CN102060330A - 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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- CN102060330A CN102060330A CN201010556664.8A CN201010556664A CN102060330A CN 102060330 A CN102060330 A CN 102060330A CN 201010556664 A CN201010556664 A CN 201010556664A CN 102060330 A CN102060330 A CN 102060330A
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- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 13
- 230000005855 radiation Effects 0.000 title claims abstract description 12
- 238000010438 heat treatment Methods 0.000 title abstract description 4
- 230000003407 synthetizing effect Effects 0.000 title abstract 2
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 11
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011941 photocatalyst Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 5
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002912 waste gas Substances 0.000 claims abstract description 5
- 239000002351 wastewater Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000010815 organic waste Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 230000004044 response Effects 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 230000000007 visual effect Effects 0.000 abstract 2
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 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 description 7
- 229940043267 rhodamine b Drugs 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000000975 dye Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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 dioxide is can catalytic decomposition water generates hydrogen and oxygen after 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 sunlight, is converted into new forms of energy or thorough mineralising organic pollutant, solves human 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 dioxide or titanium dioxide at present, but because titanium dioxide can be with broad, poor to the responding ability of visible light, its application prospect is subjected to 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 sunlight, can also improve the catalytic efficiency of photocatalyst.Bismuth composite oxide has layered crystal structure, is the photocatalyst material that a class has 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 by 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, with five water Bismuth trinitrates is the bismuth source, be dispersed in the aqueous solution by the ultrasonic cleaning instrument, concentration is 0.4-0.5mol/L, adds the sodium molybdate solution of 0.25mol/L then, 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 instrument 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 distilled 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 as follows:
By characterizing methods such as x-ray diffractometer, scanning electronic microscope, 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 height, has 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, visible light optical band in the sunlight had response performance, has 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, gained bismuth molybdate nano particle rate of recovery height, and reuse is good.
Preparation process is carried out in the microwave reaction instrument, the reaction conditions gentleness, and method is simple, and the reaction times is short.Gained catalysis bismuth molybdate Bi
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 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) scanning electronic microscope 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, be dispersed in the 2mL aqueous solution by the ultrasonic cleaning instrument, the sodium molybdate solution that adds 2mL 0.25mol/L, the ratio of the molar weight in bismuth source and molybdenum source is 2:1, regulate about the pH value to 8 of mixing solutions, stir 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 instrument, temperature is set at 140 ℃, and the time is 10 minutes, reaction naturally cools to room temperature with reaction vessel after finishing.
Reacted liquid through centrifugal, filter after, obtain white depositions, use distilled 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.
Scanning electronic microscope 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, be dispersed in the 2mL aqueous solution by the ultrasonic cleaning instrument, the sodium molybdate solution that adds 1.6mL 0.25mol/L, the ratio of the molar weight in bismuth source and molybdenum source is 2:1, regulate about the pH value to 9 of mixing solutions, stir 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 instrument, temperature is set at 160 ℃, and the time is 10 minutes, reaction naturally cools to room temperature with reaction vessel after finishing.
Reacted liquid through centrifugal, filter after, obtain white depositions, use distilled 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 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, got the solution of about 5mL every 10 minutes in centrifuge tube with dropper, 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 by 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 (2)
1. one kind adds thermal synthesis bismuth molybdate Bi with microwave radiation
3.2Mo
0.8O
7.5The method of octahedron nanometer particle, it is characterized in that with five water Bismuth trinitrates be the bismuth source, be dispersed in the aqueous solution by the ultrasonic cleaning instrument, concentration is 0.4-0.5mol/L, adds the sodium molybdate solution of 0.25mol/L then, 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 instrument 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 distilled 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.
2. the described method synthetic of claim 1 bismuth molybdate Bi
3.2Mo
0.8O
7.5The application of octahedron nanometer particle is characterized in that 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.
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Cited By (11)
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CN102502839A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing flaky bismuth molybdate nano material with uniform thickness |
CN102502834A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing surfactant-directed grown superfine bismuth molybdate nano rods |
CN102502891A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Preparation method for nickel molybdate nanorod material |
CN102502840A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Preparation method for zirconium molybdate ultra-thin nanoparticles |
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 |
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CN103663559A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Dibismuth trimolybdenum dodecaoxide nanocrystalline as well as preparation method and application thereof |
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JP2017039115A (en) * | 2014-11-21 | 2017-02-23 | 三菱化学株式会社 | Method for producing composite photocatalyst and composite photocatalyst |
CN105381808A (en) * | 2015-10-20 | 2016-03-09 | 西南科技大学 | Mo/S/BiOCl composite near normal temperature degradation catalyst and preparation method therefor and application method thereof |
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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