CN106219606A - A kind of spherical Ag of nano flower3vO4preparation method - Google Patents
A kind of spherical Ag of nano flower3vO4preparation method Download PDFInfo
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- CN106219606A CN106219606A CN201610547784.9A CN201610547784A CN106219606A CN 106219606 A CN106219606 A CN 106219606A CN 201610547784 A CN201610547784 A CN 201610547784A CN 106219606 A CN106219606 A CN 106219606A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
A kind of spherical Ag of nano flower3VO4Preparation method, use precipitation assisting alcohol-hydrothermal method synthesis, its preparation method includes: silver nitrate joins polyvinylpyrrolidone and ammonium metavanadate (NH that concentration is 0.1～0.3mol/L4VO3) in mixed solution, regulate pH value to behind 4～12 by the NaOH solution of 0.2mol/L, heat treatment 4～12h at 80～180 DEG C.Obtained precipitate uses distilled water and absolute ethanol washing after filtering respectively, and is dried in the vacuum drying oven of 60～80 DEG C.The silver vanadate powder obtained is mono-crystalline structures, and chemical composition is homogeneous, and purity is higher, has bigger specific surface area, improves the photocatalysis performance of material.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, relate to semiconductor nano material preparation and application, be specifically related to one and receive
The spherical Ag of popped rice3VO4Preparation method.
Background technology
Photocatalysis technology is the emerging technology of a field of energy environment, such as TiO2For represent catalysis material because
At room temperature the organic pollution exhaustive oxidation in environment can be decomposed into H2O、CO2Etc. nontoxic thing, and have efficiency high,
The advantages such as low cost, catalyst chemically-resistant and photochemical corrosion and more and more paid close attention to by people.Vanadate is good because having
Good photocatalysis performance and be widely studied, such as BiVO4、InVO4、FeVO4It is widely used in photocatalysis field, vanadium Deng material
Acid lithium material also has remarkable progress in field of batteries.
Ag3VO4Higher energy conduction band formed by the 3d orbital hybridization of 5s and V of Ag, and its mental retardation valence band by the 4d track of Ag and
The 2p orbital hybridization of O forms.The valence band structure of hydridization makes energy level more active, causes its monoclinic phase band gap width ＜ 2.7eV.
This construction features makes silver vanadate have wider response range to visible ray, before photocatalysis field has potential application
Scape.
At present, the pattern of the silver vanadate prepared by the method such as hydro-thermal method, microwave-hydrothermal method proposed both at home and abroad includes: granule
Shape, square block, threadiness etc..Chinese invention issued patents the 201310257173.7th discloses a kind of silver vanadate nanofiber
Photocatalyst, it uses method of electrostatic spinning to prepare, but to requirement height such as moisture, technical difficulty is big.No. 201210531539.0
Disclose a kind of bar-shaped silver vanadate nano-photocatalyst, use double note sedimentation method to prepare bar-shaped silver vanadate crystallite, but technical difficulty
Greatly, and to prepared product preservation condition height is required.No. 201310287983.7 discloses a kind of silver vanadate nano wire
Preparation method, but reaction time is long.CTAB-assisted hydrothermal synthesis of silver
Vanadates and their photocatalytic characterization.Chao-Ming Huang et al. uses
CTAB combines heat treatment mode as the hydro-thermal of surfactant and prepares Ag3VO4With Ag4V2O7Mixed phase, its product is pure
Spend the highest, and size is bigger.The preparation method of the silver vanadate of special appearance is also little at present, the therefore silver vanadate to special appearance
Research be significant.
Summary of the invention
The present invention is directed to above-mentioned the deficiencies in the prior art, propose a kind of spherical Ag of nano flower3VO4Preparation method, the method
Reaction condition is gentle, simple to operate, can repeat preparation the most in a large number, and preparation silver vanadate product purity is high, stable in properties.
To achieve these goals, the present invention is by the following technical solutions.
A kind of spherical Ag of nano flower3VO4Preparation method, comprise the following steps:
(1) polyvinylpyrrolidone is joined in ammonium metavanadate aqueous solution, stir, obtain mixed solution A；
(2) silver nitrate solution is added drop-wise in mixed solution A, stirring lower 1～3h, obtains mixed solution B；
(3) regulation mixed solution pH value is to behind 4～12, after carrying out hydro-thermal reaction 4～12h at 80～180 DEG C, and will reaction
Liquid is filtrated to get precipitation, precipitates scrubbed, dry, obtains the spherical Ag of nano flower3VO4。
The present invention is further improved by, and in step (1), the concentration of ammonium metavanadate aqueous solution is 0.1～0.3mol/L,
The amount ratio of polyvinylpyrrolidone and ammonium metavanadate aqueous solution is (0.01～0.04) g:(20～60) mL.
The present invention is further improved by, and in step (1), stirring is carried out at 40～100 DEG C, and stir
Time is 1～3h.
The present invention is further improved by, and the concentration of the silver nitrate solution described in step (2) is 0.1～0.3mol/L,
The amount ratio of silver nitrate solution and ammonium metavanadate aqueous solution is (20～60) mL:(10～60) mL.
The present invention is further improved by, and step (3) uses the NaOH solution regulation mixed solution of 0.1～0.3mol/L
The pH value of B.
The present invention is further improved by, and stirs 1～8h, then carry out hydro-thermal after regulation mixed solution pH value to 4～12
Reaction.
The present invention is further improved by, and the hydro-thermal reaction described in step (3) is to carry out in autoclave.
The present invention is further improved by, and the washing described in step (3) is by precipitation distilled water and washing with alcohol.
The present invention is further improved by, and dry described in step (3) is to carry out at 40～80 DEG C.
Compared with prior art, the present invention can obtain following beneficial effect:
(1) precipitation auxiliary water by the use of thermal means of the present invention is with NH4VO3As vanadium source, with AgNO3As silver source, PVP
As surfactant, regulate the pH value of solution with NaOH aqueous solution, then at 80～150 DEG C, carry out hydro-thermal reaction, prepare light
The silver vanadate of the flower ball-shaped of the size uniformity that catalytic performance is good.
(2) present invention wet chemistry method synthesizes silver vanadate, it is achieved that Ag, V, O mixing on a molecular scale.Product size
Uniformly, and be mono-crystalline structures.
(3) precipitation auxiliary water thermal process of the present invention, flow process is short, and technique is simple, and constant product quality and pattern are equal
One, it is easy to accomplish industrialization.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the silver vanadate that the present invention is prepared under the conditions of embodiment 3.
Fig. 2 is the scanning electron microscope diagram of the silver vanadate that the present invention is prepared under the conditions of embodiment 3, and wherein, figure (a) is
Being not added with the scanning figure of PVP prepared catalyst, figure (b) is the PVP scanning figure as surfactant prepared catalyst.
Fig. 3 is the degraded to rhodamine B under visible light illumination of the silver vanadate prepared under the conditions of embodiment 3 of the present invention
Curve chart.
Detailed description of the invention
Below in conjunction with the accompanying drawings and the present invention is described in further detail by specific embodiment:
Embodiment 1
(1) 0.01g polyvinylpyrrolidone (PVP) is joined the ammonium metavanadate (NH of 20mL 0.1mol/L4VO3) water-soluble
In liquid, magnetic agitation 1h at 90 DEG C, it is cooled to room temperature, obtains mixed solution A.
(2) by the silver nitrate (AgNO of 60mL 0.3mol/L3) solution is added drop-wise in mixed solution A, magnetic agitation 1h,
To mixed solution B.
(3) use the pH value of NaOH solution regulation mixed solution B of 0.1mol/L to magnetic agitation 3h after 12, at 180 DEG C
Lower hydro-thermal reaction 4h, after reaction terminates, is precipitated reacting liquid filtering, and obtained precipitate uses distilled water after filtering respectively
With ethanol centrifuge washing, and in the baking oven of 70 DEG C be dried, obtain the spherical Ag of nano flower3VO4。
Embodiment 2
(1) 0.02g polyvinylpyrrolidone (PVP) is joined the ammonium metavanadate (NH of 20mL 0.1mol/L4VO3) water-soluble
In liquid, magnetic agitation 1h at 80 DEG C, it is cooled to room temperature, obtains mixed solution A.
(2) by the silver nitrate (AgNO of 60mL 0.3mol/L3) solution is added drop-wise in mixed solution A, magnetic agitation 1h,
To mixed solution B.
(3) use the pH value of NaOH solution regulation mixed solution B of 0.2mol/L to magnetic agitation 3h after 10, at 150 DEG C
Lower hydro-thermal reaction 6h, after reaction terminates, is precipitated reacting liquid filtering, and obtained precipitate uses distilled water after filtering respectively
With ethanol centrifuge washing, and in the baking oven of 70 DEG C be dried, obtain the spherical Ag of nano flower3VO4。
Embodiment 3
(1) 0.03g polyvinylpyrrolidone (PVP) is joined the ammonium metavanadate (NH of 20mL 0.1mol/L4VO3) water-soluble
In liquid, magnetic agitation 1h at 60 DEG C, it is cooled to room temperature, obtains mixed solution A.
(2) by the silver nitrate (AgNO of 60mL 0.3mol/L3) solution is added drop-wise in mixed solution A, magnetic agitation 1h,
To mixed solution B.
(3) use the pH value of NaOH solution regulation mixed solution B of 0.3mol/L to magnetic agitation 3h after 7, at 120 DEG C
Hydro-thermal reaction 8h, after reaction terminates, is centrifuged with distilled water and ethanol after being filtered by the precipitate obtained by reacting liquid filtering respectively
Washing, and be dried in the baking oven of 70 DEG C, obtain the spherical Ag of nano flower3VO4。
See Fig. 1, by XRD diffracting spectrum, it is clear that Ag prepared by the present invention3VO4Tie for pure phase monocrystal
Structure；
See Fig. 2, from the stereoscan photograph of Fig. 2 (a) and Fig. 2 (b) it can be seen that the lamellar spacing 10nm of flower ball-shaped～
20nm, is self-assembled into flower ball-shaped, bouquet a diameter of 2～5 μm；
See Fig. 3, this powder body of 0.05g is put in 50mL rhodamine B solution (rhodamine B concentration 10mg/L), visible
Under the conditions of light irradiates, after reaction 4h, the degradation rate of rhodamine B is up to more than 80%.
Embodiment 4
(1) 0.04g polyvinylpyrrolidone (PVP) is joined the ammonium metavanadate (NH of 20mL 0.1mol/L4VO3) water-soluble
In liquid, magnetic agitation 1h at 40 DEG C, it is cooled to room temperature, obtains mixed solution A.
(2) by the silver nitrate (AgNO of 60mL 0.3mol/L3) solution is added drop-wise in mixed solution A, magnetic agitation 1h,
To mixed solution B.
(3) use the pH value of NaOH solution regulation mixed solution B of 0.2mol/L to magnetic agitation 3h after 4, at 100 DEG C
Hydro-thermal reaction 10h, after reaction terminates, is precipitated reacting liquid filtering, and obtained precipitate uses distilled water after filtering respectively
With ethanol centrifuge washing, and in the baking oven of 70 DEG C be dried, obtain the spherical Ag of nano flower3VO4。
Embodiment 5
(1) polyvinylpyrrolidone is joined in ammonium metavanadate aqueous solution, at 40 DEG C, stir 3h, obtain mixed solution
A；Wherein, the concentration of ammonium metavanadate aqueous solution is the amount ratio of 0.2mol/L, polyvinylpyrrolidone and ammonium metavanadate aqueous solution
For 0.02g:40mL.
(2) silver nitrate solution is added drop-wise in mixed solution A, the lower 2h of stirring, obtains mixed solution B；Wherein, silver nitrate is molten
The concentration of liquid be the amount ratio of 0.1mol/L, silver nitrate solution and ammonium metavanadate aqueous solution be 20mL:40mL.
(3) the NaOH solution regulation mixed solution pH value using 0.1mol/L stirs 1h, then at height at 80 DEG C after 8
After pressure reactor carries out hydro-thermal reaction 12h, reacting liquid filtering is precipitated, precipitates through distilled water and washing with alcohol, 40
It is dried at DEG C, obtains the spherical Ag of nano flower3VO4。
Embodiment 6
(1) polyvinylpyrrolidone is joined in ammonium metavanadate aqueous solution, at 100 DEG C, stir 1h, obtain mixing molten
Liquid A；Wherein, the concentration of ammonium metavanadate aqueous solution is the consumption of 0.3mol/L, polyvinylpyrrolidone and ammonium metavanadate aqueous solution
Ratio is 0.04g:60mL.
(2) silver nitrate solution is added drop-wise in mixed solution A, the lower 3h of stirring, obtains mixed solution B；Wherein, silver nitrate is molten
The concentration of liquid be the amount ratio of 0.2mol/L, silver nitrate solution and ammonium metavanadate aqueous solution be 40mL:60mL.
(3) use the NaOH solution regulation mixed solution pH value of 0.3mol/L to stirring 8h after 5, then at 140 DEG C
After autoclave carries out hydro-thermal reaction 7h, reacting liquid filtering is precipitated, precipitates through distilled water and washing with alcohol, 80
It is dried at DEG C, obtains the spherical Ag of nano flower3VO4。
The flower ball-shaped silver vanadate nano material photocatalyst that the present invention prepares, monocline crystalline phase, the composition expression formula of this particle
For Ag3VO4.Nanoscale twins thickness 10nm～20nm, is self-assembled into flower ball-shaped, bouquet a diameter of 2～5 μm.
Described silver vanadate is the pure phase silver vanadate obtained under condition of different pH.The silver vanadate nano material of flower ball-shaped uses heavy
The water heat transfer of auxiliary of forming sediment.Chemical composition is homogeneous, and purity is higher, has bigger specific surface area, and the light that improve material is urged
Change performance.
Claims (9)
1. the spherical Ag of nano flower3VO4Preparation method, it is characterised in that comprise the following steps:
(1) polyvinylpyrrolidone is joined in ammonium metavanadate aqueous solution, stir, obtain mixed solution A；
(2) silver nitrate solution is added drop-wise in mixed solution A, stirring lower 1～3h, obtains mixed solution B；
(3) regulation mixed solution pH value is to behind 4～12, after carrying out hydro-thermal reaction 4～12h at 80～180 DEG C, by reactant liquor mistake
Filter is precipitated, and precipitates scrubbed, dry, obtains the spherical Ag of nano flower3VO4。
A kind of spherical Ag of nano flower the most according to claim 13VO4Preparation method, it is characterised in that in step (1) partially
The concentration of ammonium vanadate aqueous solution is 0.1～0.3mol/L, and the amount ratio of polyvinylpyrrolidone and ammonium metavanadate aqueous solution is
(0.01～0.04) g:(20～60) mL.
A kind of spherical Ag of nano flower the most according to claim 13VO4Preparation method, it is characterised in that step is stirred in (1)
Mix and carry out at 40～100 DEG C, and the time stirred is 1～3h.
A kind of spherical Ag of nano flower the most according to claim 13VO4Preparation method, it is characterised in that step (2) is described
The concentration of silver nitrate solution be 0.1～0.3mol/L, the amount ratio of silver nitrate solution and ammonium metavanadate aqueous solution be (20～
60) mL:(10～60) mL.
A kind of spherical Ag of nano flower the most according to claim 13VO4Preparation method, it is characterised in that step (3) use
The pH value of the NaOH solution regulation mixed solution B of 0.1～0.3mol/L.
A kind of spherical Ag of nano flower the most according to claim 13VO4Preparation method, it is characterised in that regulation mixing molten
Liquid pH value stirs 1～8h to 4～12, then carries out hydro-thermal reaction.
A kind of spherical Ag of nano flower the most according to claim 13VO4Preparation method, it is characterised in that step (3) is described
Hydro-thermal reaction be to carry out in autoclave.
A kind of spherical Ag of nano flower the most according to claim 13VO4Preparation method, it is characterised in that step (3) is described
Washing be by precipitation distilled water and washing with alcohol.
A kind of spherical Ag of nano flower the most according to claim 13VO4Preparation method, it is characterised in that step (3) is described
Dry be to carry out at 40～80 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107827153A (en) * | 2017-10-31 | 2018-03-23 | 成都先进金属材料产业技术研究院有限公司 | A kind of preparation method of nanometer of silver vanadate |
| CN110759381A (en) * | 2019-11-05 | 2020-02-07 | 北华航天工业学院 | Preparation method of coral-shaped lithium vanadate nano material |
| CN115779929A (en) * | 2022-09-29 | 2023-03-14 | 南京师范大学 | Modified ZnIn 2 S 4 Photocatalyst and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827153A (en) * | 2017-10-31 | 2018-03-23 | 成都先进金属材料产业技术研究院有限公司 | A kind of preparation method of nanometer of silver vanadate |
| CN107827153B (en) * | 2017-10-31 | 2019-12-03 | 成都先进金属材料产业技术研究院有限公司 | A kind of preparation method of nanometer of silver vanadate |
| CN110759381A (en) * | 2019-11-05 | 2020-02-07 | 北华航天工业学院 | Preparation method of coral-shaped lithium vanadate nano material |
| CN110759381B (en) * | 2019-11-05 | 2021-11-19 | 北华航天工业学院 | Preparation method of coral-shaped lithium vanadate nano material |
| CN115779929A (en) * | 2022-09-29 | 2023-03-14 | 南京师范大学 | Modified ZnIn 2 S 4 Photocatalyst and preparation method and application thereof |
| CN115779929B (en) * | 2022-09-29 | 2024-02-23 | 南京师范大学 | Modified ZnIn 2 S 4 Photocatalyst, preparation method and application thereof |
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