CN103433060B - Core-shell TiO2/ZnIn2S4 composite photocatalyst and preparation method and application thereof - Google Patents
Core-shell TiO2/ZnIn2S4 composite photocatalyst and preparation method and application thereof Download PDFInfo
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- CN103433060B CN103433060B CN201310371019.2A CN201310371019A CN103433060B CN 103433060 B CN103433060 B CN 103433060B CN 201310371019 A CN201310371019 A CN 201310371019A CN 103433060 B CN103433060 B CN 103433060B
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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 discloses a preparation method and an application of a core-shell TiO2/ZnIn2S4 composite photocatalyst. The preparation method comprises the following steps: performing ultrasonic dispersion on TiO2 in an ethanol solvent; adding zinc chloride and indium nitrate into the ethanol solvent, and stirring to dissolve; mixing the two systems, and adding thioacetamide; transferring the mixed system into a high pressure kettle to react; performing vacuum filtration, washing, drying and grinding on a product after the reaction is finished to obtain the core-shell TiO2/ZnIn2S4 composite photocatalyst. According to the method, the core-shell TiO2/ZnIn2S4 composite photocatalyst is prepared in one step by adopting a solvothermal synthesis method, the catalyst is wide in visible light response range and high in photocatalysis activity, is applicable to organic dye wastewater degradation, and can be used for degrading methylene blue-containing wastewater in the field of solar energy transformation and utilization and environment management.
Description
Technical field
The present invention relates to a kind of photochemical catalyst, particularly relate to a kind of He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst and preparation method thereof and application; Belong to new structure catalysis material technical field, for degrading organic dye waste water.
Background technology
Along with the appearance of the problems such as the in short supply and environmental pollution of global energy, the development and utilization of novel energy becomes the theme that current era receives much attention.Solar energy because it is inexhaustible, the clean advantage such as pollution-free, renewable, so utilize semiconductor light-catalyst that light energy conversion has been become to the focus of vast scholar's research for electric energy and chemical energy.
ZnIn
2s
4a kind of very important semi-conducting material with visible light-responded performance, its energy gap 2.3eV that only has an appointment, this also makes it can absorb efficiently solar energy.In more than ten years in the past, ZnIn
2s
4oneself is widely used in the research of organic and inorganic pollutant in photocatalytic hydrogen production by water decomposition under visible ray and photocatalytic degradation water or air.But, as a kind of photochemical catalyst ZnIn
2s
4in application, also there is the problem that photocatalysis quantum efficiency is lower.In order to improve ZnIn
2s
4photocatalysis quantum efficiency, scientific research author has made many explorations, as by control pattern reach change ZnIn
2s
4the surface texture of nano particle; By ZnIn
2s
4particulate load reaches homodisperse ZnIn on Graphene or multilayer carbon nanotube
2s
4particle; Containing transition metal ion and by compound to reaching effective separation of photogenerated charge two kinds of semiconductors, thus ZnIn improved
2s
4quantum efficiency.
Summary of the invention
The object of the present invention is to provide a kind of wide visible light-responded scope, highlight catalytic active He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst.
Another object of the present invention be to provide above-mentioned visible light-responded He ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst.
The present invention also have an object be to provide He ?shell mould TiO
2/ ZnIn
2s
4the application of composite photo-catalyst in degrading organic dye waste water.
The present invention by solvent-thermal method by ZnIn
2s
4be grown in TiO
2on surface, form special He ?shell structure composite photo-catalyst, the hetero-junctions between both interfaces is conducive to the transmission of Pair production, reduces the recombination rate in its light induced electron and hole, thereby improves the photocatalysis efficiency of catalyst.
Object of the present invention is achieved through the following technical solutions:
A kind of He ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst, comprises the following steps:
(1) by TiO
2in alcohol solvent, ultrasonic dispersion, makes suspension; Every 3mL alcohol solvent adds the TiO of 1mg～4mg
2;
(2) stirring and dissolving in alcohol solvent by zinc chloride and indium nitrate;
(3) suspension step (1) being made mixes with the solution that step (2) makes, and adds thioacetamide and stirs; The mol ratio of controlling zinc chloride, inidum chloride and thioacetamide is 1:2:6;
(4) reaction system of step (3) is transferred to and in autoclave, carries out solvent thermal reaction; Control reaction temperature be 160 ?200 DEG C, the reaction time be 6 ?12 hours;
(5) pour step (4) product in vacuum filtration device suction filtration, with deionized water washing, dry, after grinding, obtain core ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst.
Preferably, in step (1) frequency of ultrasonic processing be 40 ?45KHz, power be 50 ?75W, the time be 10 ?15 minutes.In step (3), the time of stirring be 20 ?40 minutes.Described baking temperature be 60 ?80 DEG C, drying time be 4 ?6 hours.
A kind of He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst, is made by above-mentioned preparation method.
Described He ?shell mould TiO
2/ ZnIn
2s
4the application of composite photo-catalyst in organic dye waste water degraded.
With respect to prior art, tool of the present invention has the following advantages and beneficial effect:
(1) the present invention by solvent-thermal method by ZnIn
2s
4be grown in TiO
2on surface, form special He ?shell structure composite photo-catalyst, the hetero-junctions between both interfaces is conducive to the transmission of Pair production, reduces the recombination rate in its light induced electron and hole, thereby improves the photocatalysis efficiency of catalyst.
(2) by solvent thermal reaction ， He ?shell mould TiO
2/ ZnIn
2s
4formation one step of composite photo-catalyst completes, and preparation technology is simple, with low cost, is conducive to extensive preparation.
(3) composite photo-catalyst of the present invention has wide visible light-responded scope, highlight catalytic active, is applicable to the fields such as solar energy trans-utilization and environmental improvement, as the degraded that contains methylene blue organic dyestuff industrial wastewater.
Brief description of the drawings
Fig. 1 is TiO in embodiment 1
2znIn with preparation
2s
4, He ?shell mould TiO
2/ ZnIn
2s
4the X-ray diffractogram of composite photo-catalyst;
Fig. 2 is TiO in embodiment 1
2znIn with preparation
2s
4, He ?shell mould TiO
2/ ZnIn
2s
4the Zi Wai of composite photo-catalyst ?visible absorption spectra figure;
Fig. 3 be in embodiment 1, prepare He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst transmission electron microscope picture;
Fig. 4 is TiO in embodiment 1
2znIn with preparation
2s
4, He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst is the change curve with degradation time to the degradation rate of methylene blue.
Detailed description of the invention
For understanding better the present invention, below in conjunction with drawings and Examples, the invention will be further described, but embodiments of the present invention are not limited to this.
Embodiment 1
A kind of visible light-responded He ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst, comprises the following steps:
(1) by 20mg TiO
2ultrasonic dispersion 10 minutes in 30ml alcohol solvent, the frequency of ultrasonic processing is 40KHz, power is 50W;
(2) stirring and dissolving in 30ml alcohol solvent by 2mmol zinc chloride and 4mmol indium nitrate;
(3) suspension step (1) being made mixes with the solution that step (2) makes, and adds 12mmol thioacetamide and stirs 20 minutes with the rotating speed of 500r/min;
(4) reaction system of step (3) is transferred in autoclave, 160 DEG C of conditions are reacted 6 hours;
(5) pour step (4) product in vacuum filtration device suction filtration, with deionized water washing, under 60 DEG C of conditions, be dried 6 hours, after grinding, obtain core ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst.
Fig. 1 is TiO in embodiment 1
2znIn with preparation
2s
4, He ?shell mould TiO
2/ ZnIn
2s
4the X-ray diffractogram of composite photo-catalyst.As shown in Figure 1, TiO
2/ ZnIn
2s
4in the diffractive features peak of sample, can observe TiO
2and ZnIn
2s
4the characteristic peak of two kinds of materials, illustrates and has successfully prepared TiO
2/ ZnIn
2s
4composite photo-catalyst; As shown in Figure 2, TiO
2/ ZnIn
2s
4in visible-range, there is strong absorbance, TiO is described
2/ ZnIn
2s
4there is visible light catalysis activity; From Fig. 3 transmission electron microscope photo, can observe obvious He ?shell structure, confirmed successfully to make He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst.
Embodiment 2
A kind of visible light-responded He ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst, comprises the following steps:
(1) by 40mg TiO
2ultrasonic dispersion 12 minutes in 30ml alcohol solvent; The frequency of ultrasonic processing is 40KHz, and power is 50W;
(2) stirring and dissolving in 30ml alcohol solvent by 2mmol zinc chloride and 4mmol indium nitrate;
(3) suspension step (1) being made mixes with the solution that step (2) makes, and adds 12mmol thioacetamide and stirs 30 minutes with the rotating speed of 500r/min;
(4) reaction system of step (3) is transferred in autoclave, 180 DEG C of conditions are reacted 8 hours;
(5) pour step (4) product in vacuum filtration device suction filtration, with deionized water washing, under 70 DEG C of conditions, be dried 5 hours, after grinding, obtain core ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst.
TiO in the present embodiment
2/ ZnIn
2s
4x-ray diffractogram, visible light catalysis activity He the He of composite photo-catalyst ?shell structure and figure 1 ?3 similar.
Embodiment 3
A kind of visible light-responded He ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst, comprises the following steps:
(1) by 80mg TiO
2ultrasonic dispersion 15 minutes in 30ml alcohol solvent; The frequency of ultrasonic processing is 45KHz, and power is 75W;
(2) stirring and dissolving in 30ml alcohol solvent by 2mmol zinc chloride and 4mmol indium nitrate;
(3) suspension step (1) being made mixes with the solution that step (2) makes, and adds 12mmol thioacetamide and stirs 40 minutes with the rotating speed of 500r/min;
(4) reaction system of step (3) is transferred in autoclave, 200 DEG C of conditions are reacted 12 hours;
(5) pour step (4) product in vacuum filtration device suction filtration, with deionized water washing, under 80 DEG C of conditions, be dried 4 hours, after grinding, obtain core ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst.
TiO in the present embodiment
2/ ZnIn
2s
4x-ray diffractogram, visible light catalysis activity He the He of composite photo-catalyst ?shell structure and figure 1 ?3 similar.
Application Example
Use preparation He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst light degradation organic dyestuff: the photocatalytic activity of evaluating this catalyst taking aqueous solution of methylene blue as simulation sewage.Experiment condition is set to: (1) by embodiment 1 preparation 20mg He ?shell mould TiO
2/ ZnIn
2s
4it is 20mgL that composite photo-catalyst is distributed to 120mL concentration
?1aqueous solution of methylene blue in, before illumination reaction, first suspension is placed in to dark surrounds magnetic agitation 1h, so that system reaches adsorption/desorption balance; (2) open simulated solar light source, each illumination sampled after 30 minutes, centrifugal, detected the variation of the outer ?visible absorbance value of purple of Methylene Blue in Solution solution.
Fig. 4 is TiO in embodiment 1
2znIn with preparation
2s
4, He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst is the change curve with light application time to the degradation rate of methylene blue.Known in conjunction with Fig. 4, under radiation of visible light, TiO
2to methylene blue, degraded does not have catalytic activity; After illumination 4 hours, ZnIn
2s
4the methylene blue of degradable 71%, Er He ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst can reach 92% to the degradation rate of methylene blue, has greatly improved TiO
2and ZnIn
2s
4visible light catalysis activity.
Claims (6)
1. a core ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst, is characterized in that comprising the following steps:
(1) by TiO
2in alcohol solvent, ultrasonic dispersion, makes suspension; Every 3mL alcohol solvent adds the TiO of 1mg～4mg
2;
(2) stirring and dissolving in alcohol solvent by zinc chloride and indium nitrate;
(3) suspension step (1) being made mixes with the solution that step (2) makes, and adds thioacetamide and stirs; The mol ratio of controlling zinc chloride, inidum chloride and thioacetamide is 1:2:6;
(4) reaction system of step (3) is transferred to and in autoclave, carries out solvent thermal reaction; Control reaction temperature be 160 ?200 DEG C, the reaction time be 6 ?12 hours;
(5) pour step (4) product in vacuum filtration device suction filtration, with deionized water washing, dry, after grinding, obtain core ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst.
He according to claim 1 ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst, is characterized in that: in step (1) frequency of ultrasonic processing be 40 ?45KHz, power be 50 ?75W, the time be 10 ?15 minutes.
He according to claim 1 ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst, is characterized in that: in step (3), the time of stirring be 20 ?40 minutes.
He according to claim 1 ?shell mould TiO
2/ ZnIn
2s
4the preparation method of composite photo-catalyst, is characterized in that: described baking temperature be 60 ?80 DEG C, drying time be 4 ?6 hours.
5. a core ?shell mould TiO
2/ ZnIn
2s
4composite photo-catalyst, is characterized in that: its by claim 1 ?preparation method described in 4 any one make.
He claimed in claim 5 ?shell mould TiO
2/ ZnIn
2s
4the application of composite photo-catalyst in degrading organic dye waste water.
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| CN201310371019.2A CN103433060B (en) | 2013-08-22 | 2013-08-22 | Core-shell TiO2/ZnIn2S4 composite photocatalyst and preparation method and application thereof |
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| CN103433060B true CN103433060B (en) | 2014-12-03 |
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| CN107552073A (en) * | 2017-09-13 | 2018-01-09 | 重庆大学 | A kind of MoS2Preparation method of AIZS nano composite materials and products thereof and application |
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