CN103240103A - Method for preparing cadmium sulfide sensitized zinc oxide heterojunction photocatalyst by combination of ionic liquid and ultrasonic treatment - Google Patents
Method for preparing cadmium sulfide sensitized zinc oxide heterojunction photocatalyst by combination of ionic liquid and ultrasonic treatment Download PDFInfo
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- CN103240103A CN103240103A CN2013101500058A CN201310150005A CN103240103A CN 103240103 A CN103240103 A CN 103240103A CN 2013101500058 A CN2013101500058 A CN 2013101500058A CN 201310150005 A CN201310150005 A CN 201310150005A CN 103240103 A CN103240103 A CN 103240103A
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Abstract
The invention belongs to the field of preparation of an inorganic material zinc oxide heterojunction photocatalyst, and particularly relates to a method for preparing a cadmium sulfide sensitized zinc oxide heterojunction photocatalyst by combination of ionic liquid and ultrasonic treatment. The method comprises the following steps: 1, carrying out neutralization reaction on a triethylene tetramine aqueous solution and diethyl sulfate and removing water out of the mixed solution to obtain a triethylene tetramine-diethyl sulfate type ionic liquid; 2, preparing zinc oxide; and 3, preparing a triethylene tetramine-diethyl sulfate type ionic liquid aqueous solution, adding zinc oxide, cadmium chloride and thioacetamide to the triethylene tetramine-diethyl sulfate type ionic liquid aqueous solution, carrying out ultrasonic treatment and separation to finally obtain the target product. The method for preparing the cadmium sulfide sensitized zinc oxide heterojunction photocatalyst by combination of ionic liquid and ultrasonic treatment is simple to operate and low in cost and the prepared product has high purity and can be expected to be produced on large scale.
Description
Technical field
The invention belongs to the preparation field of inorganic material zinc oxide (ZnO) heterojunction photocatalyst, relate in particular to the method that a kind of ionic liquid and ultrasonic in combination prepare cadmium sulfide sensitized zinc oxide heterojunction photocatalyst.
Background technology
Current society; energy crisis and environmental pollution become the key issue [Qiu Mingyan that hinders human progress; Zhang Tianyong; Li Bin etc. material Leader A: a summary piece of writing; 2012; 26 (3): 48-52.]; how solving these two thorny difficult problems becomes the focus of numerous scholars' research; light-catalyzed reaction is to utilize ultraviolet or visible luminous energy to be converted into the required energy of chemical reaction to produce catalytic action; oxygen and hydrone around making are excited into the free radical that has oxidability, can decompose most organic pollution and inorganic substances.The photocatalysis hydrogen production technology is in case obtain to break through effectively alleviating energy crisis.But, existing oxide type photocatalysis effect is relatively poor, in order to overcome this shortcoming, people carry out modification from the visible light catalyst of development of new with to existing broad stopband oxide type photochemical catalyst, and wherein the semiconductor complex technique receives scholar's concern owing to the photocatalytic activity of the right compound raising photochemical catalyst in effective separate electronic hole.
The quantity that how to improve hetero-junctions for the heterojunction type photocatalytic agent is to improve the key of its catalytic activity, and these two kinds of semiconductors that just require to form hetero-junctions especially sensitized semiconductor have bigger surface area and namely have smaller particle size.The surface nature of nano material and its synthetic mode, reaction conditions such as the selection of reaction medium are relevant.There is document to show that ionic liquid and particle diameter for nano material such as ultrasonic have significant effects [Enakshi Dinda, Satyabrata Si, Atanu Kotal, et al. Chem. Eur. J. 2008,14,5528 – 5537; Wang Yajuan, Li Chunxi, prince's pick etc. Beijing University of Chemical Technology's journal, 2002,29(4): 8-11].The less vapour pressure of ionic liquid is conducive to the stronger cavitation of ultrasonic formation and then is formed with the external condition that is beneficial to the small particle diameter nano particle.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art part and a kind of easy operating is provided, and cost is low, purpose product purity height, and the ionic liquid that is produced on a large scale and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst.
For solving the problems of the technologies described above, the present invention realizes like this.
A kind of ionic liquid and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst, can implement as follows.
(1) the triethylene tetramine aqueous solution and dithyl sulfate are carried out neutralization reaction, remove the water in the mixed liquor, make triethylene tetramine dithyl sulfate type ionic liquid.
(2) preparation of zinc oxide.
(3) preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution is added to zinc oxide, caddy and thioacetamide in the described triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, through ultrasonic processing, separates namely getting the purpose product.
As a kind of preferred version, the mol ratio of triethylene tetramine of the present invention and dithyl sulfate can be selected 1～2:1～2.
As another kind of preferred version, the volume ratio of triethylene tetramine dithyl sulfate type ionic liquid and water is 0.14～0.30:1 in the triethylene tetramine dithyl sulfate type ionic liquid aqueous solution of the present invention.
Further, the present invention by quality ratio, described zinc oxide, caddy and thioacetamide addition are followed successively by: 0.5～1:0.7～0.9:0.22～0.3.
Further, the time of the reaction of step of the present invention (3) can be selected 60～90 min.
Further, in the step of the present invention (3), through ultrasonic processing, after the separation, be connected in 80 ℃ of dry 6h～12h down, namely get the purpose product.
Adopt triethylene tetramine to be the synthetic ionic liquid of cation one-step method in the present invention, and utilize this ionic liquid to synthesize the agent of ZnO/CdS heterojunction type photocatalytic, be that the synthetic of ionic liquid or the agent of ZnO/CdS heterojunction type photocatalytic preparation is all comparatively simple, it is the ZnO/CdS hetero-junctions of medium preparation that the process of its preparation meets that Green Chemistry principle and prepared ZnO/CdS heterojunction photocatalysis activity have apparently higher than independent ZnO with water.
The present invention adopts ionic liquid and supersonic synergic to prepare the zinc oxide heterogeneous knot of cadmium sulfide sensitization, and simple to operation, cost is low, and the product purity height that makes is expected to produce in enormous quantities.
Description of drawings
The invention will be further described below in conjunction with the drawings and specific embodiments.Protection scope of the present invention not only is confined to the statement of following content.
Fig. 1 is ZnO field emission scanning electron microscope (SEM) photo.
Fig. 2 is the local enlarged photograph of ZnO field emission scanning electron microscope (SEM).
Fig. 3 is ZnO/CdS field emission scanning electron microscope (SEM) photo of pure water and ultrasonic in combination preparation.
Field emission scanning electron microscope (SEM) photo of the ZnO/CdS that Fig. 4 makes for the inventive method.
The local enlarged photograph of field emission scanning electron microscope (SEM) of the ZnO/CdS that Fig. 5 makes for the inventive method.
Fig. 6 is ZnO, be the ZnO/CdS(water of medium preparation with water) and X-ray diffraction (XRD) spectrogram of the ZnO/CdS (IL) for preparing of the aqueous solution of ionic liquid.
Fig. 7 is ZnO, be the ZnO/CdS(water of medium preparation with water) and ZnO/CdS (IL) the photocatalytic degradation rhodamine B design sketch for preparing of the aqueous solution of ionic liquid.
The specific embodiment
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, slowly is added drop-wise in the aqueous solution of triethylene tetramine for the 1:1 dithyl sulfate in molar ratio, stir and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.14:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 0.5g then, the thioacetamide of 0.7g caddy and 0.22g joins ultrasonic processing 60 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separate and obtain product, flush away impurity, 80 ℃ of following dry 8h can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
Embodiment 2.
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, in molar ratio for the dithyl sulfate of 1:1 slowly is added drop-wise in the aqueous solution of triethylene tetramine, stirs and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.2:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 0.5 g then, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic processing 60 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separate and obtain product, flush away impurity, 80 ℃ of following dry 10h can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
Embodiment 3.
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, in molar ratio for the dithyl sulfate of 1:1 slowly is added drop-wise in the aqueous solution of triethylene tetramine, stirs and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.3:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 0.5g then, 0.7g the thioacetamide of caddy and 0.22 g joins ultrasonic processing 60 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separates obtaining product, flush away impurity, 80 ℃ of following dry 11h.Can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
Embodiment 4.
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, in molar ratio for the dithyl sulfate of 1:1 slowly is added drop-wise in the aqueous solution of triethylene tetramine, stirs and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.14:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 0.8 g then, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic processing 60 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separate and obtain product, flush away impurity, 80 ℃ of following dry 12h can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
Embodiment 5.
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, in molar ratio for the dithyl sulfate of 1:1 slowly is added drop-wise in the aqueous solution of triethylene tetramine, stirs and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.14:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 1.0g then, 0.7g the thioacetamide of caddy and 0.22 g joins ultrasonic processing 60 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separates obtaining product, flush away impurity, 80 ℃ of following dry 11h.Can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
Embodiment 6.
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, in molar ratio for the dithyl sulfate of 1:1 slowly is added drop-wise in the aqueous solution of triethylene tetramine, stirs and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.14:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 0.5 g then, 0.8 the thioacetamide of g caddy and 0.26 g joins ultrasonic processing 60 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separates obtaining product, flush away impurity, 80 ℃ of following dry 6h～12h.Can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
Embodiment 7.
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, in molar ratio for the dithyl sulfate of 1:1 slowly is added drop-wise in the aqueous solution of triethylene tetramine, stirs and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.14:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 0.5 g then, 0.9 the thioacetamide of g caddy and 0.3 g joins ultrasonic processing 60 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separates obtaining product, flush away impurity, 80 ℃ of following dry 6h～12h.Can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
Embodiment 8.
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, in molar ratio for the dithyl sulfate of 1:1 slowly is added drop-wise in the aqueous solution of triethylene tetramine, stirs and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.14:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 0.5 g then, 0.7g the thioacetamide of caddy and 0.22 g joins ultrasonic processing 80 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separates obtaining product, flush away impurity, 80 ℃ of following dry 6h～12h.Can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
Embodiment 9.
Triethylene tetramine is added dropwise in the 200mL deionized water while stirring, in molar ratio for the dithyl sulfate of 1:1 slowly is added drop-wise in the aqueous solution of triethylene tetramine, stirs and make its generation neutralization reaction.Ice bath is set to prevent in the reaction process because heat release causes solution evaporation, continues to stir 6 hours.Subsequently, the employing Rotary Evaporators steams the water in the mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can be adopted [list of references: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, also can adopt the preparation of other technologies scheme.Be 0.14:1 preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution by volume, being stirred to ionic liquid is dissolved in the water fully, get this solution of 40ml, get the zinc oxide of 0.5 g then, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic processing 90 min in the above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction finishes, separate and obtain product, flush away impurity, 80 ℃ of following dry 7h can obtain cadmium sulfide sensitized zinc oxide hetero-junctions.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. an ionic liquid and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst, it is characterized in that, implement as follows:
(1) the triethylene tetramine aqueous solution and dithyl sulfate are carried out neutralization reaction, remove the water in the mixed liquor, make triethylene tetramine dithyl sulfate type ionic liquid;
(2) preparation of zinc oxide;
(3) preparation triethylene tetramine dithyl sulfate type ionic liquid aqueous solution is added to zinc oxide, caddy and thioacetamide in the described triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, through ultrasonic processing, separates namely getting the purpose product.
2. ionic liquid according to claim 1 and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst, it is characterized in that: the mol ratio of described triethylene tetramine and dithyl sulfate is 1～2:1～2.
3. ionic liquid according to claim 2 and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst, it is characterized in that: the volume ratio of triethylene tetramine dithyl sulfate type ionic liquid and water is 0.14～0.30:1 in the described triethylene tetramine dithyl sulfate type ionic liquid aqueous solution.
4. ionic liquid according to claim 3 and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst, it is characterized in that: by quality ratio, described zinc oxide, caddy and thioacetamide addition are followed successively by: 0.5～1:0.7～0.9:0.22～0.3.
5. ionic liquid according to claim 4 and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst, it is characterized in that: the time of the reaction of described step (3) is 60～90 min.
6. the method for preparing cadmium sulfide sensitized zinc oxide heterojunction photocatalyst according to arbitrary described ionic liquid and the ultrasonic in combination of claim 1～4, it is characterized in that: in the described step (3), through ultrasonic processing, after the separation, be connected in 80 ℃ of dry 6h～12h down, namely get the purpose product.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641741A (en) * | 2011-02-16 | 2012-08-22 | 中国科学院金属研究所 | Composite photocatalyst with metal cadmium as core and heterostructure as shell and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102641741A (en) * | 2011-02-16 | 2012-08-22 | 中国科学院金属研究所 | Composite photocatalyst with metal cadmium as core and heterostructure as shell and preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 王学文等: "载流子调控的ZnO-CdS异质结构光催化制氢材料研究", 《第十三届全国太阳能光化学与光催化学术会议》, 31 December 2012 (2012-12-31), pages 92 - 293 * |
| 赵荣祥等: "离子液体对硫化镉粒径和光催化性能调控研究", 《人工晶体学报》, vol. 41, no. 4, 31 August 2012 (2012-08-31), pages 987 - 994 * |
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