
Very little big, pattern is irregular, its photoelectrochemical behaviour is caused to be affected, and limits its practical application.The present invention uses hydro-thermal for the first time
Method has successfully synthesized Bi4Ti3O12-BiCoO3Single crystal nanoplate, synthesizes that the material required temperature is low, and preparation process is simple, synthesis
It is at low cost, industrialization large-scale production may be implemented, be not necessarily to add any template in synthesis process, environmental-friendly, material shape
Looks dimensionally stable is controllable, has good visible light absorption, can rapidly and efficiently rhodamine B degradation is glimmering under visible light illumination
Photoinitiator dye.It is tested through experiment, single crystal nanoplate of the invention is reacted with rhodamine B solution can be in 15min to the drop of rhodamine B
Solution rate reaches 95%.
Detailed description of the invention
Fig. 1: the XRD spectrum for the nano crystal piece sample that step (4) differential responses time (48h, 60h, 72h) is obtained；
Fig. 2: the scanning electron microscopic picture of 1 gained nano crystal piece of embodiment；
Fig. 3: the UV, visible light for the nano crystal piece sample that step (4) differential responses time (48h, 60h, 72h) is obtained is inhaled
Receive spectrum；
Fig. 4: the scanning electron microscopic picture of 2 gained nano crystal piece of embodiment；
Fig. 5: the scanning electron microscopic picture of 3 gained nano crystal piece of embodiment；
Fig. 6: the visible absorption spectrum figure of the nano crystal piece sample degradation rhodamine B solution of embodiment 3；
Fig. 7: the visible absorption spectrum figure of comparative example rhodamine B degradation solution.
Specific embodiment
In order to clarify the technical characteristics of the invention, being illustrated below by embodiment to this programme.
Embodiment 1
A kind of preparation method of efficient visible light catalyst single crystal nanoplate, comprising the following steps:
(1) Bi is pressed4Ti3O12-BiCoO3The stoichiometric ratio of middle Bi, Co and Ti weigh 2.4499g bismuth nitrate, 0.2954g nitre
Sour cobalt and 1.0314g butyl titanate；
(2) step (1) weighed butyl titanate is dissolved in 10mL dehydrated alcohol and obtains butyl titanate ethanol solution, by step
(1) weighed bismuth nitrate and cobalt nitrate mix at room temperature is dissolved in 20mL deionized water, and titanium is added dropwise into acquired solution
Acid butyl ester ethanol solution, magnetic agitation 30min obtains solution A at room temperature；
(3) NaOH 2.0000g is weighed, is dissolved in 10mL deionized water, obtains solution B, solution B is slowly dropped to molten
In liquid A, magnetic agitation 2h obtains the suspension presoma of celadon；
(4) 30ml suspension presoma is taken to be transferred in hydrothermal reaction kettle, by reaction kettle it is closed after be put into baking oven,
200 DEG C of progress hydro-thermal reaction 48h, are cleaned 5 times after solid product is filtered, separated after reaction with deionized water；
(5) step (4) obtained solid product obtains target product through 80 DEG C of dry 12h.
Performance test: Bi prepared by the above method4Ti3O12-BiCoO3The X ray diffracting spectrum of powder sample such as Fig. 1
Shown in (48h), the diffraction maximum of the sample can be corresponding with the diffraction maximum in standard diffraction card PDF 82-0063, it was demonstrated that
BiCoO3Group enters ferroelectricity Bi4Ti3O12Lattice among.Weak diffraction maximum in diffracting spectrum near 2 θ=38 ° derives from
Co2O3, illustrate to contain a small amount of Co in gained sample2O3.Fig. 2 is the scanning electron microscopic picture of the sample, the results showed that its pattern is piece
Shape.Fig. 3 (48h) is the ultraviolet-visible absorption spectroscopy figure and its band gap diagram of product, its forbidden bandwidth is 2.47eV as the result is shown,
Illustrate that visible light can be absorbed in it.
Embodiment 2
A kind of preparation method of efficient visible light catalyst single crystal nanoplate, comprising the following steps:
(1) Bi is pressed4Ti3O12-BiCoO3The stoichiometric ratio of middle Bi, Co and Ti weigh 2.4499g bismuth nitrate, 0.2954g nitre
Sour cobalt and 1.0314g butyl titanate；
(2) step (1) weighed butyl titanate is dissolved in 10mL dehydrated alcohol and obtains butyl titanate ethanol solution, by step
(1) weighed bismuth nitrate and cobalt nitrate mix mixing at room temperature and are dissolved in 20mL deionized water obtaining solution, into acquired solution by
It is added dropwise to butyl titanate ethanol solution, magnetic agitation 30min obtains solution A at room temperature；
(3) NaOH 2.000g is weighed, is dissolved in 10mL deionized water, obtains solution B, solution B is slowly dropped to solution
In A, magnetic agitation 2h obtains the suspension presoma of celadon；
(4) 30ml suspension presoma is taken to be transferred in hydrothermal reaction kettle, by reaction kettle it is closed after be put into baking oven,
Hydro-thermal reaction 60h under the conditions of 200 DEG C is cleaned 5 times after solid product is filtered, separated after reaction with deionized water；
(5) step (4) obtained solid product obtains target product through the dry 12h of 80 DEG C of drying.
Performance test: Bi prepared by the above method4Ti3O12-BiCoO3The X ray diffracting spectrum of powder sample such as Fig. 1
Shown in (60h), the diffraction maximum of the sample can be corresponding with the diffraction maximum in standard diffraction card PDF 82-0063, it was demonstrated that
BiCoO3Group enters ferroelectricity Bi4Ti3O12Lattice among.Weak diffraction maximum in diffracting spectrum near 2 θ=38 ° derives from
Co2O3, illustrate to contain a small amount of Co in gained sample2O3.Fig. 4 is the scanning electron microscopic picture of the sample, the results showed that its pattern is piece
Shape.Fig. 3 (60h) is the ultraviolet-visible absorption spectroscopy figure and its band gap diagram of product, its forbidden bandwidth is 2.40eV as the result is shown,
Illustrate that it absorbs visible light ability enhancing.
Embodiment 3
A kind of preparation method of efficient visible light catalyst single crystal nanoplate, comprising the following steps:
(1) Bi is pressed4Ti3O12-BiCoO3The stoichiometric ratio of middle Bi, Co and Ti weigh 2.4499g bismuth nitrate, 0.2954g nitre
Sour cobalt and 1.0314g butyl titanate；
(2) step (1) weighed butyl titanate is dissolved in 10mL dehydrated alcohol and obtains butyl titanate ethanol solution, will walk
Suddenly (1) weighed bismuth nitrate and cobalt nitrate mixing are dissolved in 20mL deionized water and obtain solution, and titanium is added dropwise into acquired solution
Acid butyl ester ethanol solution, magnetic agitation 30min obtains solution A at room temperature；
(3) NaOH 2.0000g is weighed, is dissolved in 10mL deionized water, obtains solution B, solution B is slowly dropped to molten
In liquid A, magnetic agitation 2h obtains the suspension presoma of celadon；
(4) 30ml suspension presoma is taken to be transferred in hydrothermal reaction kettle, by reaction kettle it is closed after be put into baking oven,
Hydro-thermal reaction 72h is carried out at 200 DEG C, clear 5 times with deionized water after solid product is filtered, separated after reaction；
(5) step (4) obtained solid product obtains target product through 80 DEG C of dry 12h.
Performance test: Bi prepared by the above method4Ti3O12-BiCoO3The X ray diffracting spectrum of powder sample such as Fig. 1
Shown in (72h), whole diffraction maximums of the sample can be corresponding with the diffraction maximum in standard diffraction card PDF82-0063, it was demonstrated that
BiCoO3Group enters ferroelectricity Bi4Ti3O12Lattice among.Fig. 5 is the scanning electron microscopic picture of products therefrom, the results showed that its
Pattern is sheet.Fig. 3 (72h) is the ultraviolet-visible absorption spectroscopy figure and its band gap diagram of product, as the result is shown the band of the sample
Gap is 2.36eV, illustrates that visible light can be absorbed in it.Compared with product in embodiment 1,2, which absorbs the ability of visible light
It is stronger.
Rhodamine B degradation experiment: Fig. 6 is that the sample of embodiment 3 is degraded under the radiation of visible light that 800W halogen lamp provides
The photocatalytic degradation figure of rhodamine B, the results show that the rhodamine B solution of 5mg/L concentration is degraded 95% in 15min, it was demonstrated that
The sample has efficient visible light catalytic ability, can rapidly and efficiently rhodamine B degradation.
Comparative example
A kind of Bi4Ti3O12-LaFeO3The preparation method of single crystal nanoplate, comprising the following steps:
(1) Bi is pressed4Ti3O12-LaFeO3The stoichiometric ratio of middle Bi, La, Fe and Ti weigh 0.4102g ferric nitrate,
1.9599g bismuth nitrate, 0.3703g lanthanum nitrate and 1.0314g butyl titanate；
(2) step (1) weighed butyl titanate is dissolved in 10mL dehydrated alcohol and obtains butyl titanate ethanol solution, by step
(1) weighed bismuth nitrate, lanthanum nitrate and ferric nitrate, which mix to be dissolved in 20mL deionized water at room temperature, obtains solution, into acquired solution
Butyl titanate ethanol solution is added dropwise, under room temperature, magnetic agitation 30min obtains solution A；
(3) NaOH 2.000g is weighed, is dissolved in 10mL deionized water, obtains solution B, solution B is slowly dropped to solution
In A, magnetic agitation 2h obtains the suspension presoma of yellow；
(4) it takes 30ml suspension presoma to be transferred in hydrothermal reaction kettle, reaction kettle is sealed in baking oven, 220
DEG C carry out hydro-thermal reaction 72h, the solid product cleaned after product is filtered, separated after reaction with deionized water；
(5) step (4) obtained solid product obtains target product through the dry 12h of 80 DEG C of drying.
Rhodamine B degradation experiment: Fig. 7 is that comparative example is degraded Luo Dan under the radiation of visible light that 800W halogen lamp provides
The curve graph of bright B, the experimental results showed that, the rhodamine B solution of 5mg/L concentration is degraded 95% in 180min, it was demonstrated that compares
The degradation time needed for embodiment 3, the sample degradation rhodamine B of comparative example is longer, illustrates sample of the invention compared to it
Its Bi4Ti3O12Base single crystal nanoplate has better absorbing properties, and photocatalytic degradation speed is faster.
Embodiment enumerated above is not to technical solution described in the invention only for understanding that the present invention is used
Restriction, the those of ordinary skill in relation to field on the basis of the technical solution described in claim, can also make a variety of changes
Change or deformation, all equivalent variations or deformation should all be covered within the scope of the claims of the present invention.The present invention is not
Place is described in detail, is the well-known technique of those skilled in the art of the present technique.
Claims (7)
1. a kind of preparation method of efficient visible light catalyst single crystal nanoplate, which comprises the following steps:
(1) Bi is pressed4Ti3O12-BiCoO3The stoichiometric ratio of middle Bi, Co and Ti weigh bismuth nitrate, cobalt nitrate and butyl titanate；
(2) the weighed bismuth nitrate of step (1) and cobalt nitrate are mixed into solution soluble in water, step is added into acquired solution
(1) ethanol solution of weighed butyl titanate, stirring are allowed to uniformly mixed solution A；
(3) using NaOH as precipitating reagent and water environment regulator, NaOH it is soluble in water solution B, solution B be added solution A, stirring to
The suspension presoma of celadon is obtained after fully reacting；
(4) suspension presoma is transferred in hydrothermal reaction kettle, by reaction kettle it is closed after be put into baking oven, be lauched at 200 DEG C
48~72h of thermal response cleans to obtain solid product with deionized water after product is filtered, separated after reaction；
(5) step (4) obtained solid product drying obtains target product.
2. the preparation method of efficient visible light catalyst single crystal nanoplate as described in claim 1, which is characterized in that step
(2) are as follows: step (1) weighed butyl titanate is dissolved in dehydrated alcohol and obtains butyl titanate ethanol solution, and step (1) is weighed
Bismuth nitrate, cobalt nitrate mixing are dissolved in distilled water and obtain solution, and butyl titanate ethanol solution is slowly added dropwise into acquired solution,
Stirring 30min obtains solution A.
3. the preparation method of efficient visible light catalyst single crystal nanoplate as described in claim 1, which is characterized in that step
(3) are as follows: weigh suitable NaOH, NaOH be dissolved in deionized water and obtains solution B, solution B be slowly added dropwise in solution A must mix it is molten
Liquid, stirring 2h obtain the suspension presoma of celadon, and the total amount of the NaOH of addition meets mixed solution after precipitating is precipitated completely
Middle NaOH concentration is 1mol/L.
4. the preparation method of efficient visible light catalyst single crystal nanoplate as described in claim 1, which is characterized in that step
(5) are as follows: step (4) obtained solid product obtains target product through 80 DEG C of dry 12h.
5. the preparation method of efficient visible light catalyst single crystal nanoplate as described in claim 1, which is characterized in that including with
Lower step:
(1) Bi is pressed4Ti3O12-BiCoO3The stoichiometric ratio of middle Bi, Co and Ti weigh 2.4499g bismuth nitrate, 0.2954g cobalt nitrate
With 1.0314g butyl titanate；
(2) step (1) weighed butyl titanate is dissolved in 10mL dehydrated alcohol and obtains butyl titanate ethanol solution, by step
(1) weighed bismuth nitrate and cobalt nitrate, which mix to be dissolved in 20mL deionized water at room temperature, obtains solution, adds dropwise into acquired solution
Enter butyl titanate ethanol solution, magnetic agitation 30min obtains solution A at room temperature；
(3) NaOH2.0000g is weighed, is dissolved in 10mL deionized water, obtains solution B, solution B is slowly dropped in solution A,
Magnetic agitation 2h obtains the suspension presoma of celadon；
(4) 30ml suspension presoma is taken to be transferred in hydrothermal reaction kettle, by reaction kettle it is closed after be put into baking oven, at 200 DEG C
Lower hydro-thermal reaction 72h is cleaned 5 times after solid product is filtered, separated after reaction with deionized water；
(5) step (4) obtained solid product obtains target product through 80 DEG C of dry 12h.
6. efficient visible light catalyst single crystal nanoplate, feature as made from any one preparation method in claim 1 to 5
It is, the nano crystal piece is Bi4Ti3O12-BiCoO3Nano crystal piece, the single crystal nanoplate can be under visible light
Irradiate lower rhodamine B degradation fluorescent dye.
7. the efficient visible light catalyst single crystal nanoplate as made from the preparation method of claim 5, which is characterized in that described
Under nano crystal piece irradiates under visible light, to the degradation rate of rhodamine B up to being 15min the time required to 95%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433831A (en) * | 2019-08-01 | 2019-11-12 | 青岛大学 | Composite photocatalyst material and preparation method thereof |
| CN115445656A (en) * | 2022-09-26 | 2022-12-09 | 南京工业大学 | Perovskite type optical/piezoelectric co-catalyst (4-aminotetrahydropyran) 2 PbBr 4 Preparation and application of nanocrystalline |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167584A (en) * | 2010-12-31 | 2011-08-31 | 扬州大学 | Ferrotitanium bismuth cobaltate ceramic material with five-laminated structure and multiferroic performance and preparation method thereof |
| CN106994349A (en) * | 2017-05-11 | 2017-08-01 | 中国科学院新疆理化技术研究所 | A kind of Preparation method and use of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167584A (en) * | 2010-12-31 | 2011-08-31 | 扬州大学 | Ferrotitanium bismuth cobaltate ceramic material with five-laminated structure and multiferroic performance and preparation method thereof |
| CN106994349A (en) * | 2017-05-11 | 2017-08-01 | 中国科学院新疆理化技术研究所 | A kind of Preparation method and use of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433831A (en) * | 2019-08-01 | 2019-11-12 | 青岛大学 | Composite photocatalyst material and preparation method thereof |
| CN115445656A (en) * | 2022-09-26 | 2022-12-09 | 南京工业大学 | Perovskite type optical/piezoelectric co-catalyst (4-aminotetrahydropyran) 2 PbBr 4 Preparation and application of nanocrystalline |
| CN115445656B (en) * | 2022-09-26 | 2023-12-19 | 南京工业大学 | Perovskite type photo/piezoelectric co-catalyst (4-aminotetrahydropyran) 2 PbBr 4 Preparation and application of nanocrystalline |
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