Abstract

In this work, acidic niobia-silica (NbS, 4–14 wt % Nb) materials used as supports of dispersed Pd particles (1.0–2.0 wt % Pd) have been prepared from different Nb-precursors (niobium ethoxide, NBE, and ammonium niobium oxalate, ANBO) and techniques (coprecipitation and deposition), characterized, and tested in the direct synthesis of H2O2 in water and methanol solvents. In particular, on a typical NbS sample, the evolution of morphology (by N2-adsorption–desorption), crystalline-phase (by XRD), electronic structure (by UV–vis-DRS), and surface acidity with time/temperature of treatment (350–800 °C for 4–100 h) has been investigated. Surface acidity was measured by titrations with 2-phenylethylamine adsorption in various liquids: cyclohexane, for the intrinsic acidity, and water, methanol, and water–methanol mixtures for the effective acidities. Direct H2O2 synthesis reaction was performed in semibatch slurry reactor with continuous feeding of the gaseous mixture (H2, O2, and N2), under pressure (5 × 103 k...

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