CN106277039B - 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 PDF

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CN106277039B
CN106277039B CN201610574693.4A CN201610574693A CN106277039B CN 106277039 B CN106277039 B CN 106277039B CN 201610574693 A CN201610574693 A CN 201610574693A CN 106277039 B CN106277039 B CN 106277039B
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sno
catalyst
crucible
acetone
absolute ethyl
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CN106277039A (en
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李靖
徐艳
傅萍
曹译文
石庆柱
王晓辉
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Xuzhou University of Technology
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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
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/50—Agglomerated particles
    • 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

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Abstract

The invention discloses a kind of cellular SnO2Semiconductor light-catalyst and preparation method thereof, photochemical catalyst reaction raw materials include stannic chloride pentahydrate, natrium carbonicum calcinatum, acetone, absolute ethyl alcohol, and the mol ratio control of stannic chloride pentahydrate and natrium carbonicum calcinatum is 1:When 6, using simple maneuverable solid-phase synthesis, heating 2h synthesizes to obtain a kind of cellular SnO at 540 DEG C2.Preparation technology of the present invention is simple, easy to operate, using SnO made from 0.3g2In 60W days with after ultraviolet light 120min, to 300ml 50mg/LCr (VI) percent reduction up to 87.8%, it is clear that the catalyst effect of honeycomb shape is preferable, can remove Cr VI in water removal with low energy consumption.

Description

A kind of cellular SnO2Semiconductor light-catalyst and preparation method thereof
Technical field
The present invention relates to photochemical catalyst preparing technical field, specially a kind of cellular SnO2Semiconductor light-catalyst and its Preparation method.
Background technology
Photocatalitic Technique of Semiconductor can carry out catalyzing manufacturing of hydrogen, oxygen processed, processing water pollutant, gradually development using sunshine As an emerging green technology, wherein light source and photochemical catalyst is two key elements of photocatalysis technology application. Semiconductor light-catalyst more typical at present is metal oxide and sulfide (TiO2、ZnO、SnO2、WO3、Fe3O4, CdS etc.), And by the activity improvement of semiconductor obtain it is compound, doping, dye-sensitized semiconductor photochemical catalyst.
SnO2Most common structure is tetragonal crystal system rutile, SnO2Structure cell is body-centered-orthorhomic parallelepiped, by two Sn Formed with four O atoms, lattice constant a=b=0.4737nm, c=0.3186nm, c/a=0.637, body-centered and drift angle are Sn ions, ligancy 6, the ligancy of O ions is 3.Taguchi has found the SnO of sintering within 19622Ceramics are in air Trace active gas is more sensitive, and stability is very high, is a kind of excellent gas sensitive；SnO2As negative temperature coefficient heat Quick material, also it is widely applied industrial and medical etc.；In addition improving material nonlinearity coefficient, improving material The research of voltage-dependent characteristic also has very considerable application prospect.SnO2Nano material has good photocatalysis performance, photo electric Energy and air-sensitive performance etc., can be as the ideal material of environment purification, production display, solar cell, gas sensor etc..
SnO2It is after TiO as the typical n-type wide bandgap semiconductor materials that a kind of energy gap is 3.5-4.0eV2Afterwards Most one of photochemical catalyst of future.SnO2Except having and TiO2Outside similar rutile structure, TiO can also be covered2Light Spectral limit, with reference to the various excellent properties possessed, become after TiO2Most one of photochemical catalyst of future afterwards. Some research shows the porous SnO prepared using interfacial reaction2Material has larger specific surface area, uses it for photocatalysis drop Solve the methyl orange in the aqueous solution test result indicates that, in experiment condition porous SnO under the same conditions2The photocatalysis performance of material Than Degussa P25TiO2More preferably.Conventional SnO2The synthetic method of nano material has：The hot method of water (or solvent), synthesis in solid state Method, sol-gel process, chemical vapour deposition technique, template etc., has related SnO at present2The report of photochemical catalyst, but honeybee Nest shape SnO2Semiconductor light-catalyst is not developed also at present.
The content of the invention
It is an object of the invention to provide a kind of cellular SnO2Semiconductor light-catalyst and preparation method thereof, with solution State the problem of being proposed in background technology.
To achieve the above object, the present invention provides following technical scheme：A kind of cellular SnO2Semiconductor light-catalyst and Its preparation method, photochemical catalyst reaction raw materials include stannic chloride pentahydrate, natrium carbonicum calcinatum, acetone, absolute ethyl alcohol.
Preferably, its preparation method comprises the following steps：
A, first sodium carbonate is placed in vacuum drying chamber and dried, 100 DEG C of drying box temperature setting；
B, 30mmol natrium carbonicum calcinatums are weighed and are placed on agate mortar, 1ml acetone is added dropwise, grinding 10min is thin to powder It is greasy uniform；
C, after acetone completely volatilization, 10mmol stannic chloride pentahydrates is added in the reactant that step B is obtained, are tentatively stirred Mixing 5min is mixed, 2ml absolute ethyl alcohols are added dropwise；
D, after being persistently fully ground 15min, the obtained reactants of step C is transferred in crucible, crucible is placed in Muffle furnace In calcine 2h at 540 DEG C；
E, room temperature is naturally cooled to after question response terminates, takes out crucible, and adds deionized water immersion thereto；
F, will be precipitated again in crucible respectively with ionized water and absolute ethyl alcohol washing, suction filtration；
G, the sample for finally obtaining step F dries 4h in vacuum drying chamber, and drying box temperature is 80 DEG C, and grinding is standby With.
Compared with prior art, the beneficial effects of the invention are as follows：Preparation technology of the present invention is simple, easy to operate, uses SnO made from 0.3g2It is reachable to 300ml 50mg/L Cr (VI) percent reduction in 60W days with after ultraviolet light 120min 87.8%, it is clear that the catalyst effect of honeycomb shape is preferable, can remove Cr VI in water removal with low energy consumption.
Figure of description
Fig. 1 is SnO produced by the present invention2XRD spectra；
Fig. 2 is SnO produced by the present invention2FESEM figure；
Fig. 3 is SnO produced by the present invention2FTIR spectrograms；
Fig. 4 is SnO produced by the present invention2UV-Vis spectrograms；
Fig. 5 is SnO produced by the present invention2EgCurve map；
Fig. 6 is the stannic chloride pentahydrate of the present invention, natrium carbonicum calcinatum mol ratio is 1:6 SnO prepared2Photocatalytic activity Curve map.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment Only part of the 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 the premise of creative work is not made, belong to the model that the present invention protects Enclose.
The present invention provides a kind of technical scheme：A kind of cellular SnO2Semiconductor light-catalyst and preparation method thereof, light are urged Agent reaction raw materials include stannic chloride pentahydrate, natrium carbonicum calcinatum, acetone, absolute ethyl alcohol.
The preparation method of the present invention comprises the following steps：
A, first sodium carbonate is placed in vacuum drying chamber and dried, 100 DEG C of drying box temperature setting；
B, 30mmol natrium carbonicum calcinatums are weighed and are placed on agate mortar, 1ml acetone is added dropwise, grinding 10min is thin to powder It is greasy uniform；
C, after acetone completely volatilization, 10mmol stannic chloride pentahydrates is added in the reactant that step B is obtained, are tentatively stirred Mixing 5min is mixed, 2ml absolute ethyl alcohols are added dropwise；
D, after being persistently fully ground 15min, the obtained reactants of step C is transferred in crucible, crucible is placed in Muffle furnace In calcine 2h at 540 DEG C；
E, room temperature is naturally cooled to after question response terminates, takes out crucible, and adds deionized water immersion thereto；
F, will be precipitated again in crucible respectively with ionized water and absolute ethyl alcohol washing, suction filtration；
G, 4h is finally dried in vacuum drying chamber by what step F was obtained, drying box temperature is 80 DEG C, and grinding is standby.
The experiment of Cr VI in treatment with ultraviolet light water is carried out to photochemical catalyst produced by the present invention：Experiment uses laboratory certainly The ultraviolet catalytic reactor of system, is mainly made up of 60w uviol lamps and magnetic force heating stirrer.This experiment is with 50mg/L heavy chromium Sour potassium solution is as simulating pollution waste water.Specifically experimentation is：By 0.3g SnO2It is put into 300ml above-mentioned simulated wastewater In, lucifuge stirring 1h at room temperature is placed on magnetic stirring apparatus, afterwards during illumination reaction, at regular intervals from burning About 4mL suspensions are taken out in cup, clear liquid is filtrated to get by filter, each group clear liquid is determined using the hydrazine method of diphenyl phosphinylidyne two The content of middle Cr (VI), test its maximum absorption wavelength in the hydrazine of diphenyl phosphinylidyne two and Cr (VI) violet complex formed (λmax=540nm) place absorbance, and record experimental data.In the range of experimental concentration, Cr (VI) concentration and its absorbance It is directly proportional, thus using equation below：
Cr (VI) degradation rate=(A0-At)/A0× 100%
The absorbance surveyed is changed into Cr (VI) degradation rate, so as to learn degradation effect, wherein：A0For illumination 0min When etching solution absorbance, AtFor illumination tmin when etching solution absorbance.
To product SnO produced by the present invention2Carry out XRD analysis：As shown in figure 1, all diffraction maximums and tetragonal crystal system gold Red stone structure SnO2Standard diagram it is consistent, no miscellaneous peak occurs, and shows that the purity of product is high.Pass through formula：
D=K λ/Bcos θ
Estimate SnO2Particle size be 4nm, wherein, D is crystallite dimension, and λ is X-ray wavelength, and B is the half-peak of diffraction maximum Width, θ are the angle of diffraction, and K is Scherrer constants, often takes 0.9.
FESEM analyses are carried out to product produced by the present invention：As shown in Figure 2.Small of a small amount of nanometer as we can see from the figure The cake mass that grain reunion forms, what is more presented is the cellular pore space structure in agglomerate body, and the diameter of cellular cavity exists 50nm-100nm.And SnO2It is during common hydro-thermal and synthesis in solid state to form nanometer little particle or short grained aggregate more, 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 SnCl first4It is dissolved in its crystallization water, and following chemical reaction occurs：
Sn4++4H2O→Sn(OH)4+4H+
Sn4++4CH3CH2OH→Sn(OH)4+4CH3CH2 +
Sn(OH)4→SnO2+2H2O
Due to SnCl4Generation hydrolyzes and alcoholysis reaction forms unbodied Sn (OH)4, then Sn (OH) at high temperature4Hair Raw dehydrating condensation and crystallization, finally give SnO2.When system acidity is relatively low, be advantageous to SnCl4Hydrolysis, and work as acidity When higher, hydrolysis is restricted, obtained SnO2Negligible amounts, SnO2Exist with nano particle.The carbon added in the method Sour sodium is a kind of strong base-weak acid salt, has certain alkalescence, can effectively adjust the pH of reaction system, control hydrolysis and alcoholysis Journey, form the alveolate texture that the present invention synthesizes.
It is as shown in Figure 3 that FTIR spectrum analysis are carried out to product produced by the present invention：SnO2Middle Sn-O vibration performance peak is 660cm-1.667cm in Fig. 3-1It is O-Sn-O Sn-O stretching vibrations corresponding to neighbouring absworption peak；530cm-1The peak at place is then Sn-O-H Sn-O stretching vibrations, 3421cm-1、1634cm-1The peak occurred at left and right is that the flexible of O-H shakes in physical absorption water It is dynamic, flexural vibrations characteristic peak.
The UV-Vis of product produced by the present invention is analyzed：Test product SnO2UV-Vis DRS spectrum, and make Use formula：
F(R∞)=(1-R∞)2/2R∞=α/S=AC/S
R∞=Rsample/RBaSO4
Absorption spectrum is translated into, from fig. 4, it can be seen that product SnO2There is very high light absorbs energy in ultraviolet region Power.Wherein F (R∞), S, α, R, C and A be respectively Kubelka-Munk functions, scattering coefficient, absorption coefficient, reflectivity, absorbent The concentration and absorbance of kind.SnO2It is direct band-gap semicondictor material, so the band gap magnitude (E of productg) direct band gap half can be used The light absorbs theoretical formula of conductor：
α h ν=B (h ν-Eg)1/2
Wherein α is absorption coefficient, and B is the relevant constant of material person's character, and h ν are the energy of single photon.So in summary Theory, with (F (R ∞) h ν)2For ordinate, (h ν) maps for abscissa, and gained diagram is shown in Fig. 5, and its tangent line is extended into F (R After ∞)=0, estimation product band gap magnitude is 3.2eV.
Cr VI in treatment with ultraviolet light water is carried out to product produced by the present invention to test：With 300ml 50mg/L's K2Cr2O7Solution is simulating pollution thing, respectively with the made SnO of 0.3g2Photochemical catalyst is in 60W days with carrying out light under ultraviolet light source Catalytic degradation, experimental result are as shown in Figure 6.SnO in figure2Added in the system of the photocatalytic degradation simulating pollution thing of product 2ml citric acids, and line 0ml is then not to addition citric acid in photocatalytic process.By Fig. 6 to find out, SnO is added2Photocatalysis Agent is obvious to Cr (VI) degradation effect compared to photochemical catalyst is not added；After UV illumination penetrates 120min, SnO2Photocatalysis Degraded Cr (VI) efficiency is 87.8%.In addition, as seen from Figure 6, divide in photocatalytic process into light-catalyzed reaction system Not plus 0ml and 2ml citric acids are to SnO2Photocatalysis effect has significant difference, and catalytic effect can improve after citric acid is added, Because citric acid plays a part of hole agent for capturing.
Preparation technology of the present invention is simple, easy to operate, using SnO made from 0.3g2In daily 60W days ultraviolet light After 120min, to 300ml 50mg/L Cr (VI) percent reduction up to 87.8%, it is clear that the catalyst effect of honeycomb shape Preferably, Cr VI in water removal can be gone with low energy consumption.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (1)

  1. A kind of 1. cellular SnO2The preparation method of semiconductor light-catalyst, it is characterised in that：Photochemical catalyst reaction raw materials include knot Brilliant butter of tin, natrium carbonicum calcinatum, acetone, absolute ethyl alcohol, comprise the following steps：
    A, first sodium carbonate is placed in vacuum drying chamber and dried, 100 DEG C of drying box temperature setting；
    B, 30mmol natrium carbonicum calcinatums are weighed and are placed on agate mortar, 1mL acetone is added dropwise, grinding 10min is fine and smooth to powder It is even；
    C, after acetone completely volatilization, 10mmol stannic chloride pentahydrates are added in the reactant that step B is obtained, preliminary stirring is mixed 5min is closed, 2mL absolute ethyl alcohols are added dropwise；
    D, after being persistently fully ground 15min, the obtained reactants of step C is transferred in crucible, crucible is placed in Muffle furnace 2h is calcined at 540 DEG C；
    E, room temperature is naturally cooled to after question response terminates, takes out crucible, and adds deionized water immersion thereto；
    F, will be precipitated again in crucible respectively with ionized water and absolute ethyl alcohol washing, suction filtration；
    G, the sample for finally obtaining step F dries 4h in vacuum drying chamber, and drying box temperature is 80 DEG C, and grinding is standby.
CN201610574693.4A 2016-07-21 2016-07-21 A kind of cellular SnO2Semiconductor light-catalyst and preparation method thereof Expired - Fee Related CN106277039B (en)

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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
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