CN103949242B - Bismuth tungstate (Bi2WO6) preparation method of flake nano material - Google Patents
Bismuth tungstate (Bi2WO6) preparation method of flake nano material Download PDFInfo
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- CN103949242B CN103949242B CN201410122390.XA CN201410122390A CN103949242B CN 103949242 B CN103949242 B CN 103949242B CN 201410122390 A CN201410122390 A CN 201410122390A CN 103949242 B CN103949242 B CN 103949242B
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 34
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 34
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229950000845 politef Drugs 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 12
- 239000000975 dye Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 11
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 5
- 239000010865 sewage Substances 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 description 11
- 238000006731 degradation reaction Methods 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 8
- 239000002135 nanosheet Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 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 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 241000222065 Lycoperdon Species 0.000 description 2
- 241000768494 Polymorphum Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- PPNKDDZCLDMRHS-UHFFFAOYSA-N bismuth(III) nitrate Inorganic materials [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The present invention relates to a kind of bismuth tungstate (Bi with efficient visible light catalyst2WO6) preparation method of flake nano material.Tradition bismuth tungstate nano material is lamellar clustered stacked one-tenth soccer star's nano-particle, and the present invention adopts one step hydro thermal method, and by bismuth tungstate nano material prepared by adjusting solvent ratio, this material is scattered nanometer sheet.The nanometer sheet thickness prepared is uniform, good dispersion.Laminated structure makes material light catalysis activity crystal face must expose to greatest extent, has high visible light catalysis activity.This material is also equipped with selectivity simultaneously, and the absorption to different organic dyestuff, degraded has bigger difference.This flake nano material preparation method is simple, with low cost, has broad application prospects at sewage treatment area.
Description
Technical field
The invention belongs to field of material technology, relate to a kind of bismuth tungstate (Bi2WO6) preparation method of flake nano material.
Background technology
Having delivered " Nature " about since TiO2 photocatalytic water from Fujishima and Hongda in 1972, semiconductor light-catalyst just must be studied by extensive as a kind of new catalysis material.The reported first such as Kudo in 1999 bismuth tungstate has photocatalytic activity under the wavelength visible radiation more than 420nm, its energy gap (about 2.7eV), can by excited by visible light and have higher catalysis activity under visible light.Exactly because such characteristic, bismuth tungstate is taken as a kind of novel catalysis material and causes increasing concern.
At visible light-responded lower bismuth tungstate (Bi2WO6) can degrading organic dye waste water effectively, therefore, bismuth tungstate is at degradable organic pollutant, and field of sewage treatment has very important practical value.
Traditional tungstates photocatalyst is usually prepared by high-temperature calcination method, this process not only consumes the substantial amounts of energy, and the sample particle size prepared is big, and the specific surface area of catalyst is substantially reduced, though can realizing visible light-responded, but photocatalysis efficiency being unsatisfactory.Although widely used hydro-thermal method solves the problems such as high energy consumption and too low reference area, but the bismuth tungstate nano-particle synthesized is mostly gathering, stacking form, it is impossible to make material light catalysis activity crystal face must expose to greatest extent.The photocatalysis performance that cannot make bismuth tungstate nano material obtains maximum representing.
Summary of the invention
Present invention aim to overcome that above closest to the deficiencies in the prior art, disclose a kind of monodispersed bismuth tungstate (Bi2WO6) preparation method of nano lamellar material, the method synthesizes only with one step hydro thermal method, very simply, with low cost, less demanding to equipment；The flaky nanometer structure material of the present invention has highly efficient photocatalytic activity than the material of conventional gathering, stacked, and meanwhile, absorption and degraded to different dyes also have higher selectivity.
The technical scheme provided is:
A kind of bismuth tungstate (Bi2WO6) preparation method of flake nano material, it is characterised in that comprise the following steps: according to Na2WO42H2O and Bi (NO3)35H2The amount of substance of O is sampled than for 1:2, by Na2WO42H2O and Bi (NO3)35H2O is each dissolved separately in deionized water and isooctanol, and deionized water and isooctanol volume ratio are 1:4, carry out the magnetic agitation of certain time respectively, will carry out the magnetic agitation of certain time again after two kinds of solution mixing of gained.By this solution as, in politef reactor, carrying out the hydro-thermal reaction of a period of time at a certain temperature.By the material prepared through repeatedly washing, ultrasonic, centrifugal, drying operation, prepare Bi2WO6Flake nano material.
Tradition bismuth tungstate nano material is the clustered stacked spheroiding nano-particle of lamellar, and by comparison, the present invention adopts one step hydro thermal method, and by bismuth tungstate nano material prepared by adjusting solvent ratio, this material is scattered nanometer sheet..The nanometer sheet thickness that the present invention prepares is uniform, good dispersion.Laminated structure makes material light catalysis activity crystal face must expose to greatest extent, has high visible light catalysis activity.This material is also equipped with selectivity simultaneously, and the absorption to different organic dyestuff, degraded has bigger difference.This flake nano material preparation method is simple, with low cost, has broad application prospects at sewage treatment area.
Specifically, the advantage that technical solution of the present invention embodies is in that:
1, medicine used by the present invention is all commercially available from market, and preparation method is simple, to equipment and experiment condition without too high requirement, easily operated.
2, material prepared by the present invention is nano lamellar material, has great specific surface area, must be exposed by material light catalysis activity crystal face to greatest extent, thus its photocatalytic activity is greatly improved simultaneously.
3, product prepared by the present invention is while having efficient photocatalysis performance, is also equipped with the selective absorption to different dyes and degradation selectivity.As a kind of novel catalysis material, have broad application prospects in field of sewage treatment.
Accompanying drawing explanation
Fig. 1 is bismuth tungstate (Bi2WO6) SEM photograph of nanometer sheet.
Fig. 2 is bismuth tungstate (Bi2WO6) the partial enlargement SEM photograph of nanometer sheet.
Fig. 3 is bismuth tungstate (Bi2WO6) nanometer sheet XRD figure spectrum.
Fig. 4 is bismuth tungstate (Bi2WO6) the TEM photo of nanometer sheet.
Fig. 5 is bismuth tungstate (Bi2WO6) photo of catalytic degradation rhodamine B different time sections.
Fig. 6 is bismuth tungstate (Bi2WO6) photo of catalytic degradation methylene blue different time sections.
Fig. 7 is bismuth tungstate (Bi2WO6) photo of catalytic degradation methyl orange different time sections.
Fig. 8 is bismuth tungstate (Bi2WO6) the degradation efficiency broken line graph of three kinds of dyestuffs of catalytic degradation.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.The all raw materials participating in reaction system in embodiment are commercially available, Na2WO42H2O、Bi(NO3)35H2O, isooctanol are all purchased from Solution on Chemical Reagents in Shanghai company of Chinese Medicine group, and above chemical reagent is analytical pure, not purified direct use.
First step bismuth tungstate (Bi2WO6) preparation of nanometer sheet and sign
1.1 take 8ml deionized water and 32ml isooctanol respectively to conical flask, are separately added into the Na of 164.9 milligrams wherein2WO42H2Bi (the NO of O and 485.1 milligram3)35H2O, at ambient temperature magnetic agitation 1h, rotating speed is 150rpm.Fully it is dissolved to solid uniformly, obtains settled solution；
1.2, by these two parts of settled solution mixing, obtain suspension solution, at ambient temperature magnetic agitation 1h, and rotating speed is 150rpm；
This solution is proceeded in 50mL teflon-lined autoclave by 1.3, is heated to 180 DEG C in Electric heat oven, naturally cools to room temperature after insulation 20h；
1.4 solution in still is taken out after, take out the supernatant, by bottom solid sample respectively with deionized water and ethanol, each supersound washing twice, after by solid sample centrifugation.Then solid sample is positioned in the vacuum drying oven of 60 DEG C, dries 4-8 hour, obtain Lycoperdon polymorphum Vitt powder；
1.5 take a small amount of Lycoperdon polymorphum Vitt sample powder is bonded on conducting resinl, metal spraying observes pattern, by field emission scanning electron microscope (HitachiS-4800), can be seen that under 20,000 5000 times of (Fig. 1) conditions of amplification, the bismuth tungstate sample journey lamellar prepared is scattered stacking, and dispersibility is better.Adjusting enlargement ratio is 80,000 times, and the structure of single nanometer sheet (Fig. 2), nanometer sheet smooth surface be can be observed, and thickness is unanimous on the whole, is about 50nm.
1.6 by sample powder compacting, as in BrukerD8X x ray diffractometer x, tests, and obtains X ray diffracting spectrum (Fig. 3), it is possible to find out that sample crystallinity is good from diffraction peak shape.
1.7 take little power sample, and ultrasonic disperse is in a small amount of ethanol, and the solution taking 50 microliters drips on copper mesh, at room temperature allows ethanol naturally volatilize.Then sample is observed with high-resolution projection microscope (TEM, JEM-2100, JEOL).In Fig. 4, a is the single sheet sample observed under projection Electronic Speculum.In Fig. 4, b is high-resolution sample photo, it can be seen that its lattice parameter is 0.315nm, and this is consistent with (113) crystal face of rhombic system.
Second step simulated visible light degradation experiment
Bismuth tungstate nano-sheet sample is placed in 60 DEG C by 2.1 to be heated 30 minutes, makes sample have the catalytic performance of the best.
The rhodamine B solution of 2.2 configuration 20mg/mL, takes wherein 30mL and is placed in photocatalysis instrument glass tubing.
2.3 add 30mg Bismuth tungstate nano-sheet sample in glass tubing, are subsequently placed in photocatalysis instrument (Xu Jiang electrical machinery plant), use the middle pressure xenon lamp of 300W, and remove ultraviolet light with filter plate, carry out simulated visible light catalytic condition with this.
2.4 before carrying out light-catalyzed reaction, the solution in glass tubing first carries out the magnetic agitation of 1 hour in dark situation, then samples.The solution centrifugal that will take out, retains upper strata dye solution.
Xenon lamp is energized by 2.5, carries out photocatalytic degradation, every sampling in 1 hour once, totally four times, then according to method processes in 2.4.
2.6 Fig. 5 are Bismuth tungstate nano-sheet sample catalysis rhodamine B (RhB) solution degradation, the dye solution of different time sections, it can be seen that dyestuff has been close to and has been degraded completely.
2.7 Fig. 6 and Fig. 7, are under experiment condition same as described above, Bismuth tungstate nano-sheet sample catalytic degradation methylene blue (MB) and methyl orange (MO) solution, the dye solution that different time sections is extracted.
2.8 Bismuth tungstate nano-sheet synthesized by from Fig. 5-7 it can be seen that in the present invention have efficient organic dyestuff adsorption effect and the photocatalytic degradation effect under visible ray.
2.9 contrast three width figure it can be seen that Bismuth tungstate nano-sheet is for different organic dyestuff simultaneously, and its absorption property and Photocatalytic Degradation Property have bigger difference.It is embodied in, the absorbability of methylene blue (MB) is best, the photocatalytic degradation effect of rhodamine B (RhB) is best, to methyl orange (MO) without substantially absorption and degradation effect.
Dye solution in Fig. 5-7 is carried out UV, visible light test (BWS003, Newark, D), the degradation rate made-time broken line graph by 2.10 Fig. 8, it is possible to more intuitively show the selective absorption catalytic performance that in the present invention, Bismuth tungstate nano-sheet is excellent.
Claims (1)
1. a bismuth tungstate (Bi2WO6) preparation method of flake nano material, it is characterised in that comprise the following steps:
According to Na2WO42H2O and Bi (NO3)35H2The amount of substance of O is sampled than for 1:2, by Na2WO42H2O and Bi (NO3)35H2O is each dissolved separately in deionized water and isooctanol, and deionized water and isooctanol volume ratio are 1:4, carry out the magnetic agitation of certain time respectively, will carry out the magnetic agitation of certain time again after two kinds of solution mixing of gained；
This solution is placed in politef reactor, carries out the hydro-thermal reaction of a period of time at a certain temperature；
The material prepared is passed through conventional washing, ultrasonic, centrifugal, dry, prepare Bi2WO6Flake nano material.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104226212A (en) * | 2014-09-30 | 2014-12-24 | 天津大学 | Preparation of Bi2WO6 spherical cluster with exposed {010} crystal plane families |
| CN105457626A (en) * | 2016-01-25 | 2016-04-06 | 温州大学 | Preparation method and application of concave-surface bismuth tungstate nanosheet electrocatalyst |
| CN107032299B (en) * | 2016-02-03 | 2019-03-08 | 天津大学 | Carry platinum wolframic acid zinc nano material and its application in air-sensitive field |
| CN107162059A (en) * | 2017-06-13 | 2017-09-15 | 浙江大学 | One kind prepares sheet Bi2WO6Method |
| CN107188233A (en) * | 2017-06-13 | 2017-09-22 | 浙江大学 | A kind of Bi2WO6The preparation method of nanometer sheet |
| CN107188234A (en) * | 2017-06-13 | 2017-09-22 | 浙江大学 | A kind of sheet Bi2WO6Preparation method |
| CN107200355A (en) * | 2017-06-13 | 2017-09-26 | 浙江大学 | One kind prepares Bi2WO6The method of nanometer sheet |
| CN108607540B (en) * | 2018-04-12 | 2020-06-19 | 浙江大学 | Preparation method of niobium-doped bismuth tungstate photocatalytic material |
| CN114425371B (en) * | 2021-12-21 | 2023-06-20 | 北京建筑大学 | Method for inducing self-assembly of bismuth-based photocatalytic material by using biosurfactant and application |
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| JP2009166022A (en) * | 2008-01-17 | 2009-07-30 | Inha-Industry Partnership Inst | Photocatalytic agent having titanium oxide-iron titanate joint structure, and its producing method |
| CN102698739A (en) * | 2012-06-15 | 2012-10-03 | 南开大学 | Preparation method of sunlight-responding mesoporous Bi2WO6 microspheres |
| CN102910673A (en) * | 2012-10-19 | 2013-02-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing BiOCl micro-flower nanometer photocatalysis material |
| CN103599771A (en) * | 2013-11-12 | 2014-02-26 | 福州大学 | Bi2WO6 photocatalyst as well as preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009166022A (en) * | 2008-01-17 | 2009-07-30 | Inha-Industry Partnership Inst | Photocatalytic agent having titanium oxide-iron titanate joint structure, and its producing method |
| CN102698739A (en) * | 2012-06-15 | 2012-10-03 | 南开大学 | Preparation method of sunlight-responding mesoporous Bi2WO6 microspheres |
| CN102910673A (en) * | 2012-10-19 | 2013-02-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing BiOCl micro-flower nanometer photocatalysis material |
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