CN103950968A - Method for preparing CdS semiconductor photocatalyst and application of product prepared by method - Google Patents
Method for preparing CdS semiconductor photocatalyst and application of product prepared by method Download PDFInfo
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- CN103950968A CN103950968A CN201410198686.XA CN201410198686A CN103950968A CN 103950968 A CN103950968 A CN 103950968A CN 201410198686 A CN201410198686 A CN 201410198686A CN 103950968 A CN103950968 A CN 103950968A
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- cadmium
- cds
- semiconductor light
- acid
- hydrogen sulfide
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
-
- 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
Abstract
The invention discloses a method for preparing a CdS semiconductor photocatalyst and an application of a product prepared by the method. The preparation method comprises the steps of mixing hydrogen sulfide with strong acid at 20-30 DEG C, vigorously stirring, and reacting for 3-20 hours to obtain a strong acid solution of hydrogen sulfide; dropwise adding a cadmium salt solution into the strong acid solution of hydrogen sulfide, reacting for 0.5-20 hours at 20-30 DEG C, filtering, washing with water, filtering and drying to obtain CdS powder; carrying out heat treatment on the CdS powder under the protection of nitrogen, then grinding the product, washing with acid and water, filtering and drying to obtain a CdS semiconductor photocatalyst. According to the method, the dispersion effect of CdS is improved, the transport distance between CdS particles is shortened, the photocorrosion rate of a CdS surface is retarded, and the photocatalytic activity of CdS is improved. The CdS semiconductor photocatalyst has superior photocatalytic degradation activity in the application in degrading organic pollutants.
Description
Technical field
The present invention relates to field of photocatalytic material, be specifically related to a kind of preparation method of CdS semiconductor light-catalyst and make the application of product.
Background technology
Along with the field wastewater discharges such as weaving, printing and dyeing, papermaking increase day by day, how effectively to administer its pollution to environment, be one of focus of environmental area research always.Sun power is a kind of inexhaustible, nexhaustible renewable and clean energy resource, utilizes sun power to carry out photocatalysis degradation organic contaminant, is one of study hotspot of photocatalysis field always.
Photocatalyst is that one can be CO by organic pollutant degradation
2and H
2the material of O.Researcher is studied semiconductor light-catalyst on the basis of many semiconductor light-catalyst photocatalysis performances, as TiO2, Cu2S, ZnO, NiFe2O4, CdS, Bi
2s
3, CdS/CoFeO4, ZnS/CdS and CdS/TiO
2deng.In numerous semiconductor light-catalysts, CdS is because its unique advantage receives much concern.
The energy gap of CdS (Cadmium Sulfide) is 2.4 eV left and right, and has excellent visible light-responded characteristic.The experimental results shows, although CdS has certain photocatalytic activity,, CdS exist Photocatalytic activity low, be easy to the defects such as reunion, greatly limit its application in photocatalysis field.The defect existing in order to solve CdS, researcher has carried out a large amount of research work at the aspect such as reunion and Photocatalytic activity of improving CdS.At present, the method that prepared by CdS mainly contains: 1. solid phase method; 2. liquid phase method; 3. original position is synthetic etc., but after preparation, the photocatalysis performance of CdS improves not obvious.
Summary of the invention
The object of this invention is to provide a kind of preparation method of CdS semiconductor light-catalyst and make the application of product, the method has improved the dispersion effect of CdS, shorten the transmission distance between CdS particle, slow down the photoetch speed on CdS surface, not only can reduce the agglomeration of CdS, and improve the photocatalytic activity of CdS.CdS semiconductor light-catalyst is applied in organic pollutant degradation aspect, has more excellent Photocatalytic activity.
Object of the present invention is achieved through the following technical solutions:
A preparation method for CdS semiconductor light-catalyst, is characterized in that this preparation method is as follows:
(1) under 20-30 DEG C of condition, hydrogen sulfide and strong acid to be mixed, vigorous stirring, reacts 3-20h, obtains the strong acid solution of hydrogen sulfide;
(2) strong acid solution that cadmium salt soln is dropwise joined to described hydrogen sulfide is in 20-30 DEG C of reaction 0.5-20 h, after filtration, water washing, filtration, drying treatment, obtains CdS powder;
(3) CdS powder is heat-treated under nitrogen protection, heat-treating methods is: 200 DEG C～250 DEG C thermal treatment 3 h～10 h, 300 DEG C～350 DEG C roasting 3 h～10 h, roasting 3 h～10 h at 400 DEG C～450 DEG C, roasting 3 h～10 h at 450 DEG C～500 DEG C; Then through grinding, acid elution, water washing, filtration, drying treatment, obtain CdS semiconductor light-catalyst.
In the present invention, strong acid used is any or the two kinds of mixing in sulfuric acid, phosphoric acid.S in the strong acid solution of hydrogen sulfide
2-ionic concn regulates to maintain constant by hydrogen ion concentration in strong acid.Described hydrogen sulfide and sour mass percent are (0.001～10): (0.001～90).The rotating speed stirring is 50-100 r/min.
Described cadmium salt soln is any one or more in anhydrous sodium Cadmium Sulphate, anhydrous cadmium bromide, anhydrous phosphoric acid cadmium, anhydrous sodium cadmium phosphate, anhydrous Hypophosporous Acid, 50 cadmium, anhydrous slufuric acid cadmium, anhydrous acetic acid cadmium, anhydrous cadmium oleate, anhydrous oxalic acid cadmium, crystallization cadmium sulfite, crystallization cadmium bromide, crystallization cadmium phosphate, crystallization phosphorous acid cadmium, crystallization Hypophosporous Acid, 50 cadmium, crystalline sulfuric acid cadmium, crystallization cadmium acetate, crystallization cadmium oleate, crystallization cadmium oxalate.The mass ratio of hydrogen sulfide and cadmium salt is (0.001～50): (0.001～90).
The application of a kind of CdS semiconductor light-catalyst making aspect organic pollutant degradation and water decomposition hydrogen manufacturing.
The principle of the invention is as follows: one, hydrogen sulfide in water, exist light current from, produce H
+, HS
-and S
2-ion, and the required ion of preparation CdS is S
2-ion, H
+and HS
-on its synthetic not impact.Under strong acid exists, strong acid can improve H in solution
+content, the ionization of hydrogen sulfide will be suppressed, and then, the S that hydrogen sulfide ionization produces
2-ionic weight will reduce.Therefore, can be by improving H in solution
+content is controlled S in solution
2-ion content.Its two, after cadmium acetate joins in the strong acid solution of hydrogen sulfide, Cd
2+and S
2-ion forms CdS need to meet certain condition, i.e. Cd
2+and S
2-ionic concn is seized the opportunity and is greater than 8 × 10
-27, just likely form CdS.Therefore, can be by controlling S
2-the rate of addition of ion content and cadmium acetate is controlled CdS grain diameter.Therefore, CdS semiconductor light-catalyst of the present invention, under visible ray, can effectively reduce CdS grain diameter, will have more excellent Photocatalytic activity.
In CdS semiconductor light-catalyst preparation process of the present invention, first, formulating vulcanization hydrogen strong acid solution and cadmium acetate solution then, slowly drip cadmium acetate solution in hydrogen sulfide strong acid solution, are conducive to reduce the particle diameter of CdS particle, increase the specific surface area of CdS powder; Finally; under nitrogen protection; adopt the baking modes of temperature programmed control; 200 DEG C of-300 DEG C of roasting 3～10 h; roasting 3～10 h at 300 DEG C～400 DEG C, roasting 3～10 h at 400 DEG C～480 DEG C, object is for improving CdS degree of crystallinity when; reduce the agglomeration of CdS, finally improve the Photocatalytic activity of CdS.
The method has improved the dispersion effect of CdS, has shortened the transmission distance between CdS particle, slows down the photoetch speed on CdS surface, not only can reduce the agglomeration of CdS, and has improved the photocatalytic activity of CdS.CdS semiconductor light-catalyst is applied in organic pollutant degradation aspect, has more excellent Photocatalytic activity.
Brief description of the drawings
Fig. 1 is the XRD figure of the photocatalyst prepared of embodiment 1.
Fig. 2 is the SEM figure of the photocatalyst prepared of embodiment 1.
Fig. 3 adopts photocatalyst catalyzed degradation graphic representation in embodiment 1.
Embodiment
Embodiment 1
Be that 1:110 mix with sulfuric acid according to mass ratio by hydrogen sulfide, at 25 DEG C of vigorous stirring 3 h, cadmium salt soln is the cadmium acetate aqueous solution; To slowly dripping 1% cadmium acetate solution in reactor, vigorous stirring 6 h, through ultrasonic dispersion, filtration, water washing, filtration, the treatment process such as dry, obtain CdS powder successively.
Described Cadmium Sulfide presoma is processed under nitrogen protection: at 200 DEG C of thermal treatment 3 h, roasting 3 h at 300 DEG C, roasting 3 h at 400 DEG C, roasting 3 h at 480 DEG C.After processing under nitrogen protection, cooling, through treatment process such as grinding, acid elution, water washing, filtration, dry and grindings, obtain CdS semiconductor light-catalyst successively.Through XRD test, CdS semiconductor light-catalyst of the present invention only contains CdS.Fig. 1 is the XRD figure of the CdS photocatalyst prepared of embodiment 1.Characterize explanation by SEM, CdS semiconductor light-catalyst of the present invention has less grain diameter.Fig. 2 is the SEM figure of the CdS photocatalyst prepared of embodiment 1.
Embodiment 2
Be that 1:100 mix with sulfuric acid according to mass ratio by hydrogen sulfide, at 26 DEG C of vigorous stirring 4 h, in reactor, slowly drip 0.9% cadmium acetate solution, vigorous stirring 7 h, through ultrasonic dispersion, filtration, water washing, filtration, the treatment process such as dry, obtain CdS powder successively.
Described Cadmium Sulfide presoma is processed under nitrogen protection: at 200 DEG C of thermal treatment 7 h, roasting 7 h at 300 DEG C, roasting 7 h at 400 DEG C, roasting 7 h at 480 DEG C.After processing under nitrogen protection, cooling, through treatment process such as grinding, acid elution, water washing, filtration, dry and grindings, obtain CdS semiconductor light-catalyst successively.Through XRD test, CdS semiconductor light-catalyst of the present invention only contains CdS.Characterize explanation by SEM, CdS semiconductor light-catalyst of the present invention has less grain diameter.
Embodiment 3
Be that 1:120 mix with sulfuric acid according to mass ratio by hydrogen sulfide, at 27 DEG C of vigorous stirring 5 h, in reactor, slowly drip 0.7% cadmium acetate solution, vigorous stirring 5 h, through ultrasonic dispersion, filtration, water washing, filtration, the treatment process such as dry, obtain CdS powder successively.
Described Cadmium Sulfide powder is processed under nitrogen protection: at 200 DEG C of thermal treatment 5 h, roasting 5 h at 300 DEG C, roasting 6 h at 400 DEG C, roasting 6 h at 480 DEG C.After processing under nitrogen protection, cooling, through treatment process such as grinding, acid elution, water washing, filtration, dry and grindings, obtain semiconductor light-catalyst successively.Through XRD test, CdS semiconductor light-catalyst of the present invention only contains CdS.Characterize explanation by SEM, CdS semiconductor light-catalyst of the present invention has less grain diameter.
Embodiment 4
Be that 1:130 mix with sulfuric acid according to mass ratio by hydrogen sulfide, at 23 DEG C of vigorous stirring 8 h, to slowly dripping 0.5% cadmium acetate solution in reactor, vigorous stirring 7 h, obtain CdS powder through ultrasonic dispersion, filtration, water washing, filtration, the processing such as dry successively.
Described Cadmium Sulfide powder is processed under nitrogen protection: at 200 DEG C of thermal treatment 6 h, roasting 6 h at 300 DEG C, roasting 6 h at 400 DEG C, roasting 6 h at 480 DEG C.After processing under nitrogen protection, cooling, through treatment process such as grinding, acid elution, water washing, filtration, dry and grindings, obtain CdS semiconductor light-catalyst successively.Through XRD test, CdS semiconductor light-catalyst of the present invention only contains CdS.Characterize explanation by SEM, CdS semiconductor light-catalyst of the present invention has less grain diameter.
Embodiment 5
Be that 1:200 mix with sulfuric acid according to mass ratio by hydrogen sulfide, at 29 DEG C of vigorous stirring 7 h, in reactor, slowly drip 0.3% cadmium acetate solution, vigorous stirring 5 h, through ultrasonic dispersion, filtration, water washing, filtration, the treatment process such as dry, obtain CdS powder successively.
Described Cadmium Sulfide powder is processed under nitrogen protection: at 200 DEG C of thermal treatment 5 h, roasting 5 h at 300 DEG C, roasting 5 h at 400 DEG C, roasting 5 h at 480 DEG C.After processing under nitrogen protection, cooling, through treatment process such as grinding, acid elution, water washing, filtration, dry and grindings, obtain CdS semiconductor light-catalyst successively.Through XRD test, CdS semiconductor light-catalyst of the present invention only contains CdS.Characterize explanation by SEM, CdS semiconductor light-catalyst of the present invention has less grain diameter.
Embodiment 6
Be that 1:300 mix with sulfuric acid according to mass ratio by hydrogen sulfide, at 26 DEG C of vigorous stirring 9 h, to slowly dripping 0.2% cadmium acetate solution in reactor, vigorous stirring 5 h, successively through ultrasonic dispersion, filter and the processing such as be dried and obtain CdS powder.
Described Cadmium Sulfide powder is processed under nitrogen protection: at 200 DEG C of thermal treatment 4 h, roasting 4 h at 300 DEG C, roasting 4 h at 400 DEG C, roasting 4 h at 480 DEG C.After processing under nitrogen protection, cooling, through treatment process such as grinding, acid elution, water washing, dry and grindings, obtain CdS semiconductor light-catalyst successively.Through XRD test, CdS semiconductor light-catalyst of the present invention only contains CdS.Characterize explanation by SEM, CdS semiconductor light-catalyst of the present invention has less grain diameter.
Application Example
Under 250 W xenon lamp cold light sources, respectively taking tropeolin-D as probe, the different CdS semiconductor light-catalysts that adopt embodiment 1-6 to prepare carry out Photocatalytic Degradation Property evaluation.In other conditions all under the same prerequisite, using the experiment that there is no illumination and do not add photocatalyst as blank assay, blank test shows there is no degradation effect respectively.
Fig. 3 is that in the embodiment of the present invention 1, CdS semiconductor light-catalyst carries out photocatalyst for degrading graphic representation, can find out that CdS semiconductor light-catalyst of the present invention has good Photocatalytic Degradation Property.In embodiment of the present invention 2-6, semiconductor light-catalyst also has catalytic performance trend in the same manner as in Example 1.
Claims (8)
1. a preparation method for CdS semiconductor light-catalyst, is characterized in that this preparation method is as follows:
(1) under 20-30 DEG C of condition, hydrogen sulfide and strong acid to be mixed, vigorous stirring, reacts 3-20h, obtains the strong acid solution of hydrogen sulfide;
(2) strong acid solution that cadmium salt soln is dropwise joined to described hydrogen sulfide is in 20-30 DEG C of reaction 0.5-20 h, after filtration, water washing, filtration, drying treatment, obtains CdS powder;
(3) CdS powder is heat-treated under nitrogen protection, heat-treating methods is: 200 DEG C～250 DEG C thermal treatment 3 h～10 h, 300 DEG C～350 DEG C roasting 3 h～10 h, roasting 3 h～10 h at 400 DEG C～450 DEG C, roasting 3 h～10 h at 450 DEG C～500 DEG C; Then product, through grinding, acid elution, water washing, filtration, drying treatment, obtains CdS semiconductor light-catalyst.
2. the preparation method of CdS semiconductor light-catalyst according to claim 1, is characterized in that: in step (1), strong acid used is any or the two kinds of mixing in sulfuric acid, phosphoric acid.
3. the preparation method of CdS semiconductor light-catalyst according to claim 1, is characterized in that: in step (1), and S in the strong acid solution of hydrogen sulfide
2-ionic concn regulates to maintain constant by hydrogen ion concentration in strong acid.
4. the preparation method of CdS semiconductor light-catalyst according to claim 1, is characterized in that: in step (1), the mass percent of described hydrogen sulfide and strong acid is (0.001～10): (0.001～90).
5. the preparation method of CdS semiconductor light-catalyst according to claim 1, is characterized in that: in step (1), the rotating speed of stirring is 50-100 r/min.
6. the preparation method of CdS semiconductor light-catalyst according to claim 1, it is characterized in that: in step (2), described cadmium salt soln is any one or more in anhydrous sodium Cadmium Sulphate, anhydrous cadmium bromide, anhydrous phosphoric acid cadmium, anhydrous sodium cadmium phosphate, anhydrous Hypophosporous Acid, 50 cadmium, anhydrous slufuric acid cadmium, anhydrous acetic acid cadmium, anhydrous cadmium oleate, anhydrous oxalic acid cadmium, crystallization cadmium sulfite, crystallization cadmium bromide, crystallization cadmium phosphate, crystallization phosphorous acid cadmium, crystallization Hypophosporous Acid, 50 cadmium, crystalline sulfuric acid cadmium, crystallization cadmium acetate, crystallization cadmium oleate, crystallization cadmium oxalate.
7. the preparation method of CdS semiconductor light-catalyst according to claim 1, is characterized in that: in step (2), the mass ratio of hydrogen sulfide and cadmium salt is (0.001～50): (0.001～90).
8. the application of the CdS semiconductor light-catalyst that a claim 1 makes aspect organic pollutant degradation and water decomposition hydrogen manufacturing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108067255A (en) * | 2017-12-11 | 2018-05-25 | 南京工业职业技术学院 | A kind of CdNiS2/CoFe2TiO6Photochemical catalyst and preparation method thereof |
| CN108745383A (en) * | 2018-07-10 | 2018-11-06 | 常州大学 | A kind of preparation method of composite sulfuration Mn catalyst |
| CN113019397A (en) * | 2021-03-16 | 2021-06-25 | 南京信息工程大学 | Preparation method of photocatalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100250A (en) * | 1985-04-01 | 1986-07-09 | 武汉大学 | A kind of novel method for preparing the pure Cadmium Sulfide of fluorescence |
| CN103570057A (en) * | 2013-11-14 | 2014-02-12 | 吉林大学 | Method for synthesizing cadmium sulfide nano material |
-
2014
- 2014-05-13 CN CN201410198686.XA patent/CN103950968A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100250A (en) * | 1985-04-01 | 1986-07-09 | 武汉大学 | A kind of novel method for preparing the pure Cadmium Sulfide of fluorescence |
| CN103570057A (en) * | 2013-11-14 | 2014-02-12 | 吉林大学 | Method for synthesizing cadmium sulfide nano material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108067255A (en) * | 2017-12-11 | 2018-05-25 | 南京工业职业技术学院 | A kind of CdNiS2/CoFe2TiO6Photochemical catalyst and preparation method thereof |
| CN108067255B (en) * | 2017-12-11 | 2020-08-07 | 南京工业职业技术学院 | CdNiS2/CoFe2TiO6Photocatalyst and preparation method thereof |
| CN108745383A (en) * | 2018-07-10 | 2018-11-06 | 常州大学 | A kind of preparation method of composite sulfuration Mn catalyst |
| CN113019397A (en) * | 2021-03-16 | 2021-06-25 | 南京信息工程大学 | Preparation method of photocatalyst |
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Application publication date: 20140730 |