CN103240103B - A kind of ionic liquid and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst - Google Patents
A kind of ionic liquid and ultrasonic in combination prepare the method for cadmium sulfide sensitized zinc oxide heterojunction photocatalyst Download PDFInfo
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Abstract
The invention belongs to the preparation field of inorganic material zinc oxide (ZnO) heterojunction photocatalyst, particularly relate to a kind of method that ionic liquid and ultrasonic in combination prepare cadmium sulfide sensitized zinc oxide heterojunction photocatalyst, the method can be implemented as follows: the triethylene tetramine aqueous solution and dithyl sulfate are carried out neutralization reaction by (1), remove the water in mixed liquor, obtained triethylene tetramine dithyl sulfate type ionic liquid; (2) zinc oxide is prepared; (3) prepare triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, zinc oxide, caddy and thioacetamide are added in described triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, through ultrasonic process, are separated and obtain object product.The present invention adopts ionic liquid and supersonic synergic to prepare the ZnO heterojunction of cadmium sulfide sensitization, and simple to operation, cost is low, and obtained product purity is high, is expected to produce in enormous quantities.
Description
Technical field
The invention belongs to the preparation field of inorganic material zinc oxide (ZnO) heterojunction photocatalyst, particularly relate to a kind of method that ionic liquid and ultrasonic in combination prepare cadmium sulfide sensitized zinc oxide heterojunction photocatalyst.
Background technology
Society; energy crisis and environmental pollution become the key issue [Qiu Mingyan hindering human progress; Zhang Tianyong; Li Bin etc. material Leader A: a summary section; 2012; 26 (3): 48-52.]; how to solve the focus that these two thorny difficult problems become the research of numerous scholar; light-catalyzed reaction is that the energy utilizing ultraviolet or visible luminous energy to be converted into needed for chemical reaction produces catalytic action; the oxygen of surrounding and hydrone is made to be excited into the free radical having oxidability, the most organic pollution of decomposable asymmetric choice net and inorganic substances.Photocatalysis hydrogen production technology once obtain breakthrough can effective alleviating energy crisis.But, existing oxide type photocatalysis effect is poor, in order to overcome this shortcoming, people are from the visible light catalyst of development of new and carry out modification to existing broad stopband oxide type photochemical catalyst, and wherein semiconductors coupling technology is owing to compound that effectively separate electronic hole is right can improve the photocatalytic activity of photochemical catalyst and receive the concern of scholar.
The quantity how improving hetero-junctions for heterojunction type photocatalytic agent improves the key of its catalytic activity, and these two kinds of semiconductors just requiring to be formed hetero-junctions especially sensitized semiconductor have larger surface area and namely have less particle diameter.The mode of the surface nature of nano material and its synthesis, the reaction conditions such as the selection of reaction medium are relevant.Ionic liquid and the particle diameter for nano material such as ultrasonic have important impact [Enakshi Dinda, Satyabrata Si, Atanu Kotal, et al. Chem. Eur. J. 2008,14,5528 – 5537 to have document to show; Wang Yajuan, Li Chunxi, prince's pick etc. Beijing University of Chemical Technology's journal, 2002,29(4): 8-11].The vapour pressure that ionic liquid is less is conducive to the stronger cavitation of ultrasonic formation and then is formed with the external condition being beneficial to small particle diameter nano particle.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art part and provides one to be easy to operation, and cost is low, and object product purity is high, and the ionic liquid be 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.
Ionic liquid and ultrasonic in combination prepare a 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 mixed liquor, obtained triethylene tetramine dithyl sulfate type ionic liquid.
(2) preparation of zinc oxide.
(3) prepare triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, zinc oxide, caddy and thioacetamide are added in described triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, through ultrasonic process, are separated and obtain object product.
As a kind of preferred version, the mol ratio of triethylene tetramine of the present invention and dithyl sulfate can select 1 ~ 2:1 ~ 2.
As another kind of preferred version, in triethylene tetramine dithyl sulfate type ionic liquid aqueous solution of the present invention, the volume ratio of triethylene tetramine dithyl sulfate type ionic liquid and water is 0.14 ~ 0.30:1.
Further, 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 in the present invention.
Further, the time of the reaction of step of the present invention (3) can select 60 ~ 90 min.
Further, in step of the present invention (3), through ultrasonic process, after separation, dry 6h ~ 12h at being connected in 80 DEG C, obtains object product.
Triethylene tetramine is adopted to be cation one-step synthesis method ionic liquid in the present invention, and utilize this ionic liquid to synthesize the agent of ZnO/CdS heterojunction type photocatalytic, the synthesis or the ZnO/CdS heterojunction type photocatalytic agent preparation that are ionic liquid are all comparatively simple, and its process prepared meets Green Chemistry principle and prepared ZnO/CdS heterojunction photocatalysis activity has apparently higher than independent ZnO and is ZnO/CdS hetero-junctions prepared by medium with water.
The present invention adopts ionic liquid and supersonic synergic to prepare the ZnO heterojunction of cadmium sulfide sensitization, and simple to operation, cost is low, and obtained product purity is high, is expected to produce in enormous quantities.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the invention will be further described.Protection scope of the present invention is not only confined to the statement of following content.
Fig. 1 is ZnO field emission scanning electron microscope (SEM) photo.
Fig. 2 is ZnO field emission scanning electron microscope (SEM) partial enlargement photo.
Fig. 3 is ZnO/CdS field emission scanning electron microscope (SEM) photo prepared by pure water and ultrasonic in combination.
Fig. 4 is field emission scanning electron microscope (SEM) photo of the ZnO/CdS that the inventive method obtains.
Fig. 5 is field emission scanning electron microscope (SEM) the partial enlargement photo of the ZnO/CdS that the inventive method obtains.
Fig. 6 is ZnO, take water as ZnO/CdS(water prepared by medium) and X-ray diffraction (XRD) spectrogram of ZnO/CdS (IL) prepared of the aqueous solution of ionic liquid.
Fig. 7 is ZnO, take water as ZnO/CdS(water prepared by medium) and ZnO/CdS (IL) the photocatalytic degradation rhodamine B design sketch prepared of the aqueous solution of ionic liquid.
Detailed description of the invention
embodiment 1.
Triethylene tetramine is added dropwise in 200mL deionized water while stirring, is slowly added drop-wise in the aqueous solution of triethylene tetramine for 1:1 dithyl sulfate in molar ratio, stir and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5g, the thioacetamide of 0.7g caddy and 0.22g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 8h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
embodiment 2.
Triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stirs and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.2:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5 g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 10h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
embodiment 3.
Triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stirs and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.3:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then the zinc oxide of 0.5g is got, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, is separated and obtains product, wash away impurity, dry 11h at 80 DEG C.Cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
embodiment 4.
Triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stirs and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.8 g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 12h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
embodiment 5.
Triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stirs and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then the zinc oxide of 1.0g is got, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, is separated and obtains product, wash away impurity, dry 11h at 80 DEG C.Cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
embodiment 6.
Triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stirs and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then the zinc oxide of 0.5 g is got, the thioacetamide of 0.8 g caddy and 0.26 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, is separated and obtains product, wash away impurity, dry 6h ~ 12h at 80 DEG C.Cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
embodiment 7.
Triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stirs and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then the zinc oxide of 0.5 g is got, the thioacetamide of 0.9 g caddy and 0.3 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, is separated and obtains product, wash away impurity, dry 6h ~ 12h at 80 DEG C.Cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
embodiment 8.
Triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stirs and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then the zinc oxide of 0.5 g is got, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 80 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, is separated and obtains product, wash away impurity, dry 6h ~ 12h at 80 DEG C.Cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
embodiment 9.
Triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stirs and make it that neutralization reaction occur.Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours.Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid.The preparation of zinc oxide can adopt [bibliography: Yongjiang Sun, Li Wang, Xuegang Yu, Kezheng Chen. CrystEngComm, 2012,14,3199-3204], certainly, other technologies scheme also can be adopted to prepare.By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5 g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 90 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 7h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, slowly be added drop-wise in the aqueous solution of triethylene tetramine for 1:1 dithyl sulfate in molar ratio, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5g, the thioacetamide of 0.7g caddy and 0.22g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 8h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
2. 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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.2:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5 g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 10h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
3. 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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.3:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 11h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
4. 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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.8 g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 12h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
5. 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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 1.0g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 11h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
6. 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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5 g, the thioacetamide of 0.8 g caddy and 0.26 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 6h ~ 12h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
7. 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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5 g, the thioacetamide of 0.9 g caddy and 0.3 g joins ultrasonic process 60 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 6h ~ 12h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
8. 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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5 g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 80 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 6h ~ 12h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
9. 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: triethylene tetramine is added dropwise to while stirring in 200mL deionized water, in molar ratio for the dithyl sulfate of 1:1 is slowly added drop-wise in the aqueous solution of triethylene tetramine, stir and make it that neutralization reaction occur; Ice bath is set in reaction process to prevent because heat release causes solution evaporation, continues stirring 6 hours; Subsequently, employing Rotary Evaporators steams the water in mixed liquor, obtains triethylene tetramine dithyl sulfate type ionic liquid; By volume for 0.14:1 prepares triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, be stirred to ionic liquid to be dissolved in the water completely, get this solution of 40ml, then get the zinc oxide of 0.5 g, the thioacetamide of 0.7g caddy and 0.22 g joins ultrasonic process 90 min in above-mentioned triethylene tetramine dithyl sulfate type ionic liquid aqueous solution, after reaction terminates, separation obtains product, wash away impurity, dry 7h at 80 DEG C, cadmium sulfide sensitized zinc oxide hetero-junctions can be obtained.
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| 载流子调控的ZnO-CdS异质结构光催化制氢材料研究;王学文等;《第十三届全国太阳能光化学与光催化学术会议》;20121231;92-293 * |
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