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Straightforward Synthesis of Multifunctional core-shell composites and their applications

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Ultrasound and radiation-induced catalytic oxidation of 1-phenylethanol to acetophenone with iron-containing particulate catalysts
Publication . Soliman, Mohamed Mostafa Aboelhassan; Kopylovich, Maximilian N.; Alegria, Elisabete; Da Costa Ribeiro, Ana Paula; Ferraria, Ana Maria; Rego, Ana; Correia, Luís M. M.; Saraiva, Marta S.; Pombeiro, Armando
Iron-containingparticulatecatalystsof0.1–1 µmsizewerepreparedbywetandball-milling procedures from common salts and characterized by FTIR, TGA, UV-Vis, PXRD, FEG-SEM, and XPS analyses. It was found that when the wet method was used, semi-spherical magnetic nanoparticles were formed, whereas the mechanochemical method resulted in the formation of nonmagnetic microscale needles and rectangles. Catalytic activity of the prepared materials in the oxidation of 1-phenylethanol to acetophenone was assessed under conventional heating, microwave (MW) irradiation, ultrasound (US), and oscillating magnetic field of high frequency (induction heating). In general, the catalysts obtained by wet methods exhibit lower activities, whereas the materials prepared by ball milling afford better acetophenone yields (up to 83%). A significant increase in yield (up to 4 times) was observed under the induction heating if compared to conventional heating. The study demonstrated that MW, US irradiations, and induction heating may have great potential as alternative ways to activate the catalytic system for alcohol oxidation. The possibility of the synthesized material to be magnetically recoverable has been also verified.
Vanadium(V) complexes supported on porous MIL-100(Fe) as catalysts for the selective oxidation of toluene
Publication . Sutradhar, Manas; Marques, Guilherme; Soliman, Mohamed M. A.; Guedes Da Silva, M. Fátima C.; Flores, Daniela S. S.; Granadeiro, Carlos; Balula, Salete; Pombeiro, Armando; Alegria, Elisabete
The vanadium(V) complexes bearing the aroylhydrazone Schiff base 2-hydroxy-N'-((2-hydroxynaphthalen-1-yl) methylene)benzohydrazide ligand [VO(OMe)L] (1) and [Et3NH][VO2L] (2) were synthesized, characterized and supported on porous MIL-100(Fe) forming the 1@MIL-100(Fe) and 2@MIL-100(Fe) composites. The outcome of such immobilizations was assessed by several characterization techniques, namely powder X-ray diffraction, UV/ Vis, FTIR, SEM-EDS, ICP and BET surface area analysis, confirming the successful heterogenization of both va-nadium complexes. They were screened as catalysts towards the oxidation of toluene, under homogenous (1 and 2) and heterogeneous (1@MIL-100 and 2@MIL-100) conditions. The influence of several parameters, namely the type and amount of catalyst or oxidant, reaction time, temperature, and radical trapping, was studied. The main products obtained were benzaldehyde, benzyl alcohol and benzoic acid. Under the optimized conditions, using 1 and 2 as homogeneous catalysts, total yields of 19 and 23%, respectively, were achieved at 80 degrees C after 6 h. Using 1@MIL100(Fe) and 2@MIL100(Fe) composites under heterogeneous conditions, total yields up to 11% after 24 h, were achieved.

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Funding agency

Fundação para a Ciência e a Tecnologia

Funding programme

3599-PPCDT

Funding Award Number

PTDC/QUI-QIN/29778/2017

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