CN106277039A - A kind of cellular SnO2semiconductor light-catalyst and preparation method thereof - Google Patents
A kind of cellular SnO2semiconductor light-catalyst and preparation method thereof Download PDFInfo
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- CN106277039A CN106277039A CN201610574693.4A CN201610574693A CN106277039A CN 106277039 A CN106277039 A CN 106277039A CN 201610574693 A CN201610574693 A CN 201610574693A CN 106277039 A CN106277039 A CN 106277039A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000001413 cellular effect Effects 0.000 title claims abstract description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 37
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004065 semiconductor Substances 0.000 claims abstract description 13
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 12
- 239000011941 photocatalyst Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 15
- 239000011651 chromium Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 229910020923 Sn-O Inorganic materials 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241001466460 Alveolata Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000006136 alcoholysis reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 125000006267 biphenyl group Chemical group 0.000 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 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241000256844 Apis mellifera Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical group 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 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 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
-
- B01J35/39—
-
- B01J35/40—
-
- B01J35/56—
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- 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
Abstract
The invention discloses a kind of cellular SnO2Semiconductor light-catalyst and preparation method thereof, photocatalyst reaction raw materials includes stannic chloride pentahydrate, natrium carbonicum calcinatum, acetone, dehydrated alcohol, when the mol ratio of stannic chloride pentahydrate and natrium carbonicum calcinatum controls as 1:6, use simple maneuverable solid-phase synthesis, at 540 DEG C, heat 2h synthesis obtain a kind of cellular SnO2.Preparation technology of the present invention is simple, easy and simple to handle, uses the SnO that 0.3g prepares2Irradiate after 120min with ultraviolet light in 60W day, to the percent reduction of 300ml 50mg/LCr (VI) up to 87.8%, it is clear that the catalyst effect of honeycomb shape is preferable, can be with Cr VI in the removal water of low energy consumption.
Description
Technical field
The present invention relates to photocatalyst preparing technical field, a kind of cellular SnO2Semiconductor light-catalyst and
Preparation method.
Background technology
Photocatalitic Technique of Semiconductor may utilize sunlight and carries out catalyzing manufacturing of hydrogen, oxygen processed, processes water pollutant, gradually develops
Becoming an emerging green technology, wherein light source and photocatalyst are two key elements of photocatalysis technology application.
Semiconductor light-catalyst the most more typically is metal-oxide and sulfide (TiO2、ZnO、SnO2、WO3、Fe3O4, CdS etc.),
And obtained by the activity improvement of semiconductor compound, doping, dye-sensitized semiconductor photocatalyst.
SnO2Modal structure is tetragonal crystal system rutile, SnO2Structure cell is body-centered-orthorhomic parallelepiped, by two Sn
With four O atom compositions, lattice paprmeter is that a=b=0.4737nm, c=0.3186nm, c/a=0.637, body-centered and drift angle are
Sn ion, ligancy is 6, and the ligancy of O ion is 3.Within 1962, Taguchi finds the SnO of sintering2Micro-in air of pottery
Amount active gases is more sensitive, and stability is the highest, is the gas sensitive of a kind of excellence；SnO2As negative temperature coefficient heat-sensitive
Material, have also been obtained extensively application at the aspect such as industrial and medical；This external raising material nonlinearity coefficient, improve the pressure of material
The research of quick performance also has the most considerable application prospect.SnO2Nano material has good photocatalysis performance, photoelectric properties
With air-sensitive performance etc., can be as environment purification, the ideal material that produces display, solaode, gas sensor etc..
SnO2As the typical N-shaped wide bandgap semiconductor materials that a kind of energy gap is 3.5-4.0eV, it is the TiO that continues2Afterwards
Most one of photocatalyst of future.SnO2Except having and TiO2Outside similar rutile structure, it is also possible to cover TiO2Light
Spectral limit, in conjunction with the various excellent properties being had so that it is become the TiO that continues2The most most one of photocatalyst of future.?
Some research shows porous SnO using interfacial reaction to prepare2Material has bigger specific surface area, uses it for photocatalysis fall
The methyl orange solved in aqueous solution test result indicate that, porous SnO under conditions of experiment condition is identical2The photocatalysis performance of material
Ratio Degussa P25TiO2More preferably.Conventional SnO2The synthetic method of nano material has: water (or solvent) full-boiled process, solid phase synthesis
Method, sol-gel process, chemical vapour deposition technique, template etc., be correlated with SnO2The report of photocatalyst, but honeybee
Nest shape SnO2Semiconductor light-catalyst is not also developed at present.
Summary of the invention
It is an object of the invention to provide a kind of cellular SnO2Semiconductor light-catalyst and preparation method thereof, on solving
State the problem proposed in background technology.
For achieving the above object, the present invention provides following technical scheme: a kind of cellular SnO2Semiconductor light-catalyst and
Its preparation method, photocatalyst reaction raw materials includes stannic chloride pentahydrate, natrium carbonicum calcinatum, acetone, dehydrated alcohol.
Preferably, its preparation method comprises the following steps:
A, first sodium carbonate being placed in vacuum drying oven drying, drying baker temperature arranges 100 DEG C；
B, weigh 30mmol natrium carbonicum calcinatum and be placed on agate mortar, be added dropwise over 1ml acetone, grind 10min thin to powder
Greasy uniformly；
C, after acetone volatilizees completely, in the reactant that step B obtains add 10mmol stannic chloride pentahydrate, tentatively stir
Mix mixing 5min, be added dropwise over 2ml dehydrated alcohol；
D, be persistently fully ground 15min after, reactant step C obtained proceeds to, in crucible, crucible is placed in Muffle furnace
In at 540 DEG C calcine 2h；
E, question response naturally cool to room temperature after terminating, take out crucible, and add deionized water immersion wherein；
F, will crucible precipitate respectively with ionized water and absolute ethanol washing, sucking filtration again；
G, the sample finally step F obtained are dried 4h in vacuum drying oven, and drying baker temperature is 80 DEG C, grinds standby
With.
Compared with prior art, the invention has the beneficial effects as follows: preparation technology of the present invention is simple, easy and simple to handle, use
The SnO that 0.3g prepares2Irradiate after 120min with ultraviolet light in 60W day, to the percent reduction of 300ml 50mg/L Cr (VI) up to
87.8%, it is clear that the catalyst effect of honeycomb shape is preferable, can be with Cr VI in the removal water of low energy consumption.
Figure of description
Fig. 1 is the SnO that the present invention prepares2XRD spectra；
Fig. 2 is the SnO that the present invention prepares2FESEM figure；
Fig. 3 is the SnO that the present invention prepares2FTIR spectrogram；
Fig. 4 is the SnO that the present invention prepares2UV-Vis spectrogram；
Fig. 5 is the SnO that the present invention prepares2EgCurve chart；
Fig. 6 be the stannic chloride pentahydrate of the present invention, natrium carbonicum calcinatum mol ratio be SnO prepared by 1:62Photocatalytic activity
Curve chart.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment
It is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under not making creative work premise, broadly falls into the model of present invention protection
Enclose.
The present invention provides a kind of technical scheme: a kind of cellular SnO2Semiconductor light-catalyst and preparation method thereof, light is urged
Agent reaction raw materials includes stannic chloride pentahydrate, natrium carbonicum calcinatum, acetone, dehydrated alcohol.
The preparation method of the present invention comprises the following steps:
A, first sodium carbonate being placed in vacuum drying oven drying, drying baker temperature arranges 100 DEG C；
B, weigh 30mmol natrium carbonicum calcinatum and be placed on agate mortar, be added dropwise over 1ml acetone, grind 10min thin to powder
Greasy uniformly；
C, after acetone volatilizees completely, in the reactant that step B obtains add 10mmol stannic chloride pentahydrate, tentatively stir
Mix mixing 5min, be added dropwise over 2ml dehydrated alcohol；
D, be persistently fully ground 15min after, reactant step C obtained proceeds to, in crucible, crucible is placed in Muffle furnace
In at 540 DEG C calcine 2h；
E, question response naturally cool to room temperature after terminating, take out crucible, and add deionized water immersion wherein；
F, will crucible precipitate respectively with ionized water and absolute ethanol washing, sucking filtration again；
G, the dry 4h in vacuum drying oven finally step F obtained, drying baker temperature is 80 DEG C, grinds standby.
The photocatalyst preparing the present invention carries out chromic experiment in treatment with ultraviolet light water: experiment uses laboratory certainly
The ultraviolet catalytic reactor of system, is mainly made up of 60w uviol lamp and magnetic force heating stirrer.This experiment is with the heavy chromium of 50mg/L
Acid potassium solution is as simulating pollution waste water.Concrete experimentation is: by 0.3g SnO2Put into the above-mentioned simulated wastewater of 300ml
In, it is placed on magnetic stirring apparatus at room temperature lucifuge stirring 1h, afterwards during illumination reaction, at set intervals from burning
Take out about 4mL suspension in Bei, be filtrated to get clear liquid through filter, use diphenyl phosphinylidyne two hydrazine method to measure each group of clear liquid
The content of middle Cr (VI), tests the maximum absorption wavelength of its violet complex formed at diphenyl phosphinylidyne two hydrazine and Cr (VI)
(λmax=540nm) absorbance at place, and record experimental data.In the range of experimental concentration, Cr (VI) concentration becomes with its absorbance
Direct ratio, thus available equation below:
Degradation rate=(the A of Cr (VI)0-At)/A0× 100%
The absorbance surveyed is changed into the degradation rate of Cr (VI), thus learns degradation effect, wherein: A0For illumination 0min
Time etching solution absorbance, AtFor the absorbance of etching solution during illumination tmin.
The product SnO that the present invention is prepared2Carry out XRD analysis: as it is shown in figure 1, all of diffraction maximum is golden with tetragonal crystal system
Red stone structure SnO2Standard diagram consistent, occur without miscellaneous peak, show that the purity of product is high.Pass through formula:
D=K λ/Bcos θ
Estimation SnO2Size be 4nm, wherein, D is crystallite dimension, and λ is X-ray wavelength, and B is the half-peak of diffraction maximum
Width, θ is the angle of diffraction, and K is Scherrer constant, often takes 0.9.
The product preparing the present invention carries out FESEM analysis: as shown in Figure 2.A small amount of little of nanometer as we can see from the figure
The cake mass that grain is reunited, more present is the cellular pore space structure in agglomerate body, and the diameter of cellular cavity exists
50nm-100nm.And SnO2Many formation little granules of nanometer or short grained aggregate during common hydro-thermal and solid phase synthesis,
The alveolate texture formed in the method for the invention.The formation of said structure can be from SnO2Reaction of formation mechanism explain；
SnO2Reaction mechanism be, first SnCl4It is dissolved in its water of crystallization, and following chemical reaction occurs:
Sn4++4H2O→Sn(OH)4+4H+
Sn4++4CH3CH2OH→Sn(OH)4+4CH3CH2 +
Sn(OH)4→SnO2+2H2O
Due to SnCl4Hydrolysis and alcoholysis reaction is occurred to form unbodied Sn (OH)4, the most at high temperature Sn (OH)4Occur
Dehydrating condensation and crystallization, finally give SnO2.When system acidity is relatively low, beneficially SnCl4Hydrolysis, and when acidity relatively
Gao Shi, hydrolysis is restricted, the SnO obtained2Negligible amounts, SnO2Exist with nano-particle.The sodium carbonate added in the method
It is a kind of strong base-weak acid salt, there is certain alkalescence, it is possible to effectively regulate the pH of reaction system, control hydrolysis and alcoholysis process,
Form the alveolate texture of present invention synthesis.
The product preparing the present invention carries out FTIR spectrum analysis as shown in Figure 3: SnO2The vibration performance peak of middle Sn-O is
660cm-1.667cm in Fig. 3-1What neighbouring absworption peak was corresponding is the Sn-O stretching vibration of O-Sn-O；530cm-1The peak at place is then
The Sn-O stretching vibration of Sn-O-H, 3421cm-1、1634cm-1The peak occurred at Zuo You is that the flexible of O-H in physical absorption water shakes
Dynamic, bending vibration characteristic peak.
The UV-Vis of the product preparing the present invention analyzes: test product SnO2UV-Vis DRS spectrum, and make
With formula:
F(R∞)=(1-R∞)2/2R∞=α/S=AC/S
R∞=Rsample/RBaSO4
It is translated into absorption spectrum, from fig. 4, it can be seen that product SnO2At ultraviolet region, there is the highest light and absorb energy
Power.Wherein F (R∞), S, α, R, C and A be respectively Kubelka-Munk function, scattering coefficient, absorptance, reflectivity, absorbent
The concentration planted and absorbance.SnO2It is direct band-gap semicondictor material, so the band gap magnitude (E of productg) can be with direct band gap half
The light absorption approach formula of conductor:
α h ν=B (h ν-Eg)1/2
Wherein α is absorptance, and B is the constant that material person's character is relevant, and h ν is the energy of single photon.So more than Zong He
Theory, with (F (R ∞) h ν)2For vertical coordinate, (h ν) is abscissa mapping, and gained diagram is shown in Fig. 5, its tangent line is extended to F (R
After ∞)=0, estimation product band gap magnitude is 3.2eV.
The product preparing the present invention carries out the experiment of Cr VI in treatment with ultraviolet light water: with the 50mg/L's of 300ml
K2Cr2O7Solution is simulating pollution thing, respectively with the made SnO of 0.3g2Photocatalyst carries out light under 60W day ultraviolet light source
Catalytic degradation, experimental result is as shown in Figure 6.SnO in figure2The system of the photocatalytic degradation simulating pollution thing of product adds
2ml citric acid, line 0ml is then not to adding citric acid in photocatalytic process.By Fig. 6 to find out, add SnO2Photocatalysis
Agent is compared without photocatalyst obvious to the degradation effect of Cr (VI)；After UV illumination penetrates 120min, SnO2Photocatalysis
The efficiency of degraded Cr (VI) is 87.8%.It addition, as seen from Figure 6, divide in light-catalyzed reaction system in photocatalytic process
Do not add 0ml and 2ml citric acid to SnO2Photocatalysis effect has significant difference, and after adding citric acid, catalytic effect can improve,
This is because citric acid plays the effect of hole agent for capturing.
Preparation technology of the present invention is simple, easy and simple to handle, uses the SnO that 0.3g prepares2Irradiate with ultraviolet light in daily 60W day
After 120min, to the percent reduction of 300ml 50mg/L Cr (VI) up to 87.8%, it is clear that the catalyst effect of honeycomb shape
Preferably, can be with Cr VI in the removal water of low energy consumption.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, permissible
Understand and these embodiments can be carried out multiple change without departing from the principles and spirit of the present invention, revise, replace
And modification, the scope of the present invention be defined by the appended.
Claims (2)
1. a cellular SnO2Semiconductor light-catalyst and preparation method thereof, it is characterised in that: photocatalyst reaction raw materials includes
Stannic chloride pentahydrate, natrium carbonicum calcinatum, acetone, dehydrated alcohol.
The cellular SnO of one the most according to claim 12Semiconductor light-catalyst, it is characterised in that: its preparation method bag
Include following steps:
A, first sodium carbonate being placed in vacuum drying oven drying, drying baker temperature arranges 100 DEG C；
B, weigh 30mmol natrium carbonicum calcinatum and be placed on agate mortar, be added dropwise over 1ml acetone, grind 10min fine and smooth all to powder
Even；
C, after acetone volatilizees completely, the reactant that step B obtains adds 10mmol stannic chloride pentahydrate, preliminary stirring is mixed
Close 5min, be added dropwise over 2ml dehydrated alcohol；
D, be persistently fully ground 15min after, reactant step C obtained proceeds in crucible, is placed in Muffle furnace by crucible
2h is calcined at 540 DEG C；
E, question response naturally cool to room temperature after terminating, take out crucible, and add deionized water immersion wherein；
F, will crucible precipitate respectively with ionized water and absolute ethanol washing, sucking filtration again；
G, the sample finally step F obtained are dried 4h in vacuum drying oven, and drying baker temperature is 80 DEG C, grinds standby.
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| CN110918007A (en) * | 2019-11-04 | 2020-03-27 | 江苏一夫新材料产业技术研究院有限公司 | PVP polymerized SnO2-graphene aerogels and method for the production thereof |
| CN113663708A (en) * | 2021-08-16 | 2021-11-19 | 中化学朗正环保科技有限公司 | High-efficiency photocatalytic material and preparation method and application thereof |
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|---|---|---|---|---|
| CN102153133A (en) * | 2011-03-17 | 2011-08-17 | 扬州大学 | Method for preparing controllable ordered porous tin dioxide nano structures |
| CN103739007A (en) * | 2013-12-30 | 2014-04-23 | 扬州大学 | Preparation of porous tin dioxide nano structure with controllable size by employing template method |
| CN105749902A (en) * | 2016-01-25 | 2016-07-13 | 扬州大学 | Preparation method of efficient single-phase SnO2 photocatalyst |
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| CN102153133A (en) * | 2011-03-17 | 2011-08-17 | 扬州大学 | Method for preparing controllable ordered porous tin dioxide nano structures |
| CN103739007A (en) * | 2013-12-30 | 2014-04-23 | 扬州大学 | Preparation of porous tin dioxide nano structure with controllable size by employing template method |
| CN105749902A (en) * | 2016-01-25 | 2016-07-13 | 扬州大学 | Preparation method of efficient single-phase SnO2 photocatalyst |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110918007A (en) * | 2019-11-04 | 2020-03-27 | 江苏一夫新材料产业技术研究院有限公司 | PVP polymerized SnO2-graphene aerogels and method for the production thereof |
| CN110918007B (en) * | 2019-11-04 | 2022-04-22 | 江苏一夫新材料产业技术研究院有限公司 | PVP polymerized SnO2-graphene aerogels and method for the production thereof |
| CN113663708A (en) * | 2021-08-16 | 2021-11-19 | 中化学朗正环保科技有限公司 | High-efficiency photocatalytic material and preparation method and application thereof |
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