CN102060330B - Method for synthetizing bismuth molybdate octahedral nanoparticle by microwave radiation heating - Google Patents
Method for synthetizing bismuth molybdate octahedral nanoparticle by microwave radiation heating Download PDFInfo
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- CN102060330B CN102060330B CN2010105566648A CN201010556664A CN102060330B CN 102060330 B CN102060330 B CN 102060330B CN 2010105566648 A CN2010105566648 A CN 2010105566648A CN 201010556664 A CN201010556664 A CN 201010556664A CN 102060330 B CN102060330 B CN 102060330B
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Abstract
The invention discloses a method for synthetizing a bismuth molybdate Bi3.2Mo0.8O7.5 octahedral nanoparticle by microwave radiation heating, belonging to the technical field of nanometer materials and catalytic materials. In the method, the bismuth molybdate octahedral nanoparticle of which the surface has a special form is synthetized by the precursor aqueous solution for microwave radiation heating; bismuth nitrate pentahydrate serving as a bismuth source is dispersed in the aqueous solution by an ultrasound cleaning instrument; sodium molybdate is added to form a precursor solution; the pH value and reaction temperature of a control system are controlled to ensure that the particle diameter of the octahedral nanoparticle is 50-200nm; and the bismuth molybdate octahedral nanoparticle has the advantages of good dispersibility and large specific surface area, has response property within a visible light range, and can be applied for catalytic degradation of organic matters by visual light so as to solve the pollution problems of waste gas and waste water. The preparation process provided by the invention has the advantages of moderate reaction condition, and simple and easy method, and the prepared bismuth molybdate octahedron nanoparticle can serve as a photocatalyst for the visual light.
Description
Technical field
A kind ofly add thermal synthesis bismuth molybdate Bi with microwave radiation
3.2Mo
0.8O
7.5The method of octahedron nanometer particle belongs to nano material and catalytic material technical field.
Background technology
From finding that titanium oxide is can catalytically decomposed water generates hydrogen and oxygen behind UV-irradiation; In Photocatalytic Performance Study subsequently; Find that also photocatalyst can the catalyzed degradation organism; The photo-catalysis function material has encouraged the novel high-efficiency photocatalysis material of the continuous R and D of people in the high-performance that shows aspect the environmental pollution improvements such as global energy dilemma that faces of solution and waste water and gas.Light-catalysed process less energy consumption can directly utilize the energy of sunshine, is converted into new forms of energy or thorough mineralising organic pollutant, solves the mankind in the problem that is faced aspect the energy and the environment.About the research of photocatalysis nano material, great majority concentrate on the modification aspect of titanium oxide or titanium oxide at present, but because titanium oxide can be with broad, poor to the responding ability of visible light, its application prospect receives certain restriction.Research prepares the new and effective photocatalyst material with visible light-responded ability, can not only make full use of the energy of sunshine, can also improve the catalytic efficiency (of photocatalyst.Bismuth composite oxide has layered crystal structure, is one type of photocatalyst material with visible light-responded character, has the potential application prospect.Therefore, the present invention selects microwave radiation heating method simple to operation, the bismuth molybdate nano particle that the hydro-thermal reaction through gentleness prepares stably dispersing and has visible light-responded performance.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who can be applicable to the organic bismuth molybdate nano particle of Photocatalytic Activity for Degradation, prepare stable nano particle with visible light-responded performance.
Technical scheme of the present invention: a kind ofly add thermal synthesis bismuth molybdate Bi with microwave radiation
3.2Mo
0.8O
7.5The method of octahedron nanometer particle is the bismuth source with five water Bismuth trinitrates, is dispersed in the aqueous solution through the ultrasonic cleaning appearance; Concentration is 0.4-0.5mol/L, adds the sodium molybdate solution of 0.25mol/L then, and the ratio that makes the molar weight in bismuth source and molybdenum source is 2:1; The pH value of regulating mixing solutions stirs after 30 minutes to 8-9, and mixing solutions is poured in the quartz reaction container; With deionized water mixed liquor volume is diluted 2-3 doubly, and continue at ambient temperature to stir 10-20 minute; After quartz reaction cap for container sealing compacting, to put into the microwave reaction appearance and carry out microwave radiation, temperature is set at 120-180 ℃, and the time is 10 minutes, and reaction naturally cools to room temperature with reaction vessel after finishing; Reacted liquid through centrifugal, filter after, the white depositions that obtains, use zero(ppm) water, absolute ethanol washing at least three times more successively after, place dry 5 hours of 50 ℃ of vacuum drying ovens with usefulness to be detected, obtain having the bismuth molybdate nano particle on eight surfaces.
Prepared bismuth molybdate Bi
3.2Mo
0.8O
7.5Octahedron nanometer particle under radiation of visible light, is used for degraded, processing waste gas waste water, the purifying vehicle exhaust field of organic waste as photocatalyst.
Its reaction equation is following:
Through characterizing methods such as x-ray diffractometer, sem, transmission electron microscope, X X-ray photoelectron spectroscopy X (XPS), ultraviolet spectrophotometers, show the Bi for preparing
3.2Mo
0.8O
7.5Nano particle is a bismuth molybdate, and all diffraction peaks in the XRD diffraction pattern (see figure 1) of bismuth molybdate nano particle can be the Bi of cube phase by index
3.2Mo
0.8O
7.5, unit cell parameters
a=
b=
c=5.654, fit like a glove with standard card JCPDS 77-0301.In the XRD of products therefrom style figure, do not observe any impurity peaks, all characteristic diffraction peaks are all very sharp-pointed and intensity is obvious, the Bi for preparing
3.2Mo
0.8O
7.5Nano-particle product purity is high, have good crystallinity.
Beneficial effect of the present invention: the present invention adopts gentle hydro-thermal reaction, has prepared bismuth molybdate Bi
3.2Mo
0.8O
7.5Nano particle; The particles dispersed performance is good; Be difficult for assembling, the visible light optical band in the sunshine is had response performance, have good photocatalytic activity ability; Can be used for organic waste degraded, handle aspects such as waste gas waste water, environment purification, be widely used in fields such as purifying vehicle exhaust, industrial sewage processing.Compare with traditional photocatalyst, the bismuth molybdate nano particle of the specific form of the present invention's preparation has higher specific surface area, has enlarged the absorption region of light wave, has better thermostability, and the gained bismuth molybdate nano particle recovery is high, and reuse is good.
The preparation process is carried out in the microwave reaction appearance, and reaction conditions is gentle, and method is simple, and the reaction times is short.Bismuth molybdate Bi is used in gained catalysis
3.2Mo
0.8O
7.5Nano particle need not complicated aftertreatment, through centrifugal remove reaction medium after, be dispersed in the aqueous solution or be coated with to be attached on the solid interface and get final product, synthetic bismuth molybdate nano particle is evenly distributed, size between 50～200nm, stably dispersing.
Description of drawings
The XRD diffraction pattern of Fig. 1 bismuth molybdate nano particle.
Fig. 2 (A) sem characterizes the photo of bismuth molybdate nano particle; (B) transmission electron microscope characterizes the photo of bismuth molybdate nano particle.
The uv drs spectrum of Fig. 3 bismuth molybdate nano particle.
Fig. 4 uv drs spectrum transforms the gained curve according to the energy calculation formula.
Fig. 5 bismuth molybdate nano particle is as catalyzer, the uv absorption spectra of degraded rhodamine B dye solution.
Embodiment
Embodiment 1
With 1mmoL five water Bismuth trinitrates is the bismuth source, is dispersed in the 2mL aqueous solution through the ultrasonic cleaning appearance, adds the sodium molybdate solution of 2mL 0.25mol/L; The ratio of the molar weight in bismuth source and molybdenum source is 2:1, regulates about the pH value to 8 of mixing solutions, stirs after 30 minutes; Mixing solutions is poured in the quartz reaction container, liquor capacity is adjusted to 8mL, and continue at ambient temperature to stir 15 minutes with deionized water; After quartz reaction cap for container sealing compacting, put into the microwave reaction appearance, temperature is set at 140 ℃; Time is 10 minutes, and reaction naturally cools to room temperature with reaction vessel after finishing.
Reacted liquid through centrifugal, filter after, obtain white depositions, use zero(ppm) water, absolute ethanol washing at least three times more successively after, place dry 5 hours of 50 ℃ of vacuum drying ovens in order to detecting usefulness, obtain having octahedral bismuth molybdate Bi
3.2Mo
0.8O
7.5Nano particle, particle diameter is about 200nm.
Sem characterizes bismuth molybdate Bi
3.2Mo
0.8O
7.5The photo of nano particle is seen Fig. 2 (a), and transmission electron microscope characterizes bismuth molybdate Bi
3.2Mo
0.8O
7.5The photo of nano particle is seen Fig. 2 (b).
Embodiment 2
With 0.8mmol five water Bismuth trinitrates is the bismuth source, is dispersed in the 2mL aqueous solution through the ultrasonic cleaning appearance, adds the sodium molybdate solution of 1.6mL 0.25mol/L; The ratio of the molar weight in bismuth source and molybdenum source is 2:1, regulates about the pH value to 9 of mixing solutions, stirs after 30 minutes; Mixing solutions is poured in the quartz reaction container, liquor capacity is adjusted to 10mL, and continue at ambient temperature to stir 15 minutes with deionized water; After quartz reaction cap for container sealing compacting, put into the microwave reaction appearance, temperature is set at 160 ℃; Time is 10 minutes, and reaction naturally cools to room temperature with reaction vessel after finishing.
Reacted liquid through centrifugal, filter after, obtain white depositions, use zero(ppm) water, absolute ethanol washing at least three times more successively after, place dry 5 hours of 50 ℃ of vacuum drying ovens in order to detecting usefulness, obtain having octahedral bismuth molybdate Bi
3.2Mo
0.8O
7.5Nano particle, particle diameter is about 100nm.
Prepared bismuth molybdate Bi
3.2Mo
0.8O
7.5The uv drs spectrum of nano particle is seen Fig. 3, and diffuse reflection spectrum transforms the gained collection of illustrative plates according to the energy calculation formula and sees Fig. 4.
The degraded of application implementation example 1 dyestuff rhodamine B solution
With rhodamine B (rhodamine B, RhB, C
28H
31ClN
2O
3) in the water-soluble solution of dyestuff, to the bismuth molybdate Bi that wherein adds embodiment 2 preparations
3.2Mo
0.8O
7.5Nano particle, reactant ratio: rhodamine B dyes concentration 10
-5M, bismuth molybdate nano particle 0.8g/L in the dark stirred 8 hours, made it reach adsorption equilibrium.Utilize the xenon lamp of 1000W that artificial visible light source is provided; Constantly stir; Whenever the solution of getting about 5mL at a distance from 10 minutes with dropper is in centrifuge tube; It is sample that catalyzer is fallen in centrifuging, gets supernatant liquid is measured RhB residual in the solution with ultraviolet spectrophotometer Lambda-35 uv absorption spectra.Characterize the transformation efficiency that reacts through UV spectrum, ultraviolet spectrogram is seen Fig. 5.Show that by Fig. 5 with the reaction times increase, the concentration of rhodamine B reduces, and shows that dyestuff rhodamine B solution is in continuous degraded.
Claims (1)
1. one kind with the synthetic bismuth molybdate Bi of carry out microwave radiation heating
3.2Mo
0.8O
7.5The method of octahedron nanometer particle is characterized in that with five water Bismuth trinitrates be the bismuth source, is dispersed in the aqueous solution through the ultrasonic cleaning appearance; Concentration is 0.4-0.5mol/L, adds the sodium molybdate solution of 0.25mol/L then, and the ratio that makes the molar weight in bismuth source and molybdenum source is 2:1; The pH value of regulating mixing solutions stirs after 30 minutes to 8-9, and mixing solutions is poured in the quartz reaction container; With deionized water mixed liquor volume is diluted 2-3 doubly, and continue at ambient temperature to stir 10-20 minute; After quartz reaction cap for container sealing compacting, to put into the microwave reaction appearance and carry out microwave radiation, temperature is set at 120-180 ℃, and the time is 10 minutes, and reaction naturally cools to room temperature with reaction vessel after finishing; Reacted liquid through centrifugal, filter after, the white depositions that obtains, use zero(ppm) water, absolute ethanol washing at least three times more successively after, place dry 5 hours of 50 ℃ of vacuum drying ovens with usefulness to be detected, obtain having the bismuth molybdate nano particle on eight surfaces.
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| CN102502834B (en) * | 2011-11-07 | 2013-10-09 | 河北联合大学 | Method for preparing surfactant-directed grown superfine bismuth molybdate nano rods |
| CN102502840B (en) * | 2011-11-07 | 2014-08-06 | 河北联合大学 | Preparation method for zirconium molybdate ultra-thin nanoparticles |
| CN102502891B (en) * | 2011-11-07 | 2013-09-25 | 河北联合大学 | Preparation method for nickel molybdate nanorod material |
| CN102502839B (en) * | 2011-11-07 | 2014-07-23 | 河北联合大学 | Method for preparing flaky bismuth molybdate nano material with uniform thickness |
| CN102658121A (en) * | 2012-02-14 | 2012-09-12 | 南昌航空大学 | Catalyst Bi2O3/Bi2MoO6 for photodegradation of organic matters and method for preparing the same |
| CN103663559B (en) * | 2012-09-05 | 2015-07-08 | 中国石油化工股份有限公司 | Dibismuth trimolybdenum dodecaoxide nanocrystalline as well as preparation method and application thereof |
| CN103418333B (en) * | 2013-07-30 | 2015-09-23 | 安徽师范大学 | A kind of Bi 3.64mo 0.36o 6.55the preparation method of nano particle and Bi thereof 3.64mo 0.36o 6.55nano material |
| WO2016080548A1 (en) * | 2014-11-21 | 2016-05-26 | 三菱化学株式会社 | Method for manufacturing composite photocatalyst, and composite photocatalyst |
| CN105381808B (en) * | 2015-10-20 | 2017-08-25 | 西南科技大学 | A kind of Mo/S/BiOCl is combined near ambient temperature degradation catalyst and its preparation and application method |
| CN107384054A (en) * | 2017-07-17 | 2017-11-24 | 河北卫华电工机械有限公司 | A kind of sunlight board light conversion coating with purification air and self-cleaning function |
| CN109589966A (en) * | 2019-01-21 | 2019-04-09 | 合肥学院 | A kind of hetero-junctions TiO2@Bi3.64Mo0.36O6.55The preparation method of nano composite photo-catalyst |
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| WO2007119929A1 (en) * | 2006-04-18 | 2007-10-25 | Sk Energy Co., Ltd. | Bismuth molybdate-based catalysts, method of preparing thereof and method of preparing 1,3-butadiene using thereof |
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| WO2007119929A1 (en) * | 2006-04-18 | 2007-10-25 | Sk Energy Co., Ltd. | Bismuth molybdate-based catalysts, method of preparing thereof and method of preparing 1,3-butadiene using thereof |
Non-Patent Citations (3)
| Title |
|---|
| Huidong Xie et al.Microwave hydrothermal synthesis and visible-light photocatalytic activity of γ-Bi2MoO6 nanoplates.《Materials Chemistry and Physics 》.2008,第110卷 * |
| JP平2-233523A 1990.09.17 |
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