CN106512978A - Method for preparing visible-light response photocatalyst by utilizing nano Zn2SnO4 - Google Patents
Method for preparing visible-light response photocatalyst by utilizing nano Zn2SnO4 Download PDFInfo
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- CN106512978A CN106512978A CN201611070604.9A CN201611070604A CN106512978A CN 106512978 A CN106512978 A CN 106512978A CN 201611070604 A CN201611070604 A CN 201611070604A CN 106512978 A CN106512978 A CN 106512978A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910003107 Zn2SnO4 Inorganic materials 0.000 title abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 34
- 239000011858 nanopowder Substances 0.000 claims abstract description 23
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000007787 solid Substances 0.000 claims description 36
- 239000000725 suspension Substances 0.000 claims description 32
- 239000011259 mixed solution Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- 238000005406 washing Methods 0.000 claims description 24
- 239000013049 sediment Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000011701 zinc Substances 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 16
- 229960000583 acetic acid Drugs 0.000 claims description 14
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 14
- 239000012362 glacial acetic acid Substances 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 235000014121 butter Nutrition 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 6
- 235000005074 zinc chloride Nutrition 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 15
- 239000007788 liquid Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000005215 recombination Methods 0.000 abstract description 3
- 230000006798 recombination Effects 0.000 abstract description 3
- 238000000498 ball milling Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000013508 migration Methods 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 230000031700 light absorption Effects 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 6
- 229910007717 ZnSnO Inorganic materials 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 229910007694 ZnSnO3 Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 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 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- -1 is nanostructured Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229940071182 stannate Drugs 0.000 description 1
- 125000005402 stannate group Chemical group 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for preparing a visible-light response photocatalyst by utilizing nano Zn2SnO4. The method comprises a step of preparing a solvent thermal product, a step of preparing Zn2SnO4 nano powder, a step of preparing a turbid liquid, a step of preparing a hydrothermal reaction product and a step of preparing the visible-light response photocatalyst. According to the method disclosed by the invention, a synthesis process is simple and convenient, impurities introduced by follow-up processes such as high-temperature calcining and ball-milling and structure defects are avoided, operations are easy, and purity of products synthesized by reaction is high. The visible-light response photocatalyst synthesized by the method is a nano structure, is small in crystalline grain, and has a mesoporous structure and a relatively great surface area, so that light absorption capacity of the visible-light response photocatalyst is strengthened; and meanwhile, a migration distance of light-generated electrons is shortened, and recombination probability of light-generated electrons and electron-hole pairs is reduced.
Description
Technical field
The present invention relates to one kind utilizes nanometer Zn2SnO4The method for preparing visible light responsive photocatalyst.
Background technology
Traditional titanium dioxide is a kind of important n-type semiconductor, can be applicable to solaode, photocatalytic degradation organic
Pollutant and photolysis water hydrogen field, but TiO2Band-gap energy is larger, only shows preferably photocatalysis under ultraviolet light conditions
Activity, and it is vulnerable to photetching effect,
Accordingly, it would be desirable to further develop new visible light responsive photocatalyst.Zinc（Zn2SnO4）As a kind of new
Broad-band gap photocatalyst, its energy gap are about 3.6eV, and its electron mobility and quantum efficiency are high, light induced electron and hole
Recombination probability is low, effectively can degrade under ultraviolet light conditions NO and HCHO and organic pollution, but at present to Zn2SnO4's
Photocatalysis research is limited to UV light region mostly, and under its visible light conditions, photocatalytic activity is not high, it is therefore necessary to nanometer
Zn2SnO4It is modified to strengthen its visible light catalytic performance.In this research, with Hydrothermal Synthesiss Zn2SnO4Nano powder is raw material,
It is modified by hydro-thermal reaction, so as to obtain ZnSnO3Superfine nano powder, the product have excellent under visible light conditions
Photocatalysis performance, the preparation method of this novel visible catalyst is there is not yet relevant report.
The content of the invention
It is an object of the invention to provide one kind utilizes nanometer Zn2SnO4The method for preparing visible light responsive photocatalyst, the product
Thing crystal grain is tiny, with meso-hole structure, and has excellent visible light catalytic performance.
The technical scheme adopted for achieving the above object by the present invention is for utilizing nanometer Zn2SnO4Prepare visible light-responded light
The method of catalyst, comprises the following steps：Step one, a certain amount of sodium hydroxide powder body is weighed, be completely dissolved to solvent
In, be sufficiently stirred for, dissolve after be obtained concentration for 3.75mol/L NaOH solution, be labeled as solution A, it is standby；
Step 2, weigh a certain amount of butter of tin and mixed solution is formed during zinc chloride is dissolved in solvent, be sufficiently stirred for, dissolve
Afterwards, Sn in obtained mixed solution4+With Zn2+Concentration is respectively 0.25mol/L and 0.5 mol/L, is labeled as mixed solution B, standby
With；
Step 3, by volume parts ratio, take 2 respectively：Mixed solution B prepared by solution A and step 2 prepared by 1 the step of one,
Solution A and mixed solution B are mixed, and suspension is obtained after fully reacting, the suspension for obtaining is transferred in reactor,
Reactor temperature is controlled for 200-220 DEG C, after insulation 20-30h, room temperature is down to, solvent hot is obtained, it is standby；
Step 4, solvent hot obtained in step 3 is transferred in high-speed centrifuge it is centrifuged, takes solid
After precipitate, solid sediment is carried out washing, is dried, Zn is obtained2SnO4Nano powder, it is standby；
Step 5, according to the Zn of every 1-4g2SnO4Nano powder adds the ratio of the aqueous solution of 160mL glacial acetic acid, weighs step 4
Obtained Zn2SnO4Nano powder is added into the aqueous solution of glacial acetic acid, after being sufficiently stirred for, and obtains suspension, standby；
Step 6, the suspension that step 5 is obtained is transferred in reactor, reactor temperature is controlled for 145-165 DEG C, plus
Reactor is cooled to room temperature, obtains hydro-thermal reaction product by heat insulation 12-18h afterwards；
Step 7, hydro-thermal reaction product obtained in step 6 is transferred in high-speed centrifuge it is centrifuged, takes solid
After body precipitate, the solid sediment to obtaining is washed, then the solid product obtained after washing is put in drying baker,
10-12h is dried at 80-90 DEG C, obtains final product.
In the present invention, the solvent used in step one and step 2 is deionized water.
In the present invention, in step 3 and step 6, after reactor is transferred to, in reactor, suspension fills out suspension
Degree of filling is 80%.
In the present invention, in step 4 and step 7 to the method for the washing of solid sediment it is：Deionization is adopted successively
Water and dehydrated alcohol carry out alternately washing 3-5 time to the solid sediment for obtaining.
In the present invention, the Drying Technology Parameter in step 4 is at 80-90 DEG C to be dried 10-12h.
In the present invention, the volumetric concentration of the glacial acetic acid in step 5 is 5-30%.
Beneficial effect：（1）, the method synthesis technique it is easy, avoid the introducing of the subsequent techniques such as high-temperature calcination and ball milling
Impurity and fault of construction, product purity easy to operate, being synthesized are high.（2）, the method synthesis visible light responsive photocatalytic
Agent, is nanostructured, and crystal grain is little, and with meso-hole structure and larger surface area, the structure makes photoresponse type photocatalyst
Light absorpting ability strengthens, while shortening the migration distance of light induced electron, reduces light induced electron with hole to recombination probability.This
In research, photocatalytic degradation experiment is carried out to rhodamine B solution under daylight light irradiation, had under visible light conditions excellent
Photocatalysis performance, the modified product by the use of present invention synthesis is used as photocatalyst degradable rhodamine B（RhB）More than 95%.
Description of the drawings
XRD figure of the Fig. 1 for visible-light-responsive photocatalyst obtained in embodiment 1；
Fig. 2 is the TEM figures of visible-light-responsive photocatalyst obtained in embodiment 1；
Fig. 3 is the photocatalysis result of visible-light-responsive photocatalyst obtained in embodiment 1；
Fig. 4 is visible-light-responsive photocatalyst and Zn obtained in embodiment 12SnO4Light of the nano powder under the conditions of same test
Catalytic result comparison diagram.
Specific embodiment
With reference to specific embodiment, the invention will be further described, so that those skilled in the art can be more preferable
Understand the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
Using nanometer Zn2SnO4The method for preparing visible light responsive photocatalyst, comprises the following steps：Step one, weigh it is certain
The sodium hydroxide powder body of amount, is completely dissolved into solvent, be sufficiently stirred for, dissolve after concentration is obtained for 3.75mol/L
NaOH solution, is labeled as solution A, standby；Solvent used in which is deionized water；
Step 2, weigh a certain amount of butter of tin and mixed solution is formed during zinc chloride is dissolved in solvent, after being sufficiently stirred for, dissolving
Sn in obtained mixed solution4+With Zn2+Concentration is respectively 0.25mol/L and 0.5 mol/L, is labeled as mixed solution B, standby；
Solvent used in which is deionized water；
Step 3, by volume parts, take solution A prepared by 2 parts of steps one and mixed solution B prepared by 1 part of step 2 respectively,
Under stirring condition, the solution A for measuring is added into mixed solution B with the drop rate of 2mL/min, hanged after fully reacting
Turbid liquid, the suspension for obtaining is transferred in reactor, and in reactor, the compactedness of suspension is 80%, controls reactor interior temperature
Spend for 210 DEG C, after insulation 22h, be down to room temperature, obtain solvent hot, it is standby；
Step 4, solvent hot obtained in step 3 is transferred in high-speed centrifuge it is centrifuged, takes solid
After precipitate, solid sediment is washed, the solid sediment for obtaining is entered using deionized water and dehydrated alcohol successively
Row alternately washing 3-5 time, i.e., first use deionized water wash once every time, reuse absolute ethanol washing once, deionized water
Respectively wash 3-5 time with dehydrated alcohol；Then 10h is dried at 85 DEG C, obtain Zn2SnO4Nano powder, it is standby；
Step 5, Zn obtained in four the step of weigh 0.5-2g2SnO4Nano powder is added into the aqueous solution of 80mL glacial acetic acid, Jing
Cross after being sufficiently stirred for, obtain suspension, it is standby；Wherein, the volumetric concentration of glacial acetic acid is 5-30%；
Step 6, the suspension that step 5 is obtained is transferred in reactor, in reactor, the compactedness of suspension is 80%, control
Reactor temperature processed is 145 DEG C, and reactor is cooled to room temperature by heating and thermal insulation 15h afterwards, obtains hydro-thermal reaction product；
Step 7, hydro-thermal reaction product obtained in step 6 is transferred in high-speed centrifuge it is centrifuged, takes solid
After body precipitate, the solid sediment to obtaining is washed, successively using deionized water and dehydrated alcohol to the solid that obtains
Precipitate carries out alternately washing 3-5 time, then the solid product obtained after washing is put in drying baker, at 85 DEG C is dried 10h,
Obtain final product.
Product prepared by embodiment 1 carries out XRD and TEM and tests, test result as depicted in figs. 1 and 2, by XRD spectrum
Understand, the diffraction maximum of 1 synthetic product of embodiment is wider, and occur without miscellaneous peak, obtained visible light responsive photocatalyst is nanometer
ZnSnO3, synthesize ZnSnO3Nanocrystalline purity it is high；Synthetic product can be seen that for Nanoparticulate by TEM results, pattern is equal
Even, its particle diameter is little, and mean diameter is 5nm or so.
Photocatalysis performance test is carried out to the product that the present embodiment is obtained：The existing Zn of 0.1g is taken respectively2SnO4Nano powder is made
The product synthesized for matched group and the present embodiment is both included as photocatalyst, with rhodamine B as test group（RhB）Solution
For target degradation product, the concentration of RhB solution is 1 × 10-5Mol/L, volume are 40mL, from 60W fluorescent tube as light source, sample
Distance of the product away from fluorescent tube is 10cm, carries out photocatalytic degradation experiment.Through the illumination of 60min, as a result as shown in Figure 3, Figure 4.By
Fig. 3 can be seen that the intensity level of the characteristic peak of RhB and reduce with the prolongation of light application time, show RhB concentration values with during illumination
Between prolongation and reduce.With existing Zn2SnO4As photocatalyst, the concentration degradable 56% of RhB；With changing that the present embodiment synthesizes
Property product can drop 95% as the concentration of photocatalyst solution RhB；Contrast Zn2SnO4With the present embodiment synthetic product as photocatalyst
Degradation effect, as a result show, using Zn2SnO4Nano powder prepares the ZnSnO of visible-light response type3Catalyst, the production die
It is tiny, with meso-hole structure, and there is excellent visible light catalytic performance.
Embodiment 2
Using nanometer Zn2SnO4The method for preparing visible light responsive photocatalyst, comprises the following steps：Step one, weigh it is certain
The sodium hydroxide powder body of amount, is completely dissolved into solvent, be sufficiently stirred for, dissolve after concentration is obtained for 3.75mol/L
NaOH solution, is labeled as solution A, standby；Solvent used in which is deionized water；
Step 2, weigh a certain amount of butter of tin and mixed solution is formed during zinc chloride is dissolved in solvent, after being sufficiently stirred for, dissolving
Sn in obtained mixed solution4+With Zn2+Concentration is respectively 0.25mol/L and 0.5 mol/L, is labeled as mixed solution B, standby；
Solvent used in which is deionized water；
Step 3, by volume parts, take solution A prepared by 2 parts of steps one and mixed solution B prepared by 1 part of step 2 respectively,
Under stirring condition, the solution A for measuring is added into mixed solution B with the drop rate of 2mL/min, hanged after fully reacting
Turbid liquid, the suspension for obtaining is transferred in reactor, and in reactor, the compactedness of suspension is 80%, controls reactor interior temperature
Spend for 220 DEG C, after insulation 25h, be down to room temperature, obtain hydrothermal product, it is standby；
Step 4, solvent hot obtained in step 3 is transferred in high-speed centrifuge it is centrifuged, takes solid
After precipitate, solid sediment is washed, the solid sediment for obtaining is entered using deionized water and dehydrated alcohol successively
Row alternately washing 3-4 time, i.e., first use deionized water wash once every time, reuse absolute ethanol washing once, deionized water
Respectively wash 3-4 time with dehydrated alcohol；Then 10h is dried at 90 DEG C, obtain Zn2SnO4Nano powder, it is standby；
Step 5, Zn obtained in four the step of weigh 1-4g2SnO4Nano powder is added into the aqueous solution of 160mL glacial acetic acid, Jing
Cross after being sufficiently stirred for, obtain suspension, it is standby；Wherein, the volumetric concentration of glacial acetic acid is 5-30%；
Step 6, the suspension that step 5 is obtained is transferred in reactor, in reactor, the compactedness of suspension is 80%, control
Reactor temperature processed is 150 DEG C, and reactor is cooled to room temperature by heating and thermal insulation 15h afterwards, obtains hydro-thermal reaction product；
Step 7, hydro-thermal reaction product obtained in step 6 is transferred in high-speed centrifuge it is centrifuged, takes solid
After body precipitate, the solid sediment to obtaining is washed, successively using deionized water and dehydrated alcohol to the solid that obtains
Precipitate carries out alternately washing 3-5 time, then the solid product obtained after washing is put in drying baker, at 90 DEG C is dried 10h,
Obtain the visible-light response type ZnSnO of nanostructured3Photocatalyst, the mean diameter of its nano powder is 5nm.
Embodiment 3
Using nanometer Zn2SnO4The method for preparing visible light responsive photocatalyst, comprises the following steps：Step one, weigh it is certain
The sodium hydroxide powder body of amount, is completely dissolved into solvent, be sufficiently stirred for, dissolve after concentration is obtained for 3.75mol/L
NaOH solution, is labeled as solution A, standby；Solvent used in which is deionized water；
Step 2, weigh a certain amount of butter of tin and mixed solution is formed during zinc chloride is dissolved in solvent, after being sufficiently stirred for, dissolving
Sn in obtained mixed solution4+With Zn2+Concentration is respectively 0.25mol/L and 0.5 mol/L, is labeled as mixed solution B, standby；
Solvent used in which is deionized water；
Step 3, by volume parts, take solution A prepared by 2 parts of steps one and mixed solution B prepared by 1 part of step 2 respectively,
Under stirring condition, the solution A for measuring is added into mixed solution B with the drop rate of 2mL/min, hanged after fully reacting
Turbid liquid, the suspension for obtaining is transferred in reactor, and in reactor, the compactedness of suspension is 80%, controls reactor interior temperature
Spend for 200 DEG C, after insulation 28h, be down to room temperature, obtain solvent hot, it is standby；
Step 4, solvent hot obtained in step 3 is transferred in high-speed centrifuge it is centrifuged, takes solid
After precipitate, solid sediment is washed, the solid sediment for obtaining is entered using deionized water and dehydrated alcohol successively
Row alternately washing 3-4 time, i.e., first use deionized water wash once every time, using absolute ethanol washing once, deionized water
Respectively wash 3-4 time with dehydrated alcohol；Then 12h is dried at 80 DEG C, obtain Zn2SnO4Nano powder, it is standby；
Step 5, Zn obtained in four the step of weigh 1.5-2g2SnO4Nano powder is added into the aqueous solution of 80mL glacial acetic acid, Jing
Cross after being sufficiently stirred for, obtain suspension, it is standby；Wherein, the volumetric concentration of glacial acetic acid is 5-30%；
Step 6, the suspension that step 5 is obtained is transferred in reactor, in reactor, the compactedness of suspension is 80%, control
Reactor temperature processed is 155 DEG C, and reactor is cooled to room temperature by heating and thermal insulation 12h afterwards, obtains hydro-thermal reaction product；
Step 7, hydro-thermal reaction product obtained in step 6 is transferred in high-speed centrifuge it is centrifuged, takes solid
After body precipitate, the solid sediment to obtaining is washed, successively using deionized water and dehydrated alcohol to the solid that obtains
Precipitate carries out alternately washing 3-5 time, then the solid product obtained after washing is put in drying baker, at 80 DEG C is dried 12h,
Obtain the visible-light response type ZnSnO of nanostructured3Photocatalyst, the mean diameter of its nano powder is 5nm.
Embodiment 4
Using nanometer Zn2SnO4The method for preparing visible light responsive photocatalyst, comprises the following steps：Step one, weigh it is certain
The sodium hydroxide powder body of amount, is completely dissolved into solvent, be sufficiently stirred for, dissolve after concentration is obtained for 3.75mol/L
NaOH solution, is labeled as solution A, standby；Solvent used in which is deionized water；
Step 2, weigh a certain amount of butter of tin and mixed solution is formed during zinc chloride is dissolved in solvent, after being sufficiently stirred for, dissolving
Sn in obtained mixed solution4+With Zn2+Concentration is respectively 0.25mol/L and 0.5mol/L, is labeled as mixed solution B, standby；
Solvent used in which is deionized water；
Step 3, by volume parts, take solution A prepared by 2 parts of steps one and mixed solution B prepared by 1 part of step 2 respectively,
Under stirring condition, the solution A for measuring is added into mixed solution B with the drop rate of 2mL/min, hanged after fully reacting
Turbid liquid, the suspension for obtaining is transferred in reactor, and in reactor, the compactedness of suspension is 80%, controls reactor interior temperature
Spend for 200 DEG C, after insulation 30h, be down to room temperature, obtain solvent hot, it is standby；
Step 4, solvent hot obtained in step 3 is transferred in high-speed centrifuge it is centrifuged, takes solid
After precipitate, solid sediment is washed, the solid sediment for obtaining is entered using deionized water and dehydrated alcohol successively
Row alternately washing 3-4 time, i.e., first use deionized water wash once every time, using absolute ethanol washing once, deionized water
Respectively wash 3-4 time with dehydrated alcohol；Then 11h is dried at 82 DEG C, obtain zine stannate nano powder, it is standby；
Step 5, Zn obtained in four the step of weigh 3-4g2SnO4Nano powder is added into the aqueous solution of 160mL glacial acetic acid, Jing
Cross after being sufficiently stirred for, obtain suspension, it is standby；Wherein, the volumetric concentration of glacial acetic acid is 5-30%；
Step 6, the suspension that step 5 is obtained is transferred in reactor, in reactor, the compactedness of suspension is 80%, control
Reactor temperature processed is 165 DEG C, and reactor is cooled to room temperature by heating and thermal insulation 18h afterwards, obtains hydro-thermal reaction product；
Step 7, hydro-thermal reaction product obtained in step 6 is transferred in high-speed centrifuge it is centrifuged, takes solid
After body precipitate, the solid sediment to obtaining is washed, successively using deionized water and dehydrated alcohol to the solid that obtains
Precipitate carries out alternately washing 3-5 time, then the solid product obtained after washing is put in drying baker, at 83 DEG C is dried 11h,
Obtain the visible-light response type ZnSnO of nanostructured3Photocatalyst, the mean diameter of its nano powder is 5nm.
Claims (6)
1. nanometer Zn is utilized2SnO4The method for preparing visible light responsive photocatalyst, it is characterised in that：Comprise the following steps：
Step one, weigh a certain amount of sodium hydroxide powder body, be completely dissolved into solvent, be sufficiently stirred for, dissolve after be obtained
Concentration is the NaOH solution of 3.75mol/L, is labeled as solution A, standby；
Step 2, weigh a certain amount of butter of tin and mixed solution is formed during zinc chloride is dissolved in solvent, be sufficiently stirred for, dissolve
Afterwards, Sn in obtained mixed solution4+With Zn2+Concentration is respectively 0.25mol/L and 0.5 mol/L, is labeled as mixed solution B, standby
With；
Step 3, by volume parts ratio, take 2 respectively：Mixed solution B prepared by solution A and step 2 prepared by 1 the step of one,
Solution A and mixed solution B are mixed, and suspension is obtained after fully reacting, the suspension for obtaining is transferred in reactor,
Reactor temperature is controlled for 200-220 DEG C, after insulation 20-30h, room temperature is down to, solvent hot is obtained, it is standby；
Step 4, solvent hot obtained in step 3 is transferred in high-speed centrifuge it is centrifuged, takes solid
After precipitate, solid sediment is carried out washing, is dried, Zn is obtained2SnO4Nano powder, it is standby；
Step 5, according to the Zn of every 1-4g2SnO4Nano powder adds the ratio of the aqueous solution of 160mL glacial acetic acid, weighs step 4 system
The Zn for obtaining2SnO4Nano powder is added into the aqueous solution of glacial acetic acid, after being sufficiently stirred for, and obtains suspension, standby；
Step 6, the suspension that step 5 is obtained is transferred in reactor, reactor temperature is controlled for 145-165 DEG C, plus
Reactor is cooled to room temperature, obtains hydro-thermal reaction product by heat insulation 12-18h afterwards；
Step 7, hydro-thermal reaction product obtained in step 6 is transferred in high-speed centrifuge it is centrifuged, takes solid
After body precipitate, the solid sediment to obtaining is washed, then the solid product obtained after washing is put in drying baker,
10-12h is dried at 80-90 DEG C, obtains final product.
2. utilization nanometer Zn according to claim 12SnO4The method for preparing visible light responsive photocatalyst, its feature exist
In：Solvent used in step one and step 2 is deionized water.
3. utilization nanometer Zn according to claim 12SnO4The method for preparing visible light responsive photocatalyst, its feature exist
In：In step 3 and step 6, after reactor is transferred to, in reactor, the compactedness of suspension is 80% to suspension.
4. utilization nanometer Zn according to claim 12SnO4The method for preparing visible light responsive photocatalyst, its feature exist
In：In step 4 and step 7 to the method for the washing of solid sediment it is：Deionized water and dehydrated alcohol pair is adopted successively
The solid sediment for obtaining carries out alternately washing 3-5 time.
5. utilization nanometer Zn according to claim 12SnO4The method for preparing visible light responsive photocatalyst, its feature exist
In：Drying Technology Parameter in step 4 is at 80-90 DEG C to be dried 10-12h.
6. utilization nanometer Zn according to claim 12SnO4The method for preparing visible light responsive photocatalyst, its feature exist
In：The volumetric concentration of the glacial acetic acid in step 5 is 5-30%.
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