CN103723760B - A kind of cadmium sulfide photochemical catalyst and preparation method thereof - Google Patents

A kind of cadmium sulfide photochemical catalyst and preparation method thereof Download PDF

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CN103723760B
CN103723760B CN201410025527.XA CN201410025527A CN103723760B CN 103723760 B CN103723760 B CN 103723760B CN 201410025527 A CN201410025527 A CN 201410025527A CN 103723760 B CN103723760 B CN 103723760B
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photochemical catalyst
cadmium sulfide
preparation
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cadmium
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CN103723760A (en
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陈敏东
李园
楼孙棋
�田�浩
滕飞
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Nanjing University of Information Science and Technology
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Nanjing University of Information Science and Technology
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Abstract

The invention discloses a kind of Novel cadmium sulfide photocatalyst, this photochemical catalyst is made up of cadmium sulfide micron ball; Wherein, the sphere diameter size of cadmium sulfide micron ball is 5 ~ 15 μm, and its surface has aperture, and this aperture extends to centre of sphere place.The invention also discloses a kind of method adopting hydro-thermal method to prepare cadmium sulfide photochemical catalyst, this preparation method is simple, and controllability is strong, and the photochemical catalyst catalytic activity prepared is high.

Description

A kind of cadmium sulfide photochemical catalyst and preparation method thereof
Technical field
The present invention relates to a kind of photochemical catalyst, be specifically related to a kind of cadmium sulfide micron ball photochemical catalyst with hollow hole and preparation method thereof.
Background technology
In the past in centuries, catalyst has played important function in development of chemical industry.Photocatalysis technology has broad application prospects in the field such as environment and the energy and great social benefit.At present, the major obstacle limiting photocatalysis technology practical application is that the quantum efficiency of light is low, solar energy utilization ratio is low.Novel high-efficiency photocatalysis material research and development are current light-catalysed important research directions.
Cadmium sulfide is a kind of typical II-VI semiconductor, and Bohr radius is 2.4nm, and energy gap is 2.42eV.Cadmium sulfide nano material is along with the reduction of nano-scale and pattern change, and obvious change will occur its energy gap, shows the photoelectric properties more more excellent than bulk material.In view of the photoelectric properties (Xue-fengBai2010) of cadmium sulfide uniqueness, nearly ten years, be all subject to increasingly extensive attention at multiple subjects such as chemistry, physics, materialogy, biology and applied science.
Summary of the invention
The object of the invention is, in order to provide a kind of, there is new structure, cadmium sulfide photochemical catalyst that catalytic activity is high.
In order to achieve the above object, the invention provides a kind of Novel cadmium sulfide photocatalyst, photochemical catalyst is made up of cadmium sulfide micron ball; Wherein, the sphere diameter size of cadmium sulfide micron ball is 5 ~ 15 μm, and its surface has aperture, and this aperture extends to centre of sphere place.
Present invention also offers the preparation method of above-mentioned photochemical catalyst, comprise the following steps:
(1) get 40mL water, add 0.9mmol ~ 1.1mmol ethylenediamine tetra-acetic acid and 0.7mmol ~ 0.9mmol tetra-nitric hydrate cadmium under stirring, then add 0.9mmol ~ 1.1mmol thiocarbamide, fully stir and obtain mixed reaction solution;
(2) mixed reaction solution of preparation in step (1) is proceeded in autoclave, hydro-thermal reaction 35 ~ 37h at 175 ~ 185 DEG C;
(3) after having reacted, through centrifugal, be drying to obtain described photochemical catalyst.
Best preparation process is as follows:
(1) get 40mL water, under stirring, add 1.0mmol ethylenediamine tetra-acetic acid and 0.8mmol tetra-nitric hydrate cadmium, stir 1h; Add 1.0mmol thiocarbamide again, stir 30min, obtain mixed reaction solution;
(2) mixed reaction solution of preparation in step (1) is proceeded in autoclave, hydro-thermal reaction 36h at 180 DEG C;
(3) after having reacted, through centrifugal, be drying to obtain described photochemical catalyst.
The present invention has the following advantages compared to existing technology: the present invention adopts hydro-thermal method to prepare cadmium sulfide photochemical catalyst, and preparation method is simple, and controllability is strong, and the cadmium sulfide photochemical catalyst prepared is the micron ball of band hollow hole, and photocatalytic activity is high.
Accompanying drawing explanation
Fig. 1 is the SEM figure of photochemical catalyst of the present invention under 1500 multiplying powers;
Fig. 2 is the SEM figure of photochemical catalyst of the present invention under 1500 multiplying powers;
Fig. 3 is the SEM figure of photochemical catalyst of the present invention under 3500 multiplying powers;
Fig. 4 is photochemical catalyst of the present invention and common commercial TiO 2catalytic activity comparison diagram.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment one
Under room temperature, get the water of 40 milliliters, pour in beaker, add 0.7mmol tetra-nitric hydrate cadmium and 0.9mmol ethylenediamine tetra-acetic acid under agitation, abundant stir about 1 hour, then add 0.9mmol thiocarbamide, stir about 30 minutes, proceed in autoclave, hydro-thermal reaction 35h at 175 DEG C, centrifugal, be drying to obtain cadmium sulfide photochemical catalyst.
Embodiment two
Under room temperature, get the water of 40 milliliters, pour in beaker, add 0.9mmol tetra-nitric hydrate cadmium and 1.1mmol ethylenediamine tetra-acetic acid under agitation, abundant stir about 1 hour, then add 1.1mmol thiocarbamide, stir about 30 minutes, proceed in autoclave, hydro-thermal reaction 37h at 185 DEG C, centrifugal, be drying to obtain cadmium sulfide photochemical catalyst.
Embodiment three
Under room temperature, get the water of 40 milliliters, pour in beaker, add 0.8mmol tetra-nitric hydrate cadmium and 1.0mmol ethylenediamine tetra-acetic acid under agitation, abundant stir about 1 hour, then add 1.0mmol thiocarbamide, stir about 30 minutes, proceed in four polyvinyl fluoride liner autoclaves, hydro-thermal reaction 36h at 180 DEG C, centrifugal, be drying to obtain cadmium sulfide photochemical catalyst.
Observe under a scanning electron microscope, as shown in Figures 1 to 3, the photochemical catalyst that the present invention prepares is spherical, micron level, and with hollow hole.
Effect example
Photochemical catalyst cadmium sulfide prepared by the embodiment of the present invention three and common commercial TiO 2respectively as photocatalyst for degrading rhodamine B.Taking 0.05g sample respectively adds in 100mL rhodamine B solution (10mg/L), first lucifuge stirs 30min, then under full light, light-catalyzed reaction is carried out, 3mL reactant liquor is got every 5min, supernatant liquor is got after centrifugation, detect the change of rhodamine B characteristic absorption peak maximum 553nm place absorbance with spectrophotometer, weigh the change in concentration of rhodamine B in solution.Draw C/C 0curve over time, to characterize the catalytic activity of photochemical catalyst.Wherein C 0for the initial concentration of Luo Dan Ming B, C penetrates through full exposure the Luo Dan Ming B concentration value that certain hour t measurement obtains.According to testing result, we make active comparison diagram.
As can be seen from Figure 4, full exposure is penetrated down, and the photocatalytic activity of the cadmium sulfide micron ball of band hollow hole prepared by the present invention is far away higher than common commercial TiO 2, substantially increase the efficiency of degradation of organic substances.

Claims (2)

1. a cadmium sulfide photochemical catalyst, is characterized in that: described photochemical catalyst is made up of cadmium sulfide micron ball; The sphere diameter size of described cadmium sulfide micron ball is 5 ~ 15 μm; Described cadmium sulfide micron ball surface has aperture, and this aperture extends to centre of sphere place; Described photochemical catalyst is prepared by following steps: (1) gets 40mL water, 0.9mmol ~ 1.1mmol ethylenediamine tetra-acetic acid and 0.7mmol ~ 0.9mmol tetra-nitric hydrate cadmium is added under stirring, add 0.9mmol ~ 1.1mmol thiocarbamide again, fully stir and obtain mixed reaction solution; (2) mixed reaction solution of preparation in step (1) is proceeded in autoclave, hydro-thermal reaction 35 ~ 37h at 175 ~ 185 DEG C; (3) after having reacted, through centrifugal, be drying to obtain described photochemical catalyst.
2. photochemical catalyst according to claim 1, is characterized in that: described photochemical catalyst is prepared by following steps:
(1) get 40mL water, under stirring, add 1.0mmol ethylenediamine tetra-acetic acid and 0.8mmol tetra-nitric hydrate cadmium, stir 1h; Add 1.0mmol thiocarbamide again, stir 30min, obtain mixed reaction solution;
(2) mixed reaction solution of preparation in step (1) is proceeded in autoclave, hydro-thermal reaction 36h at 180 DEG C;
(3) after having reacted, through centrifugal, be drying to obtain described photochemical catalyst.
CN201410025527.XA 2014-01-21 2014-01-21 A kind of cadmium sulfide photochemical catalyst and preparation method thereof Expired - Fee Related CN103723760B (en)

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Publication number Priority date Publication date Assignee Title
CN105056974B (en) * 2015-08-03 2017-05-03 南京信息工程大学 Flower-shaped cadmium sulfide-antimony sulfide compound, preparation method and application thereof
CN105668611B (en) * 2016-01-08 2017-06-06 福州大学 A kind of spherical cadmium sulfide crystal and preparation method thereof
CN109364951B (en) * 2018-12-21 2022-09-30 苏州科技大学 Visible light catalytic composite material and preparation method and application thereof
CN110639556A (en) * 2019-10-17 2020-01-03 扬州大学 Composite photocatalyst and preparation process thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101618329A (en) * 2009-07-31 2010-01-06 黑龙江省科学院石油化学研究院 Preparation method of composite photocatalyst CdS/n-TiO2 for catalyzing and decomposing H2S to prepare hydrogen
CN101700905A (en) * 2009-10-30 2010-05-05 陕西科技大学 Preparation method of spherical cadmium sulfide nanocrystalline
CN101767021A (en) * 2009-12-17 2010-07-07 南京林业大学 Method for preparing p-CoO/n-CdS compound semiconductor photocatalyst

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101618329A (en) * 2009-07-31 2010-01-06 黑龙江省科学院石油化学研究院 Preparation method of composite photocatalyst CdS/n-TiO2 for catalyzing and decomposing H2S to prepare hydrogen
CN101700905A (en) * 2009-10-30 2010-05-05 陕西科技大学 Preparation method of spherical cadmium sulfide nanocrystalline
CN101767021A (en) * 2009-12-17 2010-07-07 南京林业大学 Method for preparing p-CoO/n-CdS compound semiconductor photocatalyst

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