Amino-functionalized MIL-101(Fe) metal-organic framework as a viable fluorescent probe for nitroaromatic compounds

Microchimica Acta - A highly luminescent iron(III)-based amino-functionalized metal-organic framework (MOF) of type NH2-MIL-101(Fe) was synthesized by a solvothermal method. Its structure and...     

Effect of Fenton-like oxidation on enhanced oxidative degradation of para-chlorobenzoic acid by ultrasonic irradiation

Sonolysis, Fenton-like oxidation (FeOOH-H2O2), and a combination of the two processes were used to facilitate the degradation of para-chlorobenzoic acid (a model compound for free radical mediated reactions). The objective of this study was to investigate the effect of FeOOH and H2O2 dosages on the degradation of para-chlorobenzoic acid (p-CBA) using ultrasound/FeOOH-H2O2. The oxidation rate of p-CBA was measured at various concentrations of H2O2 and FeOOH particles and pH conditions. pH's below the pKa of p-CBA (3.98), showed significantly better degradation of p-CBA than at higher values from 5 to 9. The rates of degradation of p-CBA by FeOOH-H2O2 were enhanced in the presence of ultrasound. The first-order rate constant, k for p-CBA degradation by ultrasound was 4.5 x 10(-3) min(-1), and in the presence of FeOOH-H2O2 this was found to be substantially faster (1.54 x 10(-2) min(-1)). The observed rate enhancements for the degradation of p-CBA can be attributed primarily to the continuous cleaning and chemical activation of the FeOOH surfaces by acoustic cavitation and the accelerated mass transport rates of reactants and products between the solution phase and the FeOOH surface. This new process provides a viable alternative to existing oxidation technologies.     

Surfactant Assisted Hydrothermal Synthesis of Superparamagnetic ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> Nanoparticles as an Efficient Visible-Light Photocatalyst for the Degradation of Organic Pollutant

Super paramagnetic ZnFe₂O₄ nanoparticles were prepared by a surfactant assisted (ethylamine) hydrothermal method along with heat treatment. The nanoparticles were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, high resolution scanning electron microscopy, Transmission electron microscopy, vibrating sample magnetometer and diffuse reflectance spectra technique. From the analyses, influence of calcination temperature on the structural, vibrational, morphological, magnetic and optical properties of ZnFe₂O₄ nanoparticles were investigated. The ZnFe₂O₄ nanoparticles with an average particle size of 17 nm showed high photocatalytic activity in the degradation of methylene blue (90 %). This work demonstrates that ZnFe₂O4 can be used as a potential monocomponent in visible-light photocatalysis for the degradation of organic pollutants. Furthermore, the products were super paramagnetic and could be conveniently separated within 15 min and recycled by using simple magnet, which is very beneficial for the degradation of organic pollutants.     

Preparation of TiO2 nano-particle photocatalysts by a multi-gelation method: the effect of pH change

TiO₂ photocatalysts were prepared by a multi-gelation method and the effect of the changes in the pH during the pH swing times, i.e., by a controlled pH swing, on the morphology of the TiO₂ particles was investigated. The photocatalytic properties of the TiO₂ catalysts prepared by controlled pH swing were compared with TiO₂ particles prepared without adjusting the pH during the swing times. The photocatalytic degradation reaction of these TiO₂ catalysts was investigated by comparing their effectiveness in 2-propanol oxidation. The experimental results showed that the TiO₂ photocatalysts prepared without adjusting the pH performed better in controlling the important parameters of the catalysts such as particle size, surface area, anatase/rutile phase ratio and pore size, as well as pore volume than the TiO₂ photocatalysts prepared by a controlled pH swing method. Deceased.     

Ultrasonic-assisted sol-gel method of preparation of TiO2 nano-particles: characterization, properties and 4-chlorophenol removal application

Nano-size TiO2 photocatalysts were prepared by sol-gel and ultrasonic-assisted sol-gel methods using two different sources of ultrasonicator, i.e., a bath type and tip type. The physicochemical characteristics of the catalysts were investigated by BET, XRD and TEM analyses and the photocatalytic properties of the TiO2 catalysts prepared by three different methods were compared. The intrinsic and extrinsic properties of TiO2, such as the particle size, surface area, pore-volume, pore-diameter, crystallinity as well as anatase, rutile and brookite phase ratios, could be controlled by the ultrasonic-assisted sol-gel method. During this preparation method, the effect of such important operating variables as the ultrasonic irradiation time, power density, the ultrasonic sources (bath-type and tip-type), magnetic stirring during synthesis, initial temperatures and size of the reactors are discussed here. It was found that each of the parameters played a significant role in controlling the properties of the TiO2 nano-particles. Among the three different methods, TiO2 photocatalysts prepared by ultrasonic (tip-US) assisted sol-gel possessed the smallest particle size, highest surface area and highest pore-volume than the catalysts prepared by the other two methods. 4-Chlorophenol was used as a pollutant to observe the photocatalytic degradation ability of the prepared photocatalysts and the TiO2 catalysts prepared by the bath-US ultrasonic-assisted sol-gel method were shown to be the most highly active. This is due to their high surface area and high pore-diameter. This study clearly demonstrates the importance and advantages of ultrasonication in the modification and improvement of the photocatalytic properties of mesoporous nano-size TiO2 particles.     

Facile synthesis of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/Cu<Subscript>2</Subscript>O nanocomposite and its visible light photocatalytic activity for the degradation of cationic dyes

Iron oxide-loaded Cu₂O photocatalysts were prepared by a facile hydrothermal method. The binary mixed metal oxide photocatalyst was characterized by XRD, FE-SEM, FTIR, UV–Vis-DRS, particle size and zeta potential measurements. XRD analysis showed that Fe₂O₃/Cu₂O catalysts were phase pure and highly crystalline in nature. FE-SEM images revealed the formation of nanospherical Fe₂O₃ over the Cu₂O surface during hydrothermal reaction. From UV–Vis diffuse reflectance spectroscopy studies, the optical band gap of the Fe₂O₃/Cu₂O photocatalyst was found to be slightly red-shifted to 1.85 eV, after loading of Fe₂O₃. The zeta potential analysis revealed that the surface of the Fe₂O₃/Cu₂O photocatalyst was negatively charged in neutral solution. The loading of n-type Fe₂O₃ on p-type Cu₂O augments the charge carrier separation at the interface, which was evident from the enhanced photodegradation of organic pollutants (Methylene blue and Rhodamine B dyes) under visible light irradiation.     

Sonochemical synthesis of graphene oxide supported Pt–Pd alloy nanocrystals as efficient electrocatalysts for methanol oxidation

Pt–Pd bimetallic nanoparticles supported on graphene oxide (GO) nanosheets were prepared by a sonochemical reduction method in the presence of polyethylene glycol as a stabilizing agent. The synthetic method allowed for a fine tuning of the particle composition without significant changes in their size and degree of aggregation. Detailed characterization of GO-supported Pt–Pd catalysts was carried out by transmission electron microscopy (TEM), AFM, XPS, and electrochemical techniques. Uniform deposition of Pt–Pd nanoparticles with an average diameter of 3 nm was achieved on graphene nanosheets using a novel dual-frequency sonication approach. GO-supported bimetallic catalyst showed significant electrocatalytic activity for methanol oxidation. The influence of different molar compositions of Pt and Pd (1:1, 2:1, and 3:1) on the methanol oxidation efficiency was also evaluated. Among the different Pt/Pd ratios, the 1:1 ratio material showed the lowest onset potential and generated the highest peak current density. The effect of catalyst loading on carbon paper (working electrode) was also studied. Increasing the catalyst loading beyond a certain amount lowered the catalytic activity due to the aggregation of metal particle-loaded GO nanosheets.     

Graphene oxide based Pt-TiO2 photocatalyst: ultrasound assisted synthesis, characterization and catalytic efficiency

An ultrasound-assisted method was used for synthesizing nanosized Pt-graphene oxide (GO)-TiO₂ photocatalyst. The Pt-GO-TiO₂ nanoparticles were characterized by diffused reflectance spectroscopy, X-ray diffraction, N₂ BET adsorption-desorption measurements, atomic force microscopy and transmission electron microscopy. The photocatalytic and sonophotocatalytic degradation of a commonly used anionic surfactant, dodecylbenzenesulfonate (DBS), in aqueous solution was carried out using Pt-GO-TiO₂ nanoparticles in order to evaluate the photocatalytic efficiency. For comparison purpose, sonolytic degradation of DBS was carried out. The Pt-GO-TiO₂ catalyst degraded DBS at a higher rate than P-25 (TiO₂), prepared TiO₂ or GO-TiO₂ photocatalysts. The mineralization of DBS was enhanced by a factor of 3 using Pt-GO-TiO₂ compared to the P-25 (TiO₂). In the presence of GO, an enhanced rate of DBS oxidation was observed and, when doped with platinum, mineralization of DBS was further enhanced. The Pt-GO-TiO₂ catalyst also showed a considerable amount of degradation of DBS under visible light irradiation. The initial solution pH had an effect on the rate of photocatalytic oxidation of DBS, whereas no such effect of initial pH was observed in the sonochemical or sonophotocatalytic oxidation of DBS. The intermediate products formed during the degradation of DBS were monitored using electrospray mass spectrometry. The ability of GO to serve as a solid support to anchor platinum particles on GO-TiO₂ is useful in developing new photocatalysts.