a b s t r a c tThe simultaneous synthesis of butyric acid methyl ester, the shortest component of the FAME (fatty acid methyl esters) family, and glycerol triacetate (TAG) from glycerol tributyrate (tributyrin) and methyl acetate was studied as a function of several reaction parameters, such as type of catalyst, temperature and products distribution. The reaction is an interesterification, a multistep consecutive ester interchange catalyzed by either acid or base catalyst. Under optimized conditions, a complete tributyrin conversion and an almost quantitative butyric acid methyl ester accumulation were achieved. The other reaction product, TAG, formed by the complete acetylation of the glycerol moiety, reached almost 70% yield, whereas the mono-and di-acetylated intermediates accumulated in the order of 5-8% and 24-27%, respectively. Similar final conversions and products yields were obtained with either acid or base homogeneous catalysts, suggesting that the final products mixture did not depend on the type of catalysis but might be limited by equilibrium conditions. In spite of similar final yields, base catalysis needed shorter reaction times (minutes instead of hours) and lower temperature (60 • C instead of 130 • C) with respect to the best acid catalyst. On the other hand, unlike heterogeneous basic catalysts, which showed low activity, a heterogeneous acid catalyst almost as active as the homogenous counterpart was found.
In this work, hierarchical Au/TiO 2 nanostructures were studied as possible photoanodes for water splitting and bisphenol A (BPA) oxidation. TiO 2 samples were synthetized by Pulsed Laser Deposition (PLD), while Au nanoparticles (NPs) were differently dispersed (i.e., NPs at the bottom or at the top of the TiO 2 , as well as integrated TiO 2 /Au-NPs assemblies). Voltammetric scans and electrochemical impedance spectroscopy analysis were used to correlate the morphology of samples with their electrochemical properties; the working mechanism was investigated in the dark and in the presence of a light radiation, under neutral pH conditions towards the possible oxidation of both bisphenol A (BPA) and water molecules. Different behavior of the samples was observed, which may be attributed mainly to the distributions of Au NPs and to their dimension as well. In particular, the presence of NPs at the bottom seems to be the crucial point for the working mechanism of the structure, thanks to scattering effects that likely allow to better exploit the radiation.
The Design of Experiment (DoE) technique has been used to investigate the photo-electrochemical removal of diuron (DRN) from wastewater. The process is carried out in a photo-electrochemical flow reactor, in which titania nanotubular electrode is irradiated with a simulated solar light. Different operative conditions have been investigated, in a planned 23 full factorial design in which imposed current density, flow rate and initial concentration have been varied at two levels. The removal process of DRN was investigated in terms of specific removal rate (K) and cell voltage (E), which were assumed as objective functions: the results show that the applied current has a paramount effect on both of the objective functions. From the analyses of the intermediates, it appears that the investigated parameters may exert different effects on the distribution of the reaction products: the initial concentration of diuron and the electrode potential seem to play a more important role, in this case.
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