CN102218333A - Method for preparing ZnIn2S4 visible-light activated photocatalyst at low temperature - Google Patents
Method for preparing ZnIn2S4 visible-light activated photocatalyst at low temperature Download PDFInfo
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- CN102218333A CN102218333A CN2011100983396A CN201110098339A CN102218333A CN 102218333 A CN102218333 A CN 102218333A CN 2011100983396 A CN2011100983396 A CN 2011100983396A CN 201110098339 A CN201110098339 A CN 201110098339A CN 102218333 A CN102218333 A CN 102218333A
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- zinc
- salt
- deionized water
- indium
- visible
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention relates to a method for preparing a visible light photocatalyst, specifically to a method for preparing a ZnIn2S4 visible-light activated photocatalyst at low temperature. The preparation method provided by the invention comprises the following steps of: adding zinc salt, indium salt and a sulfur source according to mol ratio into deionized water with uniformly mixing, placing the mixed solution into a reaction vessel, performing a hydrothermal reaction at the temperature of 30-80 DEG C; cooling, centrifuging, washing the precipitate with anhydrous ethanol and deionized water; drying to obtain the ZnIn2S4 visible-light activated photocatalyst powder. According to the invention, the ZnIn2S4 visible-light activated photocatalyst is synthesized at low temperature by using deionized water as the solvent without the addition of any other solvent, a surfactant or a template. The method provided by the invention needs mild condition as well as simple equipment and technology, and is easy to accomplish. The prepared material has a great industrial application prospect in the fields of photocatalysis, solar cells, wastewater degradation and the like.
Description
Technical field
The present invention relates to a kind of preparation method of visible light catalyst, specifically is a kind ofly to prepare ZnIn under 30 ℃-80 ℃ low temperature
2S
4The method of visible light catalyst.
Background technology
In the chemicals of produced worldwide, major part is to be made of synthetic textile dyestuff and other industrial dyes, and in all these dyestuffs, azo dyes and fluorone dyestuff are again two important parts.As everyone knows, some azo dyes (for example methyl orange) and fluorone dyestuff (for example rhodamine B) have high carcinogenic.Therefore, along with the increasingly stringent of international environment standard-required, need the key technology of these dyestuffs of efficient degradation badly.At present, the multiphase photocatalysis oxidation technology is widely used in the soluble dye in the degrading waste water.According to utilizing light source to divide, the multiphase photocatalysis oxidation technology can be divided into two kinds substantially, and a kind of is that light source is (as with TiO with the ultraviolet light
2Base is the photochemical catalyst of representative); Another kind be with the visible light be light source (as with ternary chalcongen ABxCY be representative photochemical catalyst-wherein A is Cu, Ag, Zn, Cd; B is Al, Ga, In; C is S, Se, Te; X and Y are constant).
In the multiphase photocatalysis oxidation technology take visible light as light source, ZnIn
2S
4As a kind of important ternary chalcongen compound semiconductor catalyst, because it has unique photoelectric properties and catalysis characteristics, be widely used in the fields such as thermoelectric material, material for optoelectronic devices, charge storage and the catalysis of photodissociation water.
The ZnIn that some scholars utilize diverse ways to prepare to have nanostructured or microballoon shape
2S
4, and use it for photolysis water hydrogen (Lei Z B, You W S, Liu M Y, et al.Chem.Commun.2003,2142-2143; Shen S H, Zhao L, Guo L J.Int.J.Hydrogen Energy.2008,33,4501-4510; Li M T, Su J Z, Guo L J.International Journal of Hydrogen Energy.2008,33,2891-2896), degradation of dye (Hu X L, Yu J C, Gong J M, et al.Crystal Growth Des.2007,7,2444-2448; Fang F, Chen L, Chen Y B, et al.J.Phys.Chem.C.2010,114,2393-2397), sterilization (Yu H T, Quan X, Zhang Y B, et al.Langmuir.2008,24, field such as 7599-7604).But make a general survey of existing open source literature, it prepares ZnIn
2S
4Required minimum synthesis temperature is 80 ℃, and solvent is usually selected organic solvent, also need add simultaneously other template or surfactant.
Summary of the invention
The present invention adopts the original position one kettle way, and in 30 ℃ of-80 ℃ of temperature ranges, Hydrothermal Synthesis goes out ZnIn
2S
4Visible light catalyst, solvent are deionized water, do not add other any organic solvents, template or surfactant, and have greatly improved the catalytic activity of its degradation of dye under radiation of visible light.
ZnIn of the present invention
2S
4Visible light catalyst is six side's phase crystal structures, is microspheroidal or irregular, and particle diameter is 10um-100um.
Concrete steps of the present invention are as follows:
The ratio in zinc salt, indium salt and sulphur source 1: 2: 4 in molar ratio～8 is joined in the deionized water, be stirred well to the solution mixing after, solution is sealed in from boosting in the stainless steel cauldron; Carry out hydro-thermal reaction 6～24h under 30 ℃～80 ℃ temperature conditions, hydro-thermal reaction naturally cools to 10～30 ℃ after finishing, centrifugation, and sediment is used respectively absolute ethyl alcohol and washed with de-ionized water; Being lower than under the reaction temperature condition behind (10 ℃～70 ℃) dry sediment 12～24h, obtain ZnIn
2S
4The visible light catalyst powder;
Described zinc salt is zinc nitrate, zinc chloride, zinc acetate, zinc sulfate, zinc oxalate or other divalent zinc salt, preferred zinc nitrate Zn (NO
3)
26H
2O; Described indium salt is indium nitrate, inidum chloride or other trivalent indium salt, preferred indium nitrate In (NO
3)
34.5H
2O; Described sulphur source is thiocarbamide, thioacetamide, preferred thioacetamide;
The gross mass of solutes such as described zinc salt, indium salt and sulphur source and the mass ratio of deionized water are 1～5: 10～500.
Effect of the present invention and benefit are, under 30 ℃ of lower-80 ℃ of conditions, are solvent with deionized water only, do not add any other solvent, surfactant or template, adopt the original position one kettle way to synthesize ZnIn
2S
4Visible light catalyst.This method consumed power, reaction condition be (30 ℃-80 ℃) as mild as a dove, and equipment and technology are simple, are easy to realize.Prepared material has better industrial application prospect in fields such as photocatalysis, solar cell and degrading waste waters.
Description of drawings
10 in the total accompanying drawing of the present invention, wherein:
Fig. 1 is the prepared ZnIn of embodiment 1
2S
4The X-ray powder diffraction figure of visible light catalyst.
Fig. 2 is the prepared ZnIn of embodiment 1
2S
4The SEM figure of visible light catalyst.
Fig. 3 is the prepared ZnIn of embodiment 2
2S
4The X-ray powder diffraction figure of visible light catalyst.
Fig. 4 is the prepared ZnIn of embodiment 3
2S
4The X-ray powder diffraction figure of visible light catalyst.
Fig. 5 is the prepared ZnIn of embodiment 3
2S
4The SEM figure of visible light catalyst.
Fig. 6 is the prepared ZnIn of embodiment 4
2S
4The X-ray powder diffraction figure of visible light catalyst.
Fig. 7 is the prepared ZnIn of embodiment 4
2S
4The SEM figure of visible light catalyst.
Fig. 8 is the prepared ZnIn of embodiment 5
2S
4The X-ray powder diffraction figure of visible light catalyst.
Fig. 9 is the prepared ZnIn of embodiment 6
2S
4The X-ray powder diffraction figure of visible light catalyst.
Figure 10 is prepared ZnIn among the embodiment of the invention 1, embodiment 3 and the embodiment 4
2S
4The UV-vis DRS abosrption spectrogram of visible light catalyst.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1
Accurately take by weighing 0.25mmol Zn (NO
3)
26H
2O, 0.5mmol In (NO
3)
34.5H
2The thioacetamide of O and 1.5mmol is put into the 50mL polytetrafluoroethylene bushing, accurately pipettes the 15mL deionized water as solvent with liquid-transfering gun, obtains colorless cleared solution behind the magnetic agitation 40min, and the sealing stainless steel cauldron is at 70 ℃ of lower reaction 16h.After the cooling, wash 3 times with absolute ethyl alcohol and deionized water respectively, at room temperature dried overnight obtains yellow powder.This yellow powder is accredited as six side's phase ZnIn through X-ray powder diffraction (accompanying drawing 1)
2S
4, and no any impurity in the product.Pattern characterizes (accompanying drawing 2) for being microspheroidal or irregular through ESEM, and particle diameter is at 20um-100um.
Accurately pipetting 250mL methyl orange dye waste water, to place volume be in the glass reactor of 250mL.Add 0.1g ZnIn
2S
4Particle powder places the darkroom with this reaction system, and lucifuge stirs 1h, makes suspension reach physical absorption-desorption balance fully.Open visible light source (adopt the 300W xenon lamp, filter the ultraviolet light of λ＜420nm) then, bottom stirs in illumination, every the 30min sampling, after high speed centrifugation separates, measures the back methyl orange waste water absorbance of degrading.Reaction result is: behind the illumination 1h, the methyl orange degradation rate is 50.8%; Behind the illumination 2h, degradation rate is 86.7%; Behind the illumination 2.5h, degradation rate is 95.9%; Behind the illumination 3h, degradable.
Embodiment 2
Repeat embodiment 1, other conditions are constant, will the reaction time become 8h.Products therefrom is accredited as six side's phase ZnIn through X-ray powder diffraction (accompanying drawing 3)
2S
4Degraded Methyl Orange in Wastewater reaction result is: behind the illumination 1h, the methyl orange degradation rate is 43.1%; Behind the illumination 2h, degradation rate is 79.8%; Behind the illumination 2.5h, degradation rate is 93.5%; Behind the illumination 3h, degradable.
Embodiment 3
Repeat embodiment 1, other conditions are constant, and reaction temperature is become 55 ℃.Products therefrom is accredited as six side's phase ZnIn through X-ray powder diffraction (accompanying drawing 4)
2S
4, pattern is characterized by through ESEM (accompanying drawing 5) and is microspheroidal or irregular.Degraded Methyl Orange in Wastewater reaction result is: behind the illumination 0.5h, the methyl orange degradation rate is 51.3%; Behind the illumination 1h, degradation rate is 83.5%; Behind the illumination 1.5h, degradable.
Embodiment 4
Repeat embodiment 1, other conditions are constant, and reaction temperature is become 45 ℃.Products therefrom is accredited as six side's phase ZnIn through X-ray powder diffraction (accompanying drawing 6)
2S
4, pattern is characterized by through ESEM (accompanying drawing 7) and is irregular.Degraded Methyl Orange in Wastewater reaction result is: behind the illumination 1h, the methyl orange degradation rate is 55.9%; Behind the illumination 1.5h, degradation rate is 75.0%; Behind the illumination 2h, degradation rate is 90.2%; Behind the illumination 2.5h, degradable.
Embodiment 5
Repeat embodiment 1, other conditions are constant, and reaction temperature is become 45 ℃, and the reaction time becomes 24h.Products therefrom is accredited as six side's phase ZnIn through X-ray powder diffraction (accompanying drawing 8)
2S
4
Embodiment 6
Repeat embodiment 1, other conditions are constant, and reaction temperature is become 35 ℃.Products therefrom is accredited as six side's phase ZnIn through X-ray powder diffraction (accompanying drawing 9)
2S
4Degraded Methyl Orange in Wastewater reaction result is: behind the illumination 0.5h, the methyl orange degradation rate is 65.5%; Behind the illumination 1h, degradation rate is 90.7%; Behind the illumination 1.5h, degradable.
Claims (4)
1. one kind prepares ZnIn at low temperatures
2S
4The method of visible light catalyst is characterized in that reaction raw materials is zinc salt, indium salt and sulphur source, and solvent is deionized water; Concrete preparation method is as follows:
1. the ratio with zinc salt, indium salt and sulphur source 1: 2: 4 in molar ratio～8 joins in the deionized water, is stirred well to mix;
Wherein, described zinc salt is zinc nitrate, zinc chloride, zinc acetate, zinc sulfate or zinc oxalate; Indium salt is indium nitrate or inidum chloride; The sulphur source is thiocarbamide or thioacetamide;
2. 1. described solution is transferred in the reactor, carries out hydro-thermal reaction 6～24h at 30 ℃～80 ℃;
3. hydro-thermal reaction naturally cools to 10～30 ℃ after finishing, centrifugation, and sediment is used absolute ethyl alcohol and washed with de-ionized water respectively;
4. at 10 ℃～70 ℃ dry sediment 12～24h, obtain ZnIn
2S
4The visible light catalyst powder.
2. preparation method according to claim 1 is characterized in that the gross mass of solutes such as the 1. described zinc salt of step, indium salt and sulphur source and the mass ratio of deionized water are 1～5: 10～500.
3. preparation method according to claim 1 and 2 is characterized in that described zinc salt is a zinc nitrate, and indium salt is indium nitrate, and the sulphur source is a thioacetamide.
4. preparation method according to claim 1 is characterized in that the 2. described hydrothermal temperature of step is 45 ℃～70 ℃, and the reaction time is 8～16h.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795661A (en) * | 2012-09-11 | 2012-11-28 | 黑龙江大学 | Method for preparing hierarchical floriform ZnIn2S4 ternary compound |
| CN102872885A (en) * | 2012-10-18 | 2013-01-16 | 中国科学技术大学 | Visible-light response type photocatalyst and preparation method thereof |
| CN103908971A (en) * | 2014-04-16 | 2014-07-09 | 福州大学 | Photocatalyst for selectively catalytically oxidizing and coupling amine to generate imine |
| CN105950140A (en) * | 2016-04-28 | 2016-09-21 | 江苏大学 | Method for preparing Ag:ZnIn2S4 luminescent quantum dots and photocatalyst |
| CN107744814A (en) * | 2017-10-20 | 2018-03-02 | 福州大学 | A kind of preparation method and application of composite photo-catalyst |
| CN108970623A (en) * | 2018-08-03 | 2018-12-11 | 南昌航空大学 | A kind of synthetic method of the visible light catalyst of controllable band gap |
| CN109692691A (en) * | 2018-11-30 | 2019-04-30 | 长沙学院 | Counter opal structure MIn2S4Catalysis material and its preparation method and application |
| CN110026207A (en) * | 2019-05-06 | 2019-07-19 | 青岛科技大学 | CaTiO3@ZnIn2S4Nanocomposite and the preparation method and application thereof |
| CN110721708A (en) * | 2019-10-25 | 2020-01-24 | 江西理工大学 | Full-spectrum absorption ZnIn2S4Preparation method and application of base heterojunction catalyst |
| CN111790404A (en) * | 2020-07-08 | 2020-10-20 | 齐鲁工业大学 | Defective type sulfur indium zinc microsphere visible light catalyst, preparation method and application |
| CN112960688A (en) * | 2021-02-04 | 2021-06-15 | 河南大学 | ZnIn2S4Sodium ion battery negative electrode material and preparation method thereof |
| CN113198492A (en) * | 2021-05-12 | 2021-08-03 | 郑州大学 | Catalyst for preparing pyruvate by photocatalytic oxidation of lactate and method thereof |
| CN114671457A (en) * | 2022-04-07 | 2022-06-28 | 南京工业大学 | Method for modifying surface of indium zinc sulfide by chloride ion modification |
| CN115090299A (en) * | 2022-07-25 | 2022-09-23 | 陕西科技大学 | ZnIn with sulfur defect 2 S 4 Preparation method of photocatalyst and application of photocatalyst in degrading antibiotics |
| CN115155618A (en) * | 2022-08-19 | 2022-10-11 | 广东工业大学 | ZnIn rich in Zn vacancy 2 S 4 Preparation method and application of photocatalyst |
| CN116351448A (en) * | 2023-02-20 | 2023-06-30 | 济南大学 | CoN@SiO 2 /ZnIn 2 S 4 Heterojunction photocatalyst and application thereof in photocatalytic hydrogen production |
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| CN101204652A (en) * | 2007-12-19 | 2008-06-25 | 中国科学院上海硅酸盐研究所 | High efficiency semiconductor photocatalysis and preparation method thereof |
| CN101254467A (en) * | 2008-04-11 | 2008-09-03 | 浙江大学 | Precipitating-hydrothermal preparation with high visible light catalytic activity nano CdxZn1-xS photocatalyst |
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2011
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| EP1127615A1 (en) * | 1998-09-09 | 2001-08-29 | Korea Research Institute of Chemical Technology | ZnS photocatalyst, its preparation and its use for producing hydrogen |
| CN101204652A (en) * | 2007-12-19 | 2008-06-25 | 中国科学院上海硅酸盐研究所 | High efficiency semiconductor photocatalysis and preparation method thereof |
| CN101254467A (en) * | 2008-04-11 | 2008-09-03 | 浙江大学 | Precipitating-hydrothermal preparation with high visible light catalytic activity nano CdxZn1-xS photocatalyst |
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Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795661A (en) * | 2012-09-11 | 2012-11-28 | 黑龙江大学 | Method for preparing hierarchical floriform ZnIn2S4 ternary compound |
| CN102795661B (en) * | 2012-09-11 | 2013-12-25 | 黑龙江大学 | Method for preparing hierarchical floriform ZnIn2S4 ternary compound |
| CN102872885A (en) * | 2012-10-18 | 2013-01-16 | 中国科学技术大学 | Visible-light response type photocatalyst and preparation method thereof |
| CN102872885B (en) * | 2012-10-18 | 2014-11-26 | 中国科学技术大学 | Visible-light response type photocatalyst and preparation method thereof |
| CN103908971A (en) * | 2014-04-16 | 2014-07-09 | 福州大学 | Photocatalyst for selectively catalytically oxidizing and coupling amine to generate imine |
| CN103908971B (en) * | 2014-04-16 | 2016-03-30 | 福州大学 | A kind of photochemical catalyst generating imines for selective catalytic oxidation coupling amine |
| CN105950140A (en) * | 2016-04-28 | 2016-09-21 | 江苏大学 | Method for preparing Ag:ZnIn2S4 luminescent quantum dots and photocatalyst |
| CN105950140B (en) * | 2016-04-28 | 2019-02-05 | 江苏大学 | It is a kind of to prepare Ag:ZnIn2S4The method of luminescent quantum dot and photochemical catalyst |
| CN107744814A (en) * | 2017-10-20 | 2018-03-02 | 福州大学 | A kind of preparation method and application of composite photo-catalyst |
| CN108970623A (en) * | 2018-08-03 | 2018-12-11 | 南昌航空大学 | A kind of synthetic method of the visible light catalyst of controllable band gap |
| CN109692691A (en) * | 2018-11-30 | 2019-04-30 | 长沙学院 | Counter opal structure MIn2S4Catalysis material and its preparation method and application |
| CN110026207A (en) * | 2019-05-06 | 2019-07-19 | 青岛科技大学 | CaTiO3@ZnIn2S4Nanocomposite and the preparation method and application thereof |
| CN110026207B (en) * | 2019-05-06 | 2022-04-29 | 青岛科技大学 | CaTiO3@ZnIn2S4Nano composite material and preparation method and application thereof |
| CN110721708A (en) * | 2019-10-25 | 2020-01-24 | 江西理工大学 | Full-spectrum absorption ZnIn2S4Preparation method and application of base heterojunction catalyst |
| CN111790404A (en) * | 2020-07-08 | 2020-10-20 | 齐鲁工业大学 | Defective type sulfur indium zinc microsphere visible light catalyst, preparation method and application |
| CN111790404B (en) * | 2020-07-08 | 2022-07-26 | 齐鲁工业大学 | Defective sulfur indium zinc microsphere visible light catalyst, preparation method and application |
| CN112960688A (en) * | 2021-02-04 | 2021-06-15 | 河南大学 | ZnIn2S4Sodium ion battery negative electrode material and preparation method thereof |
| CN112960688B (en) * | 2021-02-04 | 2022-04-12 | 河南大学 | ZnIn2S4Sodium ion battery negative electrode material and preparation method thereof |
| CN113198492A (en) * | 2021-05-12 | 2021-08-03 | 郑州大学 | Catalyst for preparing pyruvate by photocatalytic oxidation of lactate and method thereof |
| CN113198492B (en) * | 2021-05-12 | 2022-11-01 | 郑州大学 | Catalyst for preparing pyruvate by photocatalytic oxidation of lactate and method thereof |
| CN114671457A (en) * | 2022-04-07 | 2022-06-28 | 南京工业大学 | Method for modifying surface of indium zinc sulfide by chloride ion modification |
| CN115090299A (en) * | 2022-07-25 | 2022-09-23 | 陕西科技大学 | ZnIn with sulfur defect 2 S 4 Preparation method of photocatalyst and application of photocatalyst in degrading antibiotics |
| CN115155618A (en) * | 2022-08-19 | 2022-10-11 | 广东工业大学 | ZnIn rich in Zn vacancy 2 S 4 Preparation method and application of photocatalyst |
| CN116351448A (en) * | 2023-02-20 | 2023-06-30 | 济南大学 | CoN@SiO 2 /ZnIn 2 S 4 Heterojunction photocatalyst and application thereof in photocatalytic hydrogen production |
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Application publication date: 20111019 |