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- Synergistic catalytic action of vanadia-titania composites towards the microwave-assisted benzoin oxidationPublication . Ferretti, Francesco; Da Costa Ribeiro, Ana Paula; Alegria, Elisabete; Ferraria, Ana Maria; Kopylovich, Maximilian; Guedes Da Silva, M. Fátima C.; Marchetti, Fabio; Pombeiro, ArmandoIntensification of chemical processes according to the motto "faster, simpler, greener" is among the main concerns nowadays. One of the ways of intensification is the application of synergistic catalytic effects when the overall efficiency of a composite catalyst is much higher than the sum of the component activities. Here, we report on the preparation of synergistic catalytic materials by a simple and straightforward ball milling procedure. Oxidation of benzoin was selected as a model reaction to demonstrate the viability of the concept. For the V2O5-TiO2 (95 : 5) composite material, the synergistic effect is triggered by low power microwave irradiation with more than a tenfold jump in the catalytic activity in comparison to the activities of the individual components.
- Comparison of microwave and mechanochemical energy inputs in the catalytic oxidation of cyclohexanePublication . Da Costa Ribeiro, Ana Paula; Alegria, Elisabete; Kopylovich, Maximilian; Ferraria, Ana Maria; Rego, Ana; Pombeiro, ArmandoThe effect of microwave and mechanochemical ball milling energy inputs was studied for the peroxidative oxidation (with aqueous H2O2) of cyclohexane to cyclohexanol and cyclohexanone, over CoCl2 and/or V2O5 dispersed (μm scale) catalysts. A maximum total yield of cyclohexanol and cyclohexanone of 43% after 1 h of reaction at 30 °C, in acetonitrile and under microwave irradiation (5 W), was achieved over the CoCl2–V2O5 (3 : 1) catalyst prepared by ball milling. Cyclohexanol is the main final product with a selectivity of up to 93% over cyclohexanone. Conducting the oxidation reaction under microwave irradiation under the same conditions but without any mechanochemical treatment of the catalyst prior to use resulted in a lower total yield of 30% with a lower selectivity (69%) towards cyclohexanol over cyclohexanone. The sole application of mechanochemical treatment for the catalyst preparation and the catalytic oxidation of cyclohexane allowed to reach yields of 29% after 1 h of reaction, at room temperature, without microwave irradiation and any additive and in the absence of any organic solvent. Ball milling is shown to provide a convenient, solvent-free method to disperse these solid catalysts and to promote the above cyclohexane oxidation, although, in the latter case, not so effectively as microwave irradiation.