- Nano Express
- Open Access
One-Pot Green Synthesis of Ag-Decorated SnO2 Microsphere: an Efficient and Reusable Catalyst for Reduction of 4-Nitrophenol
© The Author(s). 2017
- Received: 2 March 2017
- Accepted: 19 June 2017
- Published: 30 June 2017
In this paper, hierarchical Ag-decorated SnO2 microspheres were synthesized by a facile one-pot hydrothermal method. The resulting composites were characterized by XRD, SEM, TEM, XPS, BET, and FTIR analysis. The catalytic performances of the samples were evaluated with the reduction of 4-nitrophenol to 4-aminophenol by potassium borohydride (KBH4) as a model reaction. Time-dependent experiments indicated that the hierarchical microspheres assembled from SnO2 and Ag nanoparticles can be formed when the react time is less than 10 h. With the increase of hydrothermal time, SnO2 nanoparticles will self-assemble into SnO2 nanosheets and Ag nanoparticles decorated SnO2 nanosheets were obtained. When evaluated as catalyst, the obtained Ag-decorated SnO2 microsphere prepared for 36 h exhibited excellent catalytic performance with normalized rate constant (κ nor) of 6.20 min−1g−1L, which is much better than that of some previous reported catalysts. Moreover, this Ag-decorated SnO2 microsphere demonstrates good reusability after the first five cycles. In addition, we speculate the formation mechanism of the hierarchical Ag-decorated SnO2 microsphere and discussed the possible origin of the excellent catalytic activity.
- Ag-decorated SnO2
SnO2 is an important n-type semiconductor with large bandgap (Eg = 3.6 eV, at 300 K), high electron mobility, and low cost, which enable it with outstanding properties in gas sensing , lithium ion batteries , optoelectronic devices, and dye sensitized solar cells [3–8]. In the past two decades, the robust SnO2 material has garnered considerable attention and various nanostructures have been reported [9, 10]. Among which, three-dimensional (3D) hierarchical structures self-assembled by nanosheets building blocks are much more interesting due to their special structure and fascinating properties [11, 12]. Nevertheless, there are only a few reports on the catalytic performance of SnO2 and the catalytic efficiency is relatively low [13–15]. It is thus important to synthesize hierarchical SnO2 structures and study the catalytic performance. Especially, as we know, noble metal nanoparticles (NPs) such as Au-, Ag-, Pt-, and Pd-modified 3D hierarchical structures will show much enhanced catalytic performance . However, most of the processes of the syntheses of the above noble metal-modified oxides are more complicated multi-step process and usually toxic and harmful environmentally . So developing facile and efficient methods to fabricate noble metal NP-modified hierarchical SnO2 and studying the catalytic performance are highly desirable.
Increased contamination of our limited water resources owing to the widespread dispersion of various industrial dyes, heavy metal ions, and other aromatic pollutants are endangering our planet . The 4-nitrophenol (4-NP), a well-known toxic pollutant, is widely present in industrial effluents and agriculture wastewater . Among various treatment techniques, such as membrane filtration , photo degradation , adsorption , and chemical reduction [23–30], the chemical reduction of 4-NP to 4-aminophenol (4-AP) is a favorable route, owing to the product (4-AP) which is an important intermediate for the manufacture of analgesic and antipyretic drugs, photographic developer, corrosion inhibitor, anticorrosion lubricant, and hair-dyeing agent [31, 32]. Hence, the reduction of 4-NP to 4-AP possesses great significance for the pollution abatement and resource regeneration .
In this paper, we reported a green synthesis of noble metal Ag nanoparticle (NP)-modified SnO2 hierarchical architectures by a simple one-pot hydrothermal route without the assistant of any templates and surfactants at mild temperature. The effects of reaction time on morphologies of Ag-decorated SnO2 microsphere were investigated, and a possible growth mechanism of Ag-decorated SnO2 hierarchical structures was proposed. The catalytic results indicate the as-synthesized products exhibit excellent catalytic performance for the reduction of 4-NP to 4-AP, with normalized rate constant (κ nor) of 6.20 min−1g−1L. In addition, the Ag-decorated SnO2 hierarchical structures sustain high catalytic efficiency in ten cycles and show stability after the first five cycles. This obtained Ag-decorated SnO2 hierarchical structures may have potential applications of water contaminant treatment, and this simple one-step hydrothermal route could be extended to design other noble metal NP-modified composite with a wide range of practical applications for the future.
Silver nitrate (AgNO3, 99.8%), urea (CO(NH2)2, 99%), ammonia solution (NH3·H2O, 25~28%), and potassium borohydride (KBH4, 97%) were purchased from Sinopharm Chemical Reagent Co. Ltd. Sodium stannate rehydrate (Na2SnO3·3H2O, 98%) and 4-nitrophenol(C6H5NO3, 98%) were supplied by Aladdin Reagent Co. Ltd. All the materials were used without further purification.
Synthesis of Ag-Decorated SnO2 Microsphere
Ag-decorated SnO2 powder (mole ratio of Ag:SnO2 = 1:1) was synthesized by one-pot hydrothermal method. In a typical procedure, 2.67 g of sodium stannate rehydrates and 0.2 g of urea were dissolved in 25 mL of ultra-pure water and stirred vigorously for 30 min to form a mixture. Then, 1.69 g of silver nitrate was dispersed in 25 mL of ultra-pure water, and then, 2.4 mL ammonium hydroxide was added into the silver nitrate solution to form silver–ammonia solution. After stirring for 5 min, the freshly prepared silver–ammonia solution was added into the mixture under magnetic stirring for 1 h. Subsequently, the resulting mixture was migrated into a 50-mL Teflon-lined autoclave and heated at 150 °C for 5, 10, 24, and 36 h. After the hydrothermal procedure, the autoclave was cooled down naturally to room temperature and the SnO2/Ag product was collected by centrifugation, followed by rinsing with deionized water and ethanol and drying in a vacuum oven at 60 °C. SnO2/Ag microsphere with different mole ratios (1.5:1, 1:1, 0.5:1, 0.01:1) of Ag to SnO2 are synthesized in a similar way except for the amounts of AgNO3 and NH3·H2O. For comparison, pure SnO2 and Ag were also synthesized by the similar procedure without the addition of AgNO3 and Na2SnO3.
The crystalline phase of the as-prepared samples were investigated by X-ray powder diffraction (XRD, Cu Kα radiation (λ = 1.5418 Å)). The scanning electron microscopy (SEM) measurements were performed on a SU-70 field emission SEM microscope with an acceleration voltage of 20 kV. Transmission electron micrograph (TEM) and high-resolution transmission electron microscopy (HRTEM) were taken on a Tecnai G2 F20 S-TWIN transmission electron microscope with an accelerating voltage of 200 kV. X-ray photo-electron spectroscopy (XPS) was performed to identify surface chemical composition and chemical states of the catalysts on a MARK II X-ray photoelectron spectrometer using Mg Kα radiation. The specific surface area of sample was evaluated by the Langmuir model and Brunauer–Emmett–Teller (BET) model based on the nitrogen adsorption isotherm obtained with a V-sorb X2008 series, while the pore size distribution was estimated by Barrett–Joyner–Halenda (BJH) theory.
Catalytic Activity of Ag-Decorated SnO2 Microsphere
The reduction of 4-NP with KBH4 solution was used as a model reaction to study the catalytic activity of Ag-decorated SnO2 composites. The catalytic reduction process was carried out in a standard quartz cell with a 1-cm path length and about 4 mL volume with 0.3 mL of freshly prepared aqueous solutions of 4-NP (20 mg/L) and KBH4 (1.5 mg). The high molar ratio of KBH4 to 4-NP ensured an excess amount of the former, and hence, its concentration remained essentially constant during the reduction reaction. Upon the addition of KBH4 into the 4-NP solution, its color changed immediately from light yellow to dark yellow due to the formation of 4-nitrophenolate ion (formed from the high alkalinity of KBH4). Later, the dark yellow color faded with time (due to the conversion of 4-NP to 4-AP) after the addition of 1.5 mg of Ag-decorated SnO2 hybrids. The UV–Vis absorption spectra were recorded by an UV–Vis spectrometer in a scanning range of 250–500 nm at room temperature at time interval of 1 min. Several consecutive reaction rounds were measured to determine the stability of the catalyst.
Characterization of Ag-Decorated SnO2 Microsphere
Catalytic Reduction of 4-NP
The apparent rate constants κ app of different cycles for all samples
κ app (min−1)
Also, the FTIR spectra of the catalyst before and after five cycles and ten cycles of catalytic reduction were shown in ESI. As shown in Additional file 1: Figure S7, after five and ten cycles of catalytic reduction, the main peaks of the samples were almost the same with the as-prepared sample and this illustrates that the catalysts are very stable.
Comparison of normalized rate (κ nor) of different catalysts for the reduction of 4-NP (at room temperature)
κ app (min−1)
κ nor (min−1g−1L)
J Mol Catal A-Chem
Appl. Catal. B: Environ
Phys. Chem. Chem. Phys
J Mol Catal A-Chem
J. Phys. Chem. C
Catal Sci Technol
J Alloy Compd
SnO2/Ag (36 h)—1st
SnO2/Ag (36 h)—5th
SnO2/Ag (36 h)—10th
In conclusion, hierarchal Ag-decorated SnO2 microsphere with uniform Ag nanoparticles and SnO2 nanosheets has been successfully prepared by a facile one-pot method. The catalysts prepared by this simple but effective method exhibit excellent catalytic performance for the reduction of 4-NP to 4-AP with κ nor of 6.20 min−1g−1L. Furthermore, the catalyst can sustain high catalytic performance after the first five cycles and could be expected to act as high-efficiency catalysts for the reduction of 4-NP. Moreover, we believe this method can be used as a new strategy to prepare other metal particle-modified semiconductor composites.
This work was financially supported by the NSF of China (nos. 51502155, 51572152, and 21373122), the Research Project of Hubei Provincial Department of Education (no. D20151203), and the NSF of Hubei Province of China (nos. 2011CDA118 and D20151203).
HM and LCK fabricated the samples. ZZW carried out the structural and catalytic characterization. QXQ analyzed the data. All authors read and approved the final manuscript.
The authors declare that they have no competing interests.
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