CN103265062A - Method for preparing flower-shaped copper oxide nanometer photocatalyst - Google Patents
Method for preparing flower-shaped copper oxide nanometer photocatalyst Download PDFInfo
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- CN103265062A CN103265062A CN2013102250346A CN201310225034A CN103265062A CN 103265062 A CN103265062 A CN 103265062A CN 2013102250346 A CN2013102250346 A CN 2013102250346A CN 201310225034 A CN201310225034 A CN 201310225034A CN 103265062 A CN103265062 A CN 103265062A
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Abstract
The invention provides method for preparing a flower-shaped copper oxide nanometer photocatalyst. By adopting the method, the homogeneity of flower-shaped copper oxide is well controlled; the particle size of the obtained product crystal is about 10 microns; the method is simple and feasible, and suitable for industrial production. The method for preparing the copper oxide concretely comprises the following steps of adding copper sulfate to water under an agitation condition, so as to form 0.01-0.5 mol/L copper sulfate solution; adding 0.1-1 mol/l sodium hydroxide solution, finally adding urotropine, stirring for 3 minutes; carrying out hydrothermal reaction at 80 DEG C for 10 hours, centrifugally separating, centrifugally washing for three times by using deionized water, and drying at 60 DEG C to obtain the flower-shaped copper oxide nanometer photocatalyst, wherein the molar ratio of the copper sulfate to the sodium hydroxide to the urotropine is (0.02-1):1:(1-10).
Description
Technical field:
The present invention relates to a kind of new catalyst, be specially a kind of preparation method of flower-shaped cupric oxide nano photocatalyst, belong to the photocatalysis technology field.
Background technology:
Human society and sustainable economic development face energy shortage and environmental degradation two large problems day by day, are in the China in urbanization and industrialization accelerated development stage, and are particularly urgent to the research and development demand of clean energy and environmental protection technology.In theory, obtain from nature and can utilize solar energy and low-cost to produce hydrogen energy source be the desirable approach that addresses the above problem, development correlation technique and novel material have bright prospects (Zhang Tong, 2009, instrumental technique and sensor).
As broad-spectrum multifunctional inorganic material, p-type narrow-band semiconductor material, nano cupric oxide have unique electricity, magnetic, catalysis characteristics, in fields such as gas sensing, magnetic phase transformation, superconduction and catalysis purposes are widely arranged.Cupric oxide has been widely used in the production of elements such as gas sensor, solar cell, magnetic memory device.The nano cupric oxide particle diameter is between 1～100nm, owing to have surface effects, quantum size effect, volume effect and macro quanta tunnel effect etc., compare with common cupric oxide, show peculiar physical and chemical performance at aspects such as magnetic, thermal resistance, photoabsorption, chemically reactive, catalyzer and fusing points, become one of broad-spectrum inorganic materials.Because nano cupric oxide shows more excellent performance in actual applications, the more excellent and easy preparation method who therefore studies and find out the nanostructure cupric oxide is significant.
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Summary of the invention:
The invention provides a kind of preparation method of flower-shaped cupric oxide nano photocatalyst, this method is controlled flower-shaped cupric oxide homogeneity preferably, obtain the product crystal particle diameter about 10um, and this method is simple, is suitable for suitability for industrialized production.
Concrete technical scheme of the present invention is as follows:
A kind of preparation method of flower-shaped cupric oxide nano photocatalyst is characterized in that: the concrete steps of the method for the preparation of this cupric oxide are as follows:
Copper sulfate is added to the water under agitation condition, forms copper sulfate 0.01 ~ 0.5mol/L solution; Add 0.1 ~ 1 mol/l sodium hydroxide solution again, add urotropine at last, stirred 3 minutes; 180 ℃ of hydro-thermals are after 10 hours, and deionized water centrifuge washing 3 times are used in centrifugation, and 60 ℃ of oven dry namely; Copper sulfate wherein: sodium hydroxide: the mol ratio of urotropine consumption is (0.02-1): 1:(1-10).
The preparation method of the flower-shaped cupric oxide nano photocatalyst of the present invention height homogeneity is for to add copper sulfate at the aqueous solution under agitation condition, sodium hydroxide, urotropine.The material that adds the growth of control catalyzer is urotropine.
The present invention has following beneficial effect compared to existing technology:
The preparation method of the flower-shaped cupric oxide nano photocatalyst of height homogeneity of the present invention, simple, in the aqueous solution, under agitation condition, add copper sulfate successively, sodium hydroxide and urotropine get final product.
Making method of the present invention is simple, and is with low cost, circulation ratio, and good stability is conducive to large-scale popularization.Compare with existing domestic and foreign literature, method is simple and easy, the photocatalyst crystals pattern that makes by single crystal to the growth of a plurality of directions form flower-shaped, height homogeneous (image of scanning electronic microscope), favorable reproducibility, and crystal stability is good.
Description of drawings
Fig. 1 is the image of scanning electronic microscope of the flower-shaped cupric oxide nano photocatalyst of embodiment one preparation.
Fig. 2 is the XRD figure picture of the flower-shaped cupric oxide nano photocatalyst of embodiment one preparation.
Fig. 3 is the image of scanning electronic microscope of the flower-shaped cupric oxide nano photocatalyst of embodiment two preparation.
Fig. 4 is the XRD figure picture of the flower-shaped cupric oxide nano photocatalyst of embodiment two preparations.
Fig. 5 is the image of scanning electronic microscope of the flower-shaped cupric oxide nano photocatalyst of embodiment three preparation.
Fig. 6 is the XRD figure picture of the flower-shaped cupric oxide nano photocatalyst of embodiment three preparations.
Fig. 7 is the rhodamine B degraded figure of the flower-shaped cupric oxide nano photocatalyst of embodiment one preparation.
Embodiment
The step of the flower-shaped cupric oxide of preparation of the present invention is as follows:
Copper sulfate is added to the water under agitation condition, forms copper sulfate 0.01 ~ 0.5mol/L solution; Add 0.1 ~ 1 mol/l sodium hydroxide solution again, add urotropine at last, stirred 3 minutes; 180 ℃ of hydro-thermals are after 10 hours, and deionized water centrifuge washing 3 times are used in centrifugation, and the cupric oxide powder that obtains black is ground in 60 ℃ of oven dry.
In above-mentioned reaction process, copper sulfate: sodium hydroxide: the mol ratio of urotropine consumption is (0.02-1): 1:(1-10).
Below be several embodiments of the present invention, further specify the present invention, but the present invention is not limited only to this.
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Embodiment one:
In this example, copper sulfate: sodium hydroxide: the mol ratio of urotropine consumption is 0.65:1:6.5.
6.5mmol copper sulfate solid is dissolved in the 20ml deionized water, stir after 10 minutes, the sodium hydroxide solution 20mL that adds 0.5mol/L, the urotropine that adds 65mmol at last stirred 3 minutes, and 180 ℃ of hydro-thermals are after 10 hours, centrifugation, with deionized water wash 3 times, 60 ℃ of oven dry get final product, and obtain flower-shaped cupric oxide nano photocatalyst of the present invention.
Fig. 1 has showed the scanning electron microscope diagram of the flower-shaped cupric oxide photocatalyst of embodiment one preparation, can find that from figure the cupric oxide for preparing is that homogeneous is flower-shaped.Fig. 2 has showed X-ray diffraction (XRD) figure of flower-shaped cupric oxide of the present invention, can find that from figure the cupric oxide for preparing is pure phase.
Embodiment two:
In this example, copper sulfate: sodium hydroxide: the mol ratio of urotropine consumption is 0.02:1:1.
0.2mmol copper sulfate solid is dissolved in the 20ml deionized water, stir after 10 minutes, the sodium hydroxide solution 20mL that adds 0.5mol/L, the urotropine that adds 10mmol at last stirred 3 minutes, and 180 ℃ of hydro-thermals are after 10 hours, centrifugation, with deionized water wash 3 times, 60 ℃ of oven dry get final product, and obtain flower-shaped cupric oxide nano photocatalyst of the present invention.
Fig. 3 has showed the scanning electron microscope diagram of the flower-shaped cupric oxide photocatalyst of embodiment two preparations, can find that from figure the cupric oxide for preparing is that homogeneous is flower-shaped.Fig. 4 has showed X-ray diffraction (XRD) figure, can find that from figure the cupric oxide for preparing is pure phase.
Embodiment three:
In this example, copper sulfate: sodium hydroxide: the mol ratio of urotropine consumption is 1:1:10.
10mmol copper sulfate solid is dissolved in the 20ml deionized water, stir after 10 minutes, the sodium hydroxide solution 20mL that adds 0.5mol/L, the urotropine that adds 100mmol at last stirred 3 minutes, and 180 ℃ of hydro-thermals are after 10 hours, centrifugal, with deionized water wash 3 times, 60 ℃ of oven dry get final product, and obtain flower-shaped cupric oxide nano photocatalyst of the present invention.
Fig. 5 has showed the scanning electron microscope diagram of the flower-shaped cupric oxide photocatalyst of embodiment three preparations, can find that from figure the cupric oxide for preparing is that homogeneous is flower-shaped.Fig. 6 has showed X-ray diffraction (XRD) figure, can find that from figure the cupric oxide for preparing is pure phase.
Effect example one:
The flower-shaped cupric oxide powder that embodiment one is obtained is used as the catalyst degradation rhodamine B.
The flower-shaped cupric oxide powder sample that takes by weighing among the 100mg embodiment one adds 200mL rhodamine B (RhB) solution (10-50mg/L), and lucifuge stirs 10 min, makes rhodamine B (RhB) solution reach absorption/desorption balance at catalyst surface.Open light source then and carry out light-catalyzed reaction, get the 5mL reaction solution every 10-20 min, after centrifugation, supernatant liquor detects with spectrophotometer (specturumlab 722sp).
Determine rhodamine B in the degradation process (RhB) change in concentration according to flower-shaped cupric oxide powder sample at 550 nm place absorbances.That the present invention adopts is 300W(CEL-HXB F300) xenon lamp, use spectral filter to be visible light (400 ~ 800nm) to guarantee incident light.
The degraded situation of rhodamine B (RhB) as shown in Figure 7, the figure shows the curve of C/C0 with respect to the time, to characterize the catalytic activity of catalyzer, wherein C0 is the starting point concentration of Luo Dan Ming B, the Luo Dan Ming B concentration value of C for measuring after for some time through UV-irradiation, t is that Luo Dan Ming B concentration drops to the used time of certain concentration.From the figure as can be seen: when not adding catalyzer, rhodamine B (curve a), and when flower-shaped copper oxide catalyst is arranged, the rhodamine B obvious degradation (curve b) of not degrading substantially.Therefore flower-shaped cupric oxide has photocatalysis performance efficiently.
Claims (1)
1. the preparation method of a flower-shaped cupric oxide nano photocatalyst, it is characterized in that: the concrete steps of the method for the preparation of this cupric oxide are as follows:
Copper sulfate is added to the water under agitation condition, forms copper sulfate 0.01 ~ 0.5mol/L solution; Add 0.1 ~ 1 mol/l sodium hydroxide solution again, add urotropine at last, stirred 3 minutes; 180 ℃ of hydro-thermals are after 10 hours, and deionized water centrifuge washing 3 times are used in centrifugation, and 60 ℃ of oven dry namely; Copper sulfate wherein: sodium hydroxide: the mol ratio of urotropine consumption is (0.02-1): 1:(1-10).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663539A (en) * | 2013-12-09 | 2014-03-26 | 上海应用技术学院 | CuO nanometer sheet and preparation method thereof |
| CN111517358A (en) * | 2020-06-16 | 2020-08-11 | 盐城工学院 | Synthetic method and application of flower-shaped copper oxide nanospheres |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462762A (en) * | 2009-01-16 | 2009-06-24 | 哈尔滨工程大学 | Method for inducing self-assembled shuttle-shaped nano cupric oxide |
| CN102502770A (en) * | 2011-10-21 | 2012-06-20 | 中国科学院过程工程研究所 | Flower-like copper oxide catalyst and preparation method and application thereof |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462762A (en) * | 2009-01-16 | 2009-06-24 | 哈尔滨工程大学 | Method for inducing self-assembled shuttle-shaped nano cupric oxide |
| CN102502770A (en) * | 2011-10-21 | 2012-06-20 | 中国科学院过程工程研究所 | Flower-like copper oxide catalyst and preparation method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| F. TENG ET AL.: ""Synthesis of flower-like CuO nanostructures as a sensitive sensor for catalysis"", 《SENSORS AND ACTUATORS B》 * |
| F. TENG ET AL.: ""Synthesis of flower-like CuO nanostructures as a sensitive sensor for catalysis"", 《SENSORS AND ACTUATORS B》, vol. 134, no. 2, 25 June 2008 (2008-06-25), pages 761 - 768, XP025429968, DOI: doi:10.1016/j.snb.2008.06.023 * |
| 张红霞: ""铜、锌氧化物的形貌控制合成及性能研究"", 《中国博士学位论文全文数据库 信息科技辑》 * |
| 杨慧等: ""花状氧化铜纳米结构的制备及其性能研究"", 《陕西师范大学学报（自然科学版）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663539A (en) * | 2013-12-09 | 2014-03-26 | 上海应用技术学院 | CuO nanometer sheet and preparation method thereof |
| CN111517358A (en) * | 2020-06-16 | 2020-08-11 | 盐城工学院 | Synthetic method and application of flower-shaped copper oxide nanospheres |
| CN111517358B (en) * | 2020-06-16 | 2021-11-02 | 盐城工学院 | Synthetic method and application of flower-shaped copper oxide nanospheres |
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Application publication date: 20130828 |