CN103263906A - Nanocrystal tin oxide photocatalyst and preparation method thereof - Google Patents
Nanocrystal tin oxide photocatalyst and preparation method thereof Download PDFInfo
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- CN103263906A CN103263906A CN2013101827411A CN201310182741A CN103263906A CN 103263906 A CN103263906 A CN 103263906A CN 2013101827411 A CN2013101827411 A CN 2013101827411A CN 201310182741 A CN201310182741 A CN 201310182741A CN 103263906 A CN103263906 A CN 103263906A
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Abstract
The invention discloses a nanocrystal tin oxide photocatalyst. The grain size of the tin oxide powder is 10-20 nm, the particle size of the tin oxide is 200-300 nm, and the tin oxide particle surface has prisms. By designing and optimizing the particle size and controllable appearance of the tin oxide surface, the preparation method of the nanocrystal tin oxide photocatalyst greatly enhances the pollutant degradation efficiency, and solves the problems of narrow application range and poor catalytic property in the existing photocatalyst.
Description
Technical field
The invention belongs to nano material and photocatalysis technology field, relate to a kind of semiconductor light-catalyst, be specifically related to a kind of nanocrystalline tin oxide photochemical catalyst, the invention still further relates to the preparation method of above-mentioned nanocrystalline tin oxide photochemical catalyst.
Background technology
Nano tin dioxide is because size is little, specific area is big, thereby surface atom ratio height, the chemical bond that hangs is many, increased the activity of nano material, and the existence of outstanding key makes interfacial polarization in a large number, and high specific area causes multiple scattering, has lower preparation temperature and higher chemical stability simultaneously, and it is widely used at aspects such as pottery, electrically conducting transparent, luminescent material, flat-panel monitor, solar cell, gas sensor, catalyst.The tin oxide superfine powder of therefore prepare the purity height, pattern is even, crystal grain is tiny, nothing is reunited is the focus of Recent study always.
Along with the industrialized fast development in the whole world, problem of environmental pollution is more and more serious.Administer and pollute, the protection environment realizes that sustainable development becomes global common recognition already, pollutes and handles the important research content that therefore becomes researcher.Conductor photocatalysis has advantages such as degradation speed is fast, degraded is complete, energy-conservation, reusable, becomes the noticeable new technology of pollutant process field.At present with the material of photocatalyst common TiO arranged
2, ZnO, SnO
2, WO
3, ZrO
2, Nb
2O
5, Fe
2O
3, SrTiO
3, BaTiO
3, oxides such as CdO, CuS, ZnS sulfides, selenides and SiC such as CdSe, GaP, GaAs.SnO
2Nano material has good photocatalytic activity, but SnO
2Greater band gap (3.8eV) needs ultraviolet excitation, thereby has limited SnO
2Application.For the photochemical catalyst that obtains excited by visible light must comprise crystal morphology control, doping, surface sensitizing, composite etc. to its modification.The nearest small size tin oxide crystal of discovering V-arrangement has demonstrated photocatalysis performance preferably under radiation of visible light.Research to light-catalyzed reaction mechanism, most of people think that the granule size, crystalline structure, surface topography etc. of catalyst are the principal elements that determines photocatalytic activity, so the nano tin dioxide of preparation different-shape structure and the research of its photocatalysis performance had very important meaning.
Summary of the invention
The purpose of this invention is to provide a kind of nanocrystalline tin oxide photochemical catalyst, by the design and optimization to tin oxide surface composition grain graininess size and controllable appearance, improve it greatly to the degradation efficiency of pollutant, solved existing photocatalyst applications narrow range, the problem that catalytic performance is bad.
Another object of the present invention provides the preparation method of above-mentioned nanocrystalline tin oxide photochemical catalyst.
The technical solution adopted in the present invention is, a kind of nanocrystalline tin oxide photochemical catalyst, and the crystallite dimension of tin oxide powder is 10～20nm, and granules of stannic oxide is of a size of 200～300nm, and there is prism on the granules of stannic oxide surface.
Another technical scheme of the present invention is, a kind of preparation method of nanocrystalline tin oxide photochemical catalyst specifically implements according to following steps:
Step 1: take by weighing stannous chloride and under magnetic agitation, be dissolved in deionized water and obtain white solution;
Step 2: in the white solution of step 1 gained, add NaOH, continue stirring until solution and become transparent;
Step 3: be that 30% hydrogen peroxide slowly is added drop-wise in the solution of step 2 gained with mass concentration, stir;
Step 4: in the solution of step 3 gained, add polyvinylpyrrolidone, be stirred to abundant dissolving, obtain polyvinylpyrrolidonesolution solution;
Step 5: the solution of step 4 gained is transferred in the band teflon-lined reactor, microwave hydrothermal 30～90min under 160～200 ℃ of conditions, reaction naturally cools to room temperature after finishing, obtain white precipitate, the collecting precipitation product is also used deionized water, absolute ethyl alcohol centrifuge washing successively, place 60 ℃ of dry 12h of vacuum drying chamber, obtain the nanocrystalline tin oxide photochemical catalyst of the present invention.
Characteristics of the present invention also are,
Quality-the volumetric concentration of white solution is 1:40g/mL～1:8g/mL in the step 1 wherein.
The mass ratio of white solution and NaOH is 1:40～4 in the step 2 wherein.
The volume ratio of hydrogen peroxide and solution is 1:20～2 in the step 3 wherein.
Mixing time is 2～10 minutes in the step 3 wherein.
Quality-the volumetric concentration of polyvinylpyrrolidonesolution solution is 1:50g/mL～1:10g/mL in the step 4 wherein.
The invention has the beneficial effects as follows,
The microwave-hydrothermal method that the present invention uses is that traditional hydro-thermal method and microwave field are united two into one, and has the thermal source of microwave and the advantage of hydro-thermal method itself simultaneously concurrently, has heating and evenly, does not have advantages such as thermograde, acceleration chemical reaction fast.
The temperature of microwave hydrothermal is the degree of crystallinity of the nanocrystalline stannic oxide materials of influence and the key factor of pattern among the present invention, and the degree of crystallinity of the nanocrystalline stannic oxide materials that different temperatures obtains is different with pattern.
Dispersiveness and the pattern of the nanocrystalline stannic oxide materials of time effects of microwave hydrothermal among the present invention, the long reaction time can cause the dispersiveness of nanocrystalline stannic oxide materials and microscopic appearance to be affected.The microwave-hydrothermal method of inducing by surfactant, all price is cheap for the crystallization stannous chloride of choosing (Xi Yuan), NaOH (alkali source), hydrogen peroxide (oxidant), polyvinylpyrrolidone (surfactant), and pattern homogeneous, the size of the nanocrystalline tin oxide catalysis material of preparing is less, particle diameter is evenly distributed, monodispersity is good.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum of the nanocrystalline tin oxide catalysis material of the embodiment of the invention 2 preparations;
Fig. 2 is the electron scanning micrograph of the nanocrystalline tin oxide catalysis material of the embodiment of the invention 3 preparations, and wherein a amplifies 5000 times electron scanning micrograph, and b amplifies 20000 electron scanning micrograph;
Fig. 3 is the electron scanning micrograph of the nanocrystalline tin oxide catalysis material of the embodiment of the invention 4 preparations, and wherein a amplifies 5000 times electron scanning micrograph, and b amplifies 20000 electron scanning micrograph;
Fig. 4 is the photocatalysis rhodamine B degradation curve of the nanocrystalline tin oxide catalysis material of the embodiment of the invention 5 preparations.
The specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The nanocrystalline tin oxide photochemical catalyst of the present invention, it is characterized by: the crystallite dimension of tin oxide powder is 10～20nm, particle size is 200～300nm, and there is little prism on the granules of stannic oxide surface, and the experiment of photocatalytic degradation rhodamine B shows: nanocrystalline tin oxide has higher photocatalytic activity.
The preparation method of the nanocrystalline tin oxide photochemical catalyst of the present invention, specifically implement according to following steps:
Step 1: take by weighing stannous chloride and be dissolved under magnetic agitation and form white solution in the deionized water, the quality-volumetric concentration of the white solution that obtains is 1:40g/mL～1:8g/mL;
Step 2: add NaOH and continue stirring until solution in step 1 gained solution and become transparently, the mass ratio of white solution and NaOH is 1:40～1:4;
Step 3: be that 30% hydrogen peroxide slowly is added drop-wise in the solution of step 2 gained with concentration, stirred 2～10 minutes; The volume ratio of hydrogen peroxide and solution is 1:20～1:2;
Step 4: add polyvinylpyrrolidone in the solution of step 3 gained, stirring makes it fully dissolve the formation homogeneous solution, and the quality-volumetric concentration of the polyvinylpyrrolidonesolution solution that obtains is 1:50g/mL～1:10g/mL;
Step 5: the solution of step 4 gained is transferred in the 100mL band teflon-lined reactor, 160～200 ℃ of microwave hydrothermal 30～90min in microwave dissolver, reaction naturally cools to room temperature after finishing, obtain white precipitate, the collecting precipitation product is also used deionized water and absolute ethyl alcohol centrifuge washing successively, places 60 ℃ of dry 12h of vacuum drying chamber to obtain the nanocrystalline tin oxide photochemical catalyst of the present invention.
Embodiment 1
Taking by weighing stannous chloride is dissolved under magnetic agitation and forms white solution in the deionized water; Quality-the volumetric concentration of the solution that obtains is 1:40g/mL; Adding NaOH and continue stirring until solution in above-mentioned gained solution becomes transparent; The mass ratio of white solution and NaOH is 1:4; Hydrogen peroxide with 30% slowly is added drop-wise in the solution of above-mentioned gained, stirs 10 minutes; The volume ratio of hydrogen peroxide and solution is 1:10; Add polyvinylpyrrolidone in the solution of above-mentioned gained, stirring makes it fully dissolve the formation homogeneous solution; Quality-the volumetric concentration of the polyvinylpyrrolidonesolution solution that obtains is 1:50g/mL; The solution of above-mentioned gained is transferred in the 100mL band teflon-lined reactor, 160 ℃ of microwave hydrothermal 90min in microwave dissolver, reaction naturally cools to room temperature after finishing, obtain white precipitate, the collecting precipitation product is also used deionized water and absolute ethyl alcohol centrifuge washing, places 60 ℃ of dry 12h of vacuum drying chamber to obtain nanocrystalline tin oxide powder.
Embodiment 2
Taking by weighing stannous chloride is dissolved under magnetic agitation and forms white solution in the deionized water; Quality-the volumetric concentration of the solution that obtains is 1:20g/mL; Adding NaOH and continue stirring until solution in above-mentioned gained solution becomes transparent; The mass ratio of white solution and NaOH is 1:8; Hydrogen peroxide with 30% slowly is added drop-wise in the solution of above-mentioned gained, stirs 7 minutes; The volume ratio of hydrogen peroxide and solution is 1:20; Add polyvinylpyrrolidone in the solution of above-mentioned gained, stirring makes it fully dissolve the formation homogeneous solution; Quality-the volumetric concentration of the polyvinylpyrrolidonesolution solution that obtains is 1:10g/mL; The solution of above-mentioned gained is transferred in the 100mL band teflon-lined reactor, 180 ℃ of microwave hydrothermal 30min in microwave dissolver, reaction naturally cools to room temperature after finishing, obtain white precipitate, the collecting precipitation product is also used deionized water and absolute ethyl alcohol centrifuge washing, places 60 ℃ of dry 12h of vacuum drying chamber to obtain nanocrystalline tin oxide powder.Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of prepared nanocrystalline tin oxide, and as can be seen from the figure, product is cubic rutile structure, and degree of crystallinity is higher, and purity is higher.
Embodiment 3
Taking by weighing stannous chloride is dissolved under magnetic agitation and forms white solution in the deionized water; Quality-the volumetric concentration of the solution that obtains is 1:30g/mL; Adding NaOH and continue stirring until solution in above-mentioned gained solution becomes transparent; The mass ratio of white solution and NaOH is 1:40; Hydrogen peroxide with 30% slowly is added drop-wise in the solution of above-mentioned gained, stirs 5 minutes; The volume ratio of hydrogen peroxide and solution is 1:8; Add polyvinylpyrrolidone in the solution of above-mentioned gained, stirring makes it fully dissolve the formation homogeneous solution; Quality-the volumetric concentration of the polyvinylpyrrolidonesolution solution that obtains is 1:25g/mL; The solution of above-mentioned gained is transferred in the 100mL band teflon-lined reactor, 200 ℃ of microwave hydrothermal 60min in microwave dissolver, reaction naturally cools to room temperature after finishing, obtain white precipitate, the collecting precipitation product is also used deionized water and absolute ethyl alcohol centrifuge washing, places 60 ℃ of dry 12h of vacuum drying chamber to obtain nanocrystalline tin oxide powder.Fig. 2 is the stereoscan photograph of prepared nanocrystalline tin oxide, and as can be seen from the figure, product is spherical, and it is the little prism in four directions that there is the cross section on the spherical particle surface.
Embodiment 4
Taking by weighing stannous chloride is dissolved under magnetic agitation and forms white solution in the deionized water; Quality-the volumetric concentration of the solution that obtains is 1:8g/mL; Adding NaOH and continue stirring until solution in above-mentioned gained solution becomes transparent; The mass ratio of white solution and NaOH is 1:10; Hydrogen peroxide with 30% slowly is added drop-wise in the solution of above-mentioned gained, stirs 8 minutes; The volume ratio of hydrogen peroxide and solution is 1:2; Add polyvinylpyrrolidone in the solution of above-mentioned gained, stirring makes it fully dissolve the formation homogeneous solution; Quality-the volumetric concentration of the polyvinylpyrrolidonesolution solution that obtains is 2:25g/mL; The solution of above-mentioned gained is transferred in the 100mL band teflon-lined reactor, 185 ℃ of microwave hydrothermal 75min in microwave dissolver, reaction naturally cools to room temperature after finishing, obtain white precipitate, the collecting precipitation product is also used deionized water and absolute ethyl alcohol centrifuge washing, places 60 ℃ of dry 12h of vacuum drying chamber to obtain nanocrystalline tin oxide powder.Fig. 3 is the stereoscan photograph of prepared nanocrystalline tin oxide, as can be seen from the figure, the pattern homogeneous of tin oxide powder, the less 18nm that is about of crystallite dimension, particle size is about 200～300nm, and monodispersity is good.
Embodiment 5
Taking by weighing stannous chloride is dissolved under magnetic agitation and forms white solution in the deionized water; Quality-the volumetric concentration of the solution that obtains is 1:12g/mL; Adding NaOH and continue stirring until solution in above-mentioned gained solution becomes transparent; The mass ratio of white solution and NaOH is 1:20; Hydrogen peroxide with 30% slowly is added drop-wise in the solution of above-mentioned gained, stirs 2 minutes; The volume ratio of hydrogen peroxide and solution is 1:4; Add polyvinylpyrrolidone in the solution of above-mentioned gained, stirring makes it fully dissolve the formation homogeneous solution; Quality-the volumetric concentration of the polyvinylpyrrolidonesolution solution that obtains is 3:50g/mL; The solution of above-mentioned gained is transferred in the 100mL band teflon-lined reactor, 170 ℃ of microwave hydrothermal 80min in microwave dissolver, reaction naturally cools to room temperature after finishing, obtain white precipitate, the collecting precipitation product is also used deionized water and absolute ethyl alcohol centrifuge washing, places 60 ℃ of dry 12h of vacuum drying chamber to obtain nanocrystalline tin oxide powder.Fig. 4 is the photocatalysis rhodamine B degradation curve of prepared nanocrystalline tin oxide powder, prepares nanocrystalline tin oxide catalysis material as can be seen from degradation curve the rhodamine B the water body is had higher degradation efficiency.
The parameter area of key of the present invention is the mass ratio of quality-volumetric concentration, white solution and NaOH of stannous chloride solution and the quality-volumetric concentration of polyvinylpyrrolidonesolution solution; Can control the hydrolysis situation of stannous chloride effectively by choose reasonable, regulation and control parameter area, thereby prepare the nano tin dioxide powder that possesses controllable appearance.Being greater than or less than this parameter area can cause the preparation of the nano tin dioxide of controllable appearance to go wrong because of disappearance or the unreasonable consumption improper and template agent polyvinylpyrrolidone saturated, system pH of source material.
Claims (7)
1. a nanocrystalline tin oxide photochemical catalyst is characterized in that the crystallite dimension of tin oxide powder is 10～20nm, and granules of stannic oxide is of a size of 200～300nm, and there is prism on the granules of stannic oxide surface.
2. the preparation method of a nanocrystalline tin oxide photochemical catalyst is characterized in that, the nanocrystalline tin oxide photochemical catalyst for preparing, and the crystallite dimension of tin oxide powder is 10～20nm, and granules of stannic oxide is of a size of 200～300nm, and there is prism on the granules of stannic oxide surface;
Specifically implement according to following steps:
Step 1: take by weighing stannous chloride and under magnetic agitation, be dissolved in deionized water and obtain white solution;
Step 2: in the white solution of step 1 gained, add NaOH, continue stirring until solution and become transparent;
Step 3: be that 30% hydrogen peroxide slowly is added drop-wise in the solution of step 2 gained with mass concentration, stir;
Step 4: in the solution of step 3 gained, add polyvinylpyrrolidone, be stirred to abundant dissolving, obtain polyvinylpyrrolidonesolution solution;
Step 5: the solution of step 4 gained is transferred in the band teflon-lined reactor, microwave hydrothermal 30～90min under 160～200 ℃ of conditions, reaction naturally cools to room temperature after finishing, obtain white precipitate, the collecting precipitation product is also used deionized water, absolute ethyl alcohol centrifuge washing successively, place 60 ℃ of dry 12h of vacuum drying chamber, obtain the nanocrystalline tin oxide photochemical catalyst of the present invention.
3. the preparation method of nanocrystalline tin oxide photochemical catalyst according to claim 2 is characterized in that, the quality-volumetric concentration of white solution is 1:40g/mL～1:8g/mL in the described step 1.
4. the preparation method of nanocrystalline tin oxide photochemical catalyst according to claim 2 is characterized in that, the mass ratio of white solution and NaOH is 1:40～4 in the described step 2.
5. the preparation method of nanocrystalline tin oxide photochemical catalyst according to claim 2 is characterized in that, the volume ratio of hydrogen peroxide and solution is 1:20～2 in the described step 3.
6. the preparation method of nanocrystalline tin oxide photochemical catalyst according to claim 2 is characterized in that, mixing time is 2～10 minutes in the described step 3.
7. the preparation method of nanocrystalline tin oxide photochemical catalyst according to claim 2 is characterized in that, the quality-volumetric concentration of polyvinylpyrrolidonesolution solution is 1:50g/mL～1:10g/mL in the described step 4.
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Cited By (8)
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|---|---|---|---|---|
| CN105129842A (en) * | 2015-09-12 | 2015-12-09 | 景德镇陶瓷学院 | Preparation method of high-activity SnO2 nanocrystal responding to visible light |
| CN106000384A (en) * | 2016-05-13 | 2016-10-12 | 淮北师范大学 | Preparation method of tin-based oxide with controllable components and photocatalytic application of tin-based oxide |
| CN106268750A (en) * | 2016-10-14 | 2017-01-04 | 山东大学 | A kind of visible-light response type Photoreduction Activity of Isolated SnO2 Xthe preparation method of nano-particle |
| CN107045942A (en) * | 2017-01-21 | 2017-08-15 | 深圳孔雀科技开发有限公司 | A kind of high catalytic activity probe material and preparation method and application |
| CN107486194A (en) * | 2017-07-24 | 2017-12-19 | 安徽华亿农牧科技发展有限公司 | A kind of preparation method of the load cerium tin oxide composite microsphere photocatalyst of aquiculture waste water processing |
| CN108855153A (en) * | 2018-05-28 | 2018-11-23 | 河南师范大学 | A kind of preparation method of faint yellow alkali formula stannous chloride visible light responsible photocatalytic material |
| CN110302775A (en) * | 2019-06-28 | 2019-10-08 | 陕西科技大学 | A kind of preparation method of mangano-manganic oxide/tin dioxide nucleic shell structured catalysis material |
| CN111450817A (en) * | 2020-05-12 | 2020-07-28 | 重庆工商大学 | Titanium-doped tin oxide photocatalyst and preparation method thereof |
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Cited By (12)
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| CN105129842A (en) * | 2015-09-12 | 2015-12-09 | 景德镇陶瓷学院 | Preparation method of high-activity SnO2 nanocrystal responding to visible light |
| CN106000384A (en) * | 2016-05-13 | 2016-10-12 | 淮北师范大学 | Preparation method of tin-based oxide with controllable components and photocatalytic application of tin-based oxide |
| CN106000384B (en) * | 2016-05-13 | 2018-04-10 | 淮北师范大学 | A kind of preparation method and its photocatalytic applications for forming controllable tin-based oxide |
| CN106268750A (en) * | 2016-10-14 | 2017-01-04 | 山东大学 | A kind of visible-light response type Photoreduction Activity of Isolated SnO2 Xthe preparation method of nano-particle |
| CN106268750B (en) * | 2016-10-14 | 2019-05-28 | 山东大学 | A kind of visible-light response type Photoreduction Activity of Isolated SnO2-XThe preparation method of nano particle |
| CN107045942A (en) * | 2017-01-21 | 2017-08-15 | 深圳孔雀科技开发有限公司 | A kind of high catalytic activity probe material and preparation method and application |
| CN107486194A (en) * | 2017-07-24 | 2017-12-19 | 安徽华亿农牧科技发展有限公司 | A kind of preparation method of the load cerium tin oxide composite microsphere photocatalyst of aquiculture waste water processing |
| CN108855153A (en) * | 2018-05-28 | 2018-11-23 | 河南师范大学 | A kind of preparation method of faint yellow alkali formula stannous chloride visible light responsible photocatalytic material |
| CN108855153B (en) * | 2018-05-28 | 2021-03-16 | 河南师范大学 | Preparation method of faint yellow basic stannous chloride visible light response photocatalytic material |
| CN110302775A (en) * | 2019-06-28 | 2019-10-08 | 陕西科技大学 | A kind of preparation method of mangano-manganic oxide/tin dioxide nucleic shell structured catalysis material |
| CN110302775B (en) * | 2019-06-28 | 2021-11-30 | 陕西科技大学 | Preparation method of manganous-manganic oxide/stannic oxide core-shell structure catalytic material |
| CN111450817A (en) * | 2020-05-12 | 2020-07-28 | 重庆工商大学 | Titanium-doped tin oxide photocatalyst and preparation method thereof |
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Application publication date: 20130828 |