CN109999787A - A kind of zero dimension/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst and preparation method - Google Patents
A kind of zero dimension/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst and preparation method Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002096 quantum dot Substances 0.000 claims abstract description 23
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 claims description 6
- 238000006731 degradation reaction Methods 0.000 claims description 6
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims 1
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 239000002127 nanobelt Substances 0.000 abstract description 8
- 229910002915 BiVO4 Inorganic materials 0.000 abstract description 7
- 238000001354 calcination Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 230000006798 recombination Effects 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000001523 electrospinning Methods 0.000 abstract 1
- 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 8
- 229940043267 rhodamine b Drugs 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000004065 semiconductor Substances 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
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 bismuthino Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts 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
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of zero dimension/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst and preparation methods, specifically pucherite quantum dot is prepared using hydro-thermal method first, zirconium oxychloride and pucherite quantum dot are added in the DMF and aqueous solution of PVP afterwards and carry out ultrasound and stir process, it is uniformly mixed and generates electrospinning colloidal sol and obtain BiVO using method of electrostatic spinning4/ZrO2Tunica fibrosa, after by calcination processing obtain BiVO4/ZrO2Nanobelt photochemical catalyst.It is characteristic of the invention that combining calcine technology to prepare BiVO afterwards using hydro-thermal method in conjunction with two step of method of electrostatic spinning4/ZrO2Nanobelt photochemical catalyst, this can make BiVO4Quantum dot uniformly loads to ZrO2On nanobelt, significantly increase the specific surface area of catalyst, more active sites are made it have, and effectively promotes the efficiency of transmission of electronics by the formation of heterojunction structure and reduces the recombination rate of electron hole, make the catalyst of preparation that there is very high photocatalytic activity.
Description
Technical field
The invention belongs to photocatalysis technology fields, the specially preparation of pucherite quantum dot and zirconia nanopowder carrying material
Method.
Background technique
It is rapidly developed in science and technology, the today's society of industrial economy prosperity, the control of environmental pollution becomes the head that people face
Want one of problem.Environmental-friendly due to having the characteristics that, application of the photocatalysis in curbing environmental pollution increasingly causes people
Concern.It can be used for various aspects, such as water purification, sterilization, self-cleaning, air cleaning, antifog and heat dissipation, and since it has
The advantages that lower cost, Gao Chengxiao, semiconductor light-catalyst are increasingly becoming the research hotspot in processing water pollution field.
Traditional photochemical catalyst TiO2It is used from Fujishima and Honda(Nature 1972,238,37-8 in 1972)
As electrode by water electrolysis at H2And O2Since, since there is many advantages, such as at low cost, high-efficient, stability is good to cause people for it
Extensive concern.But it since its biggish forbidden bandwidth (~ 3.2eV) determines that it cannot absorb visible light, seriously limits
It is applied.In order to overcome this disadvantage, people give great concern to novel photocatalyst, wherein people is most allowed to feel excited
It is visible light activity bismuthino photochemical catalyst, and pucherite is therefrom shown one's talent with its lesser band gap (~ 2.4eV).But it passes through
It crosses people to study for a long period of time discovery, although its light absorption range is bigger, single pucherite semiconductor light-catalyst is higher due to its
Electron-hole recombination rate causes its photocatalytic activity unsatisfactory, and can be effective by constructing heterojunction structure with other substances
Reduce the compound of electron hole.Pucherite heterojunction structure photocatalysis is studied there are many seminar at present, such as
Meryam Zalfani(J.Mater.Chem.A, 2014,00,1-3) et al. be prepared for BiVO using hydro-thermal method4/TiO2It is heterogeneous
Structure nanometer composite material finds the relatively simple BiVO of its degradation efficiency to rhodamine B4Nano particle improves about four
Times.And opposite TiO2, ZrO2With its more stable property, and the ZrO that electrostatic spinning obtains relatively2Nanobelt and BiVO4
Quantum dot has bigger specific surface area, its suction can be made by being loaded to pucherite quantum dot by two-step method on zirconia nanopowder band
Luminosity greatly enhances, and is formed on its surface more active sites, these advantages are all very beneficial for its drop to pollutant
The promotion of solution and photocatalysis efficiency.
Summary of the invention
Obtaining object of the present invention is to the heterojunction structure using building pucherite quantum dot and zirconia nanopowder band has bloom
The catalyst of catalytic activity.
To achieve the purpose of the present invention, the following technical schemes are provided:
A kind of zero dimension/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst and preparation method, comprises the following steps that
(1) enuatrol is placed in deionized water, and the sodium oleate solution that 30min obtains mass concentration 0.1% is stirred at room temperature
A；
(2) bismuth nitrate and ammonium metavanadate are added in solution A, stir 10 ~ 10min at room temperature；
(3) solution A is added in reaction kettle and 6 ~ 10h is reacted in heating in 90 DEG C of baking oven；
(4) by solution after the reaction was completed be repeatedly centrifuged and by obtained material using ethyl alcohol and deionized water repeatedly wash with
Obtain pucherite quantum dot；
(5) polyvinylpyrrolidone (PVP) is dissolved in the in the mixed solvent of N,N-dimethylformamide and a small amount of deionized water simultaneously
Stir evenly acquisition solution B；
(6) zirconium oxychloride and pucherite quantum dot are added in the solution B that PVP mass concentration is about 10 ~ 20%, ultrasound 20 ~
2h is stirred at room temperature after 40min and obtains spinnable colloidal sols；
(7) spinnable colloidal sols obtained are added in syringe needle tube, carry out electrostatic spinning；
(8) tunica fibrosa made from electrostatic spinning is calcined, obtains the zirconia nanopowder band of pucherite quantum dot load.
, according to the invention it is preferred to, in step (1), the mass concentration of enuatrol is 0.09%.
, according to the invention it is preferred to, in step (2), the mass concentration of bismuth nitrate is 0.12%, and the quality of ammonium metavanadate is dense
Degree is 0.1%.
, according to the invention it is preferred to, in step (3), heating time 8h.
, according to the invention it is preferred to, in step (5), PVP mass concentration is 10%.
, according to the invention it is preferred to, in step (6), zirconium oxychloride and pucherite quantum dot molar ratio are 1:1.
, according to the invention it is preferred to, in step (8), the temperature of calcining is 500 DEG C, and calcining rate is 1 DEG C/min, heat preservation
Time is 60min.
The present invention is to construct heterogeneous structural nano rank photochemical catalyst using pucherite quantum dot and zirconia nanopowder band, will
Pucherite quantum dot loads on zirconia nanopowder band, greatly increases the specific surface area of zirconia nanopowder band, enhances catalysis
Agent further improves photocatalytic activity to the absorbability of sunlight.System is combined with electrostatic spinning two-step method using hydro-thermal
Standby heterojunction structure photochemical catalyst out, has effectively promoted electronics transfer and has greatly reduced the recombination rate of photo-generate electron-hole,
Significantly improve the photocatalysis efficiency of photochemical catalyst.
Detailed description of the invention
Fig. 1 is the experiment flow figure of present example 1.
Fig. 2 is the XRD diagram of present example 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of present example 1.
Fig. 4 is the transmission electron microscope picture of present example 1.
Fig. 5 is the pollution degradation property contrast curve chart of present example 1.
Fig. 6 is the ultraviolet curve of rhodamine B degradation of present example 1.
Fig. 7 is the nitrogen adsorption desorption and pore size distribution curve of present example 1.
Specific embodiment
Following embodiment is intended to illustrate invention rather than limitation of the invention further.
Embodiment 1:
(1) 0.730g enuatrol is placed in 80mL deionized water, and 30min acquisition mass concentration is stirred at room temperature and is about
0.1% sodium oleate solution A；
(2) 0.097g bismuth nitrate and 0.080g ammonium metavanadate are added in solution A, stir 10 ~ 10min at room temperature；
(3) solution A is added in reaction kettle and 8h is reacted in heating in 90 DEG C of baking oven；
(4) by solution after the reaction was completed be repeatedly centrifuged and by obtained material using ethyl alcohol and deionized water repeatedly wash with
Obtain pucherite quantum dot；
(5) 1.0g polyvinylpyrrolidone (PVP) is dissolved in the mixing of 10mL N,N-dimethylformamide and 1mL deionized water
In solvent and stir evenly acquisition solution B；
(6) 0.064g zirconium oxychloride and 0.065g pucherite quantum dot are added in solution B, room temperature after 20 ~ 40min of ultrasound
It stirs 2h and obtains spinnable colloidal sols；
(7) spinnable colloidal sols obtained are added in syringe needle tube, carry out electrostatic spinning；
(8) tunica fibrosa made from electrostatic spinning is calcined, obtains the zirconia nanopowder band of pucherite quantum dot load；
Electron-microscope scanning is carried out to product made from this example, as shown, the nanobelt size of preparation is in 100 ~ 150nm or so.
Embodiment 2:
(1) 0.730g enuatrol is placed in 80mL deionized water, and 30min acquisition mass concentration is stirred at room temperature and is about
0.1% sodium oleate solution A；
(2) 0.097g bismuth nitrate and 0.080g ammonium metavanadate are added in solution A, stir 10 ~ 10min at room temperature；
(3) solution A is added in reaction kettle and 6h is reacted in heating in 90 DEG C of baking oven；
(4) by solution after the reaction was completed be repeatedly centrifuged and by obtained material using ethyl alcohol and deionized water repeatedly wash with
Obtain pucherite quantum dot.
Embodiment 3:
(1) 1.0g polyvinylpyrrolidone (PVP) is dissolved in the mixing of 10mL N,N-dimethylformamide and 1mL deionized water
In solvent and stir evenly acquisition solution A；
(2) 0.064g zirconium oxychloride is added in solution A, 2h is stirred at room temperature after 20 ~ 40min of ultrasound and obtains spinnable colloidal sols；
(3) spinnable colloidal sols obtained are added in syringe needle tube, carry out electrostatic spinning；
(4) tunica fibrosa made from electrostatic spinning is calcined, obtains zirconia nanopowder band.
Experimental example
It is tested by the absorption of nitrobenzene (NB) and rhodamine B (RhB) and photocatalytic degradation, test b iVO4/ZrO2Hetero-junctions
The photocatalysis performance of structure nanobelt.
Light-catalyzed reaction carries out under room temperature in cylindrical glass container, is reacted using light source immersion, and light source is
800W xenon lamp evaluates the pollutant cleaning performance of heterogeneous structural nano band using NB and RhB as simulating pollution object.Experimentation
In, respectively by 60mg BiVO4Quantum dot, ZrO2Nanobelt and BiVO4/ZrO2Heterogeneous structural nano carry sample is placed in NB
(RhB) solution (50mg/L), magnetic agitation and dark reaction 60min under dark condition, works as NB(RhB) solution and sample reach suction
Xenon lamp is opened after attached balance carries out illumination.4mL is sampled every 30min, ultraviolet-visible is used after syringe filters filter
The absorbance of photometric determination filtrate simultaneously calculates remaining NB(RhB) concentration.Fig. 5 is BiVO prepared by embodiment 14/ZrO2It is different
Matter structure nano band and BiVO4Quantum dot and ZrO2The degradation efficiency of nanobelt compares, it can be seen that prepared by embodiment 1
BiVO4/ZrO2Heterogeneous structural nano band degradation efficiency highest.
Claims (7)
1. a kind of zero dimension/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst, which is characterized in that the catalyst by
Pucherite quantum dot, zirconia nanopowder band composition.
2. zero dimension according to claim 1/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst, feature
It is, the catalyst pucherite is monoclinic phase, and zirconium oxide is tetragonal phase.
3. zero dimension according to claim 1/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst, feature
It is, by the amount percentages of substance: vanadic acid bi content 50%, zirconia content 50%.
4. zero dimension according to claim 1/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst, feature
It is, the specific surface area of the catalyst is 44.45m2/g。
5. zero dimension according to claim 1/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst, feature
It is, the catalyst reaches 95.1% to 210 minutes degradation rates of 50mg/L nitrobenzene under visible light.
6. a kind of zero dimension/one-dimensional heterojunction structure pucherite/zirconia nanopowder band photochemical catalyst and preparation according to claim 1
Method, it is characterised in that solvent is deionized water, at least one of n,N-Dimethylformamide.
7. a kind of zero dimension described in claim 1/one-dimensional heterojunction structure pucherite/preparation side of the zirconia nanopowder with photochemical catalyst
Method comprises the following steps that
(1) enuatrol is placed in deionized water, and the sodium oleate solution that 30min obtains mass concentration 0.1% is stirred at room temperature
A；
(2) bismuth nitrate and ammonium metavanadate are added in solution A, stir 10 ~ 20min at room temperature；
(3) solution A is added in reaction kettle and 8 ~ 12h is reacted in heating in 90 DEG C of baking oven；
(4) by solution after the reaction was completed be repeatedly centrifuged and by obtained material using ethyl alcohol and deionized water repeatedly wash with
Obtain pucherite quantum dot；
(5) polyvinylpyrrolidone (PVP) is dissolved in the mixing of N,N-dimethylformamide and a small amount of deionized water and is stirred
Uniformly obtain solution B；
(6) zirconium oxychloride and pucherite quantum dot are added in the solution B that PVP mass concentration is about 10 ~ 20%, ultrasound 20 ~
2 h are stirred at room temperature after 40min and obtain spinnable colloidal sols；
(7) spinnable colloidal sols obtained are added in syringe needle tube, carry out electrostatic spinning；
(8) tunica fibrosa made from electrostatic spinning is calcined, obtains the zirconia nanopowder band of pucherite quantum dot load.
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Application publication date: 20190712 |