CN112875755B - Preparation method of bismuth tungstate nano powder - Google Patents

Preparation method of bismuth tungstate nano powder Download PDF

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CN112875755B
CN112875755B CN202011604122.3A CN202011604122A CN112875755B CN 112875755 B CN112875755 B CN 112875755B CN 202011604122 A CN202011604122 A CN 202011604122A CN 112875755 B CN112875755 B CN 112875755B
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bismuth
bismuth nitrate
tungstate
sodium tungstate
nano powder
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CN112875755A (en
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鲍亮
张怀伟
白王峰
吴诗婷
元勇军
陈逸凡
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Hangzhou Dianzi University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • 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
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Abstract

The invention discloses a preparation method of bismuth tungstate nano powder, which comprises the following steps: 1) Dissolving bismuth nitrate in ethylene glycol to form a bismuth nitrate solution; 2) Dissolving sodium tungstate in deionized water to form a sodium tungstate solution; 3) Pouring the bismuth nitrate solution obtained in the step 1) into the sodium tungstate solution obtained in the step 2), stirring and transferring to a high-pressure reaction kettle; 4) And (3) sealing the reaction kettle with the high-pressure reaction materials, carrying out heat treatment, cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying to obtain the bismuth tungstate nano powder. The method has the advantages of simple process, easy control, no environmental pollution, low cost and easy large-scale production. The product has stable quality, high purity and good powder particle dispersibility.

Description

Preparation method of bismuth tungstate nano powder
Technical Field
The invention belongs to the technical field of inorganic non-metallic material manufacturing, and particularly relates to bismuth tungstate (Bi) 2 WO 6 ) A method for preparing nano powder.
Background
Energy is the most important material basis for human survival development, and with the increasing shortage of traditional fossil energy and the increasing demand of human for energy, new energy, particularly renewable energy, becomes a hot spot for the current social and scientific development. Bismuth tungstate (Bi) 2 WO 6 ) The photocatalyst is a novel photocatalyst with narrow forbidden band width, and can simultaneously generate response in ultraviolet light and visible light regions. Bi 2 WO 6 The catalyst is also a simple Aurivillius type oxide, the forbidden bandwidth of the catalyst is about 2.7eV, and the catalyst can absorb visible light with the wavelength within 450nm, so that organic pollutants can be catalytically degraded under the irradiation of the visible light, and the utilization efficiency of sunlight is effectively improved. Meanwhile, the raw material resources are rich, the environment is friendly, the stability is good, and the like, so that the method has a wide application prospect.
Currently synthesized Bi 2 WO 6 By the main process ofThe method comprises microwave, deposition, hydrothermal method and the like, wherein the hydrothermal solvothermal method is widely used for preparing various nano materials due to the advantages of easy control of crystal growth reaction kinetics, high product crystallinity and the like, and different particle morphologies show different electrochemical properties. Bi synthesized at home and abroad at present 2 WO 6 Has the problems of complex process, large grain size and inhibited photocatalytic activity.
Disclosure of Invention
The invention aims to provide bismuth tungstate (Bi) with simple process and easy control 2 WO 6 ) A hydrothermal synthesis preparation method of nano powder.
The invention adopts the following technical scheme:
a preparation method of bismuth tungstate nano powder is characterized by comprising the following steps:
1) Dissolving bismuth nitrate in ethylene glycol to form a bismuth nitrate solution;
2) Dissolving sodium tungstate in deionized water to form a sodium tungstate solution;
3) Pouring the bismuth nitrate solution obtained in the step 1) into the sodium tungstate solution obtained in the step 2), stirring and transferring to a high-pressure reaction kettle;
4) And (3) sealing the reaction kettle equipped with the high-pressure reaction material, carrying out heat treatment, cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying to obtain the bismuth tungstate nano powder.
Preferably, the concentration of the bismuth nitrate solution in the step 1) is 0.1-0.2 mol/L.
Preferably, the concentration of the sodium tungstate solution in the step 2) is 0.01-0.02 mol/L.
Preferably, the molar ratio of the sodium tungstate to the bismuth nitrate in the step 3) is 1:1-1:2.
Preferably, step 4), heat treatment is carried out at 120-140 ℃ for 14-20 hours.
Preferably, step 4), drying at the temperature of 60-80 ℃ to obtain the bismuth tungstate nano powder.
Bi prepared by the invention 2 WO 6 The nano powder has good dispersibility and thickness of not more than 20nm, so thatSo as to effectively increase the specific surface area of the material and have higher application value in the aspects of photocatalysis and the like.
The purity of the raw materials of sodium tungstate, potassium bismuth nitrate, the solvent of ethylene glycol, deionized water and absolute ethyl alcohol used in the invention is not lower than that of chemical purity.
By using the Bi of the present invention 2 WO 6 Preparation method of nanosheet and prepared Bi 2 WO 6 Good dispersibility and thickness not greater than 20nm.
The invention takes bismuth nitrate, sodium tungstate and the like as raw materials, controls Bi by regulating and controlling the time and the temperature of hydrothermal treatment by regulating and controlling the quantity proportion of each raw material substance in a mixed solvent 2 WO 6 Thereby realizing Bi growth process 2 WO 6 And (4) synthesizing nano powder. The cleaning of the water/solvothermal synthesis product is carried out to remove the excess reactant and obtain pure Bi 2 WO 6 Nanosheet powder. Dehydration with absolute ethyl alcohol and drying at a temperature of not higher than 80 ℃ are adopted to obtain Bi with good dispersibility 2 WO 6 And (3) nano powder.
The method has the advantages of simple process, easy control, no environmental pollution, low cost and easy large-scale production. Prepared Bi 2 WO 6 Is in the form of granules, and its thickness is not greater than 20nm. The product has stable quality, high purity and good powder particle dispersibility.
Drawings
FIG. 1 Bi synthesized by the present invention 2 WO 6 An X-ray diffraction (XRD) pattern of the nanopowder;
FIG. 2 Bi synthesized by the present invention 2 WO 6 Scanning Electron Microscope (SEM) photographs of the nanopowders.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
Bi is synthesized according to the following process steps 2 WO 6 Nano powder:
1) Metering and measuring bismuth nitrate, dissolving the bismuth nitrate into ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution as follows: 0.2mol/L (mol per liter).
2) Weighing sodium tungstate in a metering manner, dissolving the sodium tungstate in deionized water, and adjusting the concentration of the formed sodium tungstate solution to be: 0.02mol/L (mol per liter).
3) Slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to 1:2, stirring, transferring to a high-pressure reaction kettle, and adjusting the volume of the solution to be 4/5 of the volume of the reaction kettle by using deionized water.
4) The reaction kettle with the reaction materials is sealed and heat-treated at 140 ℃ for 20 hours. Then cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain Bi 2 WO 6 And (3) nano powder.
Bi synthesized in this example 2 WO 6 The X-ray diffraction (XRD) pattern of the nanopowder is shown in FIG. 1. The Scanning Electron Microscope (SEM) photograph thereof is shown in FIG. 2.
This example synthesizes Bi with a width of not more than 20nm by a water/solvothermal method 2 WO 6 And (3) nano powder.
Example 2
Bi is synthesized according to the following process steps 2 WO 6 Nano powder:
1) Measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.1mol/L.
2) Weighing sodium tungstate in a metering manner, dissolving the sodium tungstate in deionized water, and adjusting the concentration of the formed sodium tungstate solution to be: 0.01mol/L.
3) Slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to 1:1, stirring, transferring to a high-pressure reaction kettle, and adjusting the volume of the solution to be 2/3 of the volume of the reaction kettle by using deionized water.
4) The reaction kettle with the reaction materials is sealed, and heat treatment is carried out at 120 ℃ for 14 hours. Then cooling to room temperature, filtering, washing with deionized water and absolute ethyl alcohol in sequence, and drying at the temperature of 80 ℃ to obtain Bi 2 WO 6 And (3) nano powder.
Example 3
Press and press withSynthesis of Bi by the following process steps 2 WO 6 Nano powder:
1) Measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.1mol/L.
2) Weighing sodium tungstate to be dissolved in deionized water, and adjusting the concentration of the formed sodium tungstate solution to be: 0.01mol/L.
3) Slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to 1:2, stirring, transferring to a high-pressure reaction kettle, and adjusting the volume of the solution to be 3/4 of the volume of the reaction kettle by using deionized water.
4) The reaction kettle with the reaction materials is sealed and heat-treated at 140 ℃ for 20 hours. Then cooling to room temperature, filtering, washing with deionized water and absolute ethyl alcohol in sequence, and drying at the temperature of 80 ℃ to obtain Bi 2 WO 6 And (3) nano powder.
Example 4
Bi is synthesized according to the following process steps 2 WO 6 Nano powder:
1) Measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.15mol/L.
2) Weighing sodium tungstate to be dissolved in deionized water, and adjusting the concentration of the formed sodium tungstate solution to be: 0.015mol/L.
3) Slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 1.5, stirring, transferring to a high-pressure reaction kettle, and adjusting the volume of the solution to be 2/3 of the volume of the reaction kettle by using deionized water.
4) The reaction kettle with the reaction materials is sealed, and heat treatment is carried out at 130 ℃ for 18 hours. Then cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at 70 ℃ to obtain Bi 2 WO 6 And (3) nano powder.
Example 5
Bi is synthesized according to the following process steps 2 WO 6 Nano powder:
1) Measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.18mol/L.
2) Weighing sodium tungstate to be dissolved in deionized water, and adjusting the concentration of the formed sodium tungstate solution to be: 0.012mol/L.
3) Slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 1.3.
4) The reaction kettle with the reaction materials is sealed and is thermally treated for 15 hours at 125 ℃. Then cooling to room temperature, filtering, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 65 ℃ to obtain Bi 2 WO 6 And (3) nano powder.
The invention has simple preparation operation, low cost and strong repeatability, and adopts common raw material reagents. The bismuth tungstate nano powder prepared by the simple hydrothermal method has good dispersibility and the thickness of not more than 20nm, so that Bi can be reduced 2 WO 6 The particle size of the material effectively increases the specific surface area of the material, is beneficial to subsequent load treatment, and has higher application value in the aspects of photocatalysis and the like.

Claims (2)

1. A preparation method of bismuth tungstate nano powder is characterized by comprising the following steps:
1) Dissolving bismuth nitrate in ethylene glycol to form a bismuth nitrate solution;
2) Dissolving sodium tungstate in deionized water to form a sodium tungstate solution;
3) Pouring the bismuth nitrate solution obtained in the step 1) into the sodium tungstate solution obtained in the step 2), stirring and transferring to a high-pressure reaction kettle;
4) Sealing the reaction kettle equipped with the high-pressure reaction material, carrying out heat treatment, then cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying to obtain bismuth tungstate nano powder;
step 1), the concentration of the bismuth nitrate solution is 0.1-0.2 mol/L;
step 2), the concentration of the sodium tungstate solution is 0.01-0.02 mol/L;
step 3), the molar ratio of the sodium tungstate to the bismuth nitrate is 1:1-1:2;
and 4) performing heat treatment at the temperature of between 120 and 140 ℃ for 14 to 20 hours.
2. The method for preparing bismuth tungstate nano-powder according to claim 1, wherein in the step 4), the bismuth tungstate nano-powder is dried at a temperature of 60-80 ℃ to obtain the bismuth tungstate nano-powder.
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