CN112520788A - Preparation method of nano bismuth vanadate powder - Google Patents

Preparation method of nano bismuth vanadate powder Download PDF

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CN112520788A
CN112520788A CN202011492515.XA CN202011492515A CN112520788A CN 112520788 A CN112520788 A CN 112520788A CN 202011492515 A CN202011492515 A CN 202011492515A CN 112520788 A CN112520788 A CN 112520788A
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bismuth vanadate
nano bismuth
preparation
vanadate powder
preparing nano
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魏志顺
姚远卓
常鹰
谌援
周志文
孔琦
李镇昊
王艳霞
冯宇扬
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Hubei University of Technology
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Hubei University of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00Compounds of vanadium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/20Vanadium, niobium or tantalum
    • B01J23/22Vanadium
    • B01J35/39
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The invention discloses a preparation method of nano bismuth vanadate powder. The method specifically comprises the following steps: with Bi (NO)3)3·5H2O and NaVO3The preparation method comprises the following steps of taking CTAB as a surfactant and deionized water as a solvent as raw materials, reacting by a hydrothermal method to prepare nano bismuth vanadate powder, adjusting the purity, crystallinity, morphology and the like of the prepared nano bismuth vanadate by changing reaction time, reaction temperature, surfactant amount and solvent amount, and obtaining a final product by combining centrifugal collection and high-temperature drying treatment. The preparation method is simple in preparation system and short in period, and the nano bismuth vanadate powder with high purity, regular crystal morphology and good dispersibility can be prepared by the method. In addition, the preparation raw materials are nontoxic and harmless, the cost is low, the preparation process is simple and efficient, the preparation method is suitable for mass production, and the obvious economic effect is achievedBenefit and environmental protection benefit.

Description

Preparation method of nano bismuth vanadate powder
Technical Field
The invention relates to the technical field of photocatalysis, relates to a preparation technology of a nano photocatalytic material, and particularly relates to a preparation method of nano bismuth vanadate powder.
Background
Bismuth vanadate (BiVO)4) As an excellent photocatalytic material, the material has the characteristics of good performance, no heavy metal element, bright and bright color, strong covering power, wide visible light utilization range, no harm to human bodies and environment and the like, and has great potential application value in many fields such as catalysis, decomposition, adsorption, coating and the like.
At present, the preparation method of nano bismuth vanadate mainly comprises a sol-gel method, a hydrothermal method, a coprecipitation method, a high-temperature solid-phase reaction method and the like. Patent CN107629482B provides a preparation method of orange bismuth vanadate pigment, which adopts a coprecipitation method, and after uniformly mixing a dilute nitric acid solution of a vanadium compound, a bismuth compound, aluminum nitrate, cerium nitrate and zinc nitrate and a molybdenum compound aqueous solution, adding ammonia water as a precipitator to obtain a bismuth vanadate precursor, and calcining at high temperature to obtain nano bismuth vanadate powder. The patent CN109110811A adopts a solid-phase sintering method, takes bismuth oxide and vanadium oxide as reaction raw materials, and prepares bismuth vanadate yellow powder by ball milling at high temperature. The patent CN105032394A adopts an ultrasonic-assisted reflux method, bismuth vanadate nano-powder precursor liquid is obtained through bismuth nitrate and ammonium metavanadate, and bismuth vanadate powder is prepared through ultrasonic-assisted reflux. The above patents have the problems of easy agglomeration of products, difficult control of reaction process, complex preparation system, low sample purity, high cost and the like, which restrict the mass production of nano bismuth vanadate.
Disclosure of Invention
The invention aims to overcome the defects of easy agglomeration of products, difficult control of reaction process, complex preparation system, low sample purity and high cost in the prior art and provide a preparation method of nano bismuth vanadate powder. The invention uses Bi (NO)3)3·5H2O and NaVO3The method is characterized in that CTAB (cetyl trimethyl ammonium bromide) is used as a surfactant, deionized water is used as a solvent, a hydrothermal method is adopted, the purity, crystallinity, morphology and the like of nano bismuth vanadate are controlled by controlling hydrothermal temperature, hydrothermal time, surfactant concentration and solvent amount, and a final product is obtained by combining centrifugal collection and high-temperature drying. The preparation method is simple in preparation system and short in period, and the nano bismuth vanadate powder which is high in purity, regular in crystal morphology and good in dispersity is prepared through the method. In addition, the preparation raw materials are nontoxic and harmless, the cost is low, the preparation process is simple and efficient, and the method is suitable for mass production and has obvious economic benefit and environmental protection benefit.
The purpose of the invention is realized by the following technical scheme:
a method for preparing nano bismuth vanadate powder comprises the following steps:
step (1) Bi (NO) with a certain mass3)3·5H2O、NaVO3The solid and a certain amount of CTAB are simultaneously dissolved in a certain amount of deionized water and placed in a polytetrafluoroethylene lining. At room temperature, uniformly stirring the solution by using a magnetic stirrer, and then putting the solution into a high-pressure kettle for hydrothermal reaction;
and (2) centrifugally collecting the product obtained in the step (1), washing with alcohol for multiple times, and drying at high temperature to obtain nano bismuth vanadate powder.
Preferably, in step (1), Bi is contained in the solution3+And VO3 3-The concentration ratio is preferably 1:2 to 2: 1.
In the step (1), the Bi (NO) is3)3·5H2O、NaVO3The molar ratio of the solid, CTAB and deionized water is: 2-4: 2-4: 0.2-0.4: 1000 to 3000.
Preferably, step (a)In step (1), said Bi (NO)3)3·5H2The preferable dosage of O is 2-4 mmol; NaVO3The dosage is preferably 2-4 mmol; the concentration of CTAB in the solution is preferably 0.002-0.02 mol/L.
Preferably, in the step (1), the concentration of CTAB in the solution is preferably 0.002-0.01 mol/L.
Preferably, in the step (1), the concentration of CTAB in the solution is preferably 0.003-0.01 mol/L.
Preferably, in the step (1), the hydrothermal reaction temperature is preferably 140-180 ℃.
Preferably, in the step (1), the hydrothermal reaction time is preferably 3-24 h.
Preferably, in the step (1), the dosage of the solvent deionized water is preferably 20-60 ml.
Preferably, in the step (2), the number of washing is preferably 3 to 5.
Preferably, in the step (2), the centrifugation condition is preferably 4000r/min for 5 min.
Preferably, in the step (2), the drying condition is preferably 70-95 ℃ for 8-16 h.
Compared with the prior art, the invention has the following advantages and remarkable progress:
(1) according to the method, CTAB is selected as a surfactant, the polyhedral morphology of the bismuth vanadate crystal can be well regulated and controlled, and proper doping is beneficial to the exertion of the photocatalytic performance of the bismuth vanadate;
(2) according to the method, a hydrothermal method is adopted for synthesizing the bismuth vanadate, the raw materials can be subjected to full reaction under the hydrothermal condition, the sample purity is high, and the control on conditions such as reaction time and temperature is easy to realize;
(3) the raw materials used in the method are nontoxic and harmless, and meet the current requirements of environmental protection and conservation;
(4) the method has the advantages of short reaction period, simple preparation system and lower cost, and is suitable for mass production.
Drawings
FIG. 1 is a flow chart of the preparation of nano bismuth vanadate powder.
Fig. 2 is scanning electron micrographs of nano bismuth vanadate powder prepared in five specific examples, wherein fig. 2(a) to 2(f) are scanning electron micrographs of nano bismuth vanadate powder prepared in examples 1 to 5, respectively.
FIG. 3 is the XRD pattern of the nano bismuth vanadate powder prepared by the five embodiments.
Detailed Description
The present invention is described in further detail below with reference to examples, but the embodiments of the present invention are not limited thereto.
The method relates to a method for preparing nano bismuth vanadate powder, namely Bi (NO)3)3·5H2O and NaVO3The method comprises the steps of taking CTAB as a raw material, taking deionized water as a solvent, adopting a hydrothermal method, controlling the hydrothermal temperature, hydrothermal time, surfactant concentration and solvent amount to control the purity, crystallinity, morphology and the like of bismuth vanadate powder, centrifugally collecting and washing, and finally drying centrifugally collected powder at 70-95 ℃ for 8-16h to obtain a final product, namely nano bismuth vanadate powder.
Observing the morphology of the sample powder by using a Scanning Electron Microscope (SEM); the crystal structure of the sample powder was examined by X-ray diffraction (XRD).
The following examples were carried out according to the above procedure using the reagents listed in Table 1.
TABLE 1 list of reagents
Figure BDA0002841139840000031
Example 1
(1) Weighing 2mmol of Bi (NO)3)3·5H2O, 2mmol of NaVO3And 0.2mmol CTAB, dissolved in 60mL of deionized water, can be placed directly into the polytetrafluoroethylene liner. After stirring with a magnetic stirrer for 5min, the above solutions were mixed to a stable orange-yellow solution. Then the mixture is put into an autoclave and treated for 24 hours in a high-temperature drying oven at 160 ℃.
(2) And (3) centrifugally washing the obtained product for 3 times, wherein the rotating speed of each time is 4000r/min, the duration is 5min, and then drying the product in a drying oven at the temperature of 80 ℃ for 12h to obtain bright yellow powder (nano bismuth vanadate powder).
Example 2
(1) Weighing 2mmol of Bi (NO)3)3·5H2O, 2mmol of NaVO3And 0.2mmol CTAB, dissolved in 60mL of deionized water, can be placed directly into the polytetrafluoroethylene liner. After stirring with a magnetic stirrer for 5min, the above solutions were mixed to a stable orange-yellow solution. Then the mixture is put into an autoclave and treated for 24 hours in a high-temperature drying oven at 180 ℃.
(2) And (3) centrifugally washing the obtained product for 3 times, wherein the rotating speed of each time is 4000r/min, the duration is 5min, and then drying the product in a drying oven at the temperature of 80 ℃ for 12h to obtain bright yellow powder (nano bismuth vanadate powder).
Example 3
(1) Weighing 2mmol of Bi (NO)3)3·5H2O, 2mmol of NaVO3And 0.4mmol CTAB, dissolved in 60mL of deionized water, can be placed directly into the polytetrafluoroethylene liner. After stirring with a magnetic stirrer for 5min, the above solutions were mixed to a stable orange-yellow solution. Then placing the mixture into an autoclave, and treating the mixture for 24 hours in a high-temperature drying oven at 160 DEG C
(2) And (3) centrifugally washing the obtained product for 3 times, wherein the rotating speed of each time is 4000r/min, the duration is 5min, and then drying the product in a drying oven at the temperature of 80 ℃ for 12h to obtain bright yellow powder (nano bismuth vanadate powder).
Example 4
(1) Weighing 2mmol of Bi (NO)3)3·5H2O, 2mmol of NaVO3And 0.2mmol CTAB, dissolved in 60mL of deionized water, can be placed directly into the polytetrafluoroethylene liner. After stirring with a magnetic stirrer for 5min, the above solutions were mixed to a stable orange-yellow solution. Then the mixture is put into an autoclave and treated for 6 hours in a high-temperature drying oven at 160 ℃.
(2) And (3) centrifugally washing the obtained product for 3 times, wherein the rotating speed of each time is 4000r/min, the duration is 5min, and then drying the product in a drying oven at the temperature of 80 ℃ for 12h to obtain bright yellow powder (nano bismuth vanadate powder).
Example 5
(1) Weighing 2mmol of Bi (NO)3)3·5H2O, 2mmol of NaVO3And 0.2mmol CTAB, dissolved in 20mL of deionized water, can be placed directly into the polytetrafluoroethylene liner. After stirring with a magnetic stirrer for 5min, the above solutions were mixed to a stable orange-yellow solution. Then the mixture is put into an autoclave and treated for 24 hours in a high-temperature drying oven at 160 ℃.
(2) And (3) centrifugally washing the obtained product for 3 times, wherein the rotating speed of each time is 4000r/min, the duration is 5min, and then drying the product in a drying oven at the temperature of 80 ℃ for 12h to obtain bright yellow powder (nano bismuth vanadate powder).
The scanning electron microscope image of the nano bismuth vanadate powder prepared in the embodiment of the invention is shown in fig. 2 (examples 1, 2, 3, 4 and 5 correspond to a, b, c, d and e in the figure respectively). The powder obtained in the example 1 contains a large number of polyhedral particles, and the shape is regular; the regularity of the polyhedral morphology in the powder obtained in example 2 is reduced; the polyhedral morphology in the powder obtained in example 3 is relatively irregular, and the particle agglomeration phenomenon exists; the powder obtained in the example 4 also has polyhedral particles, and the particle agglomeration phenomenon exists; the powder obtained in example 5 has many polyhedral particles and good dispersibility.
The X-ray diffraction pattern of the nano bismuth vanadate powder prepared by the embodiment of the invention is shown in FIG. 3 (examples 1, 2, 3, 4 and 5 correspond to (1), (2), (3), (4) and (5) in the figure, respectively). The diffraction pattern shows that all the yellow powders obtained in the examples are nano bismuth vanadate, and some examples contain impurities. The sample of example 1 has good crystallinity and contains no other impurities; example 2 the sample contained some impurities; the purity of bismuth vanadate in the embodiment 3 is better; the intensity of the diffraction peak of bismuth vanadate in example 4 was slightly lower than that of example 1, probably due to too short reaction time; the purity of bismuth vanadate in the sample of example 5 was also better.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention and are equivalent to the replacement of the above embodiments are included in the protection scope of the present invention.

Claims (10)

1. A method for preparing nano bismuth vanadate powder is characterized by comprising the following steps:
step (1) Bi (NO) with a certain mass3)3·5H2O、NaVO3The solid and a certain amount of CTAB are simultaneously dissolved in a certain amount of deionized water and placed in a polytetrafluoroethylene lining. At room temperature, uniformly stirring the solution by using a magnetic stirrer, and then putting the solution into a high-pressure kettle for hydrothermal reaction;
and (2) centrifugally collecting the product obtained in the step (1), washing with alcohol for multiple times, and drying at high temperature to obtain nano bismuth vanadate powder.
2. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (1), the Bi3+And VO3 3-The concentration ratio is 1: 2-2: 1.
3. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (1), the Bi (NO) is3)3·5H2O、NaVO3The molar ratio of the solid, CTAB and deionized water is: 2-4: 2-4: 0.2-0.4: 1000 to 3000.
4. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (1), the concentration of CTAB in the solution is 0.002-0.02 mol/L.
5. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (1), the hydrothermal reaction temperature is 140-180 ℃.
6. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (1), the hydrothermal reaction time is 3-24 h.
7. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (1), the dosage of the solvent, namely deionized water is 20-60 ml.
8. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (2), the centrifugation is carried out for 5min at the rotating speed of 4000 r/min.
9. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (2), the drying condition is that the drying is carried out for 8 to 16 hours at a temperature of between 70 and 95 ℃.
10. The method for preparing nano bismuth vanadate powder according to claim 1, wherein: in the step (2), the obtained product is washed by alcohol for 3-5 times and then dried at high temperature.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318700A (en) * 2008-07-16 2008-12-10 武汉大学 Bismuth vanadate powder and preparation method thereof
CN102502821A (en) * 2011-09-29 2012-06-20 北京工业大学 Mixed organic solvent-thermal method for preparing spherical or hollow spherical BiVO4
CN111017994A (en) * 2019-12-10 2020-04-17 广西大学 Preparation method of nano green-phase bismuth yellow vanadate powder

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318700A (en) * 2008-07-16 2008-12-10 武汉大学 Bismuth vanadate powder and preparation method thereof
CN102502821A (en) * 2011-09-29 2012-06-20 北京工业大学 Mixed organic solvent-thermal method for preparing spherical or hollow spherical BiVO4
CN111017994A (en) * 2019-12-10 2020-04-17 广西大学 Preparation method of nano green-phase bismuth yellow vanadate powder

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张爱平等: "水热法制备不同形貌和结构的BiVO_4粉末", 《物理学报》 *
王久生等: "高催化效率钒酸铋的合成及光催化性能", 《人工晶体学报》 *
长春工程学院学报: "朱丽伟等", 《长春工程学院学报》 *

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Application publication date: 20210319