Polysaccharides extracted from natural sources can be used as starting material for the preparation of nanoparticle supported composites. A novel family of bio-nanocomposites was mechanochemically synthesized by using niobium oxide and enzymatically produced polysaccharides. The structural, textural and surface properties of nanomaterials, were determined by X-Ray diffraction (XRD), nitrogen adsorption-desorption (N_2 porosimetry), pulse chromatography, infrared spectroscopy (ATR-IR) and dynamic light scattering (DLS). Selective oxidation of isoeugenol to vanillin was carried out to demonstrate the catalytic activity of the Nb-polysaccharides nanocomposites. Interestingly, most of our material showed high conversion of isoeugenol (60-70%) with selectivity to vanillin over 40%. The optimum conversion and selectivity were achieved with a reaction time between 8 and 24 h.Catalysts 2019, 9, 38 2 of 12 activity and selectivity of the catalysts [3,[6][7][8]. Heterogeneous catalysis can therefore be considered a key and priority activity for a Sustainable Chemistry [9].On the other hand, nanotechnology has generated a great scientific interest since allows discovering a multitude of new materials. But also evaluating already known materials from a new point of view. This is the case of metallic nanoparticles. They have been known since antiquity and from which, as early as 1857, Faraday [10] performed a first systematic study, based on the synthesis and properties of colloidal suspensions in catalysis [11]. However, it has been in recent years that most progress has been made in this regard.Nanoparticles (NP) have been studied in recent years due to their high activity, interaction specificity and interesting properties compared to metals (high surface/volume ratio combined with their small sizes) [12][13][14]. The specific properties of NP are directly related to their morphology and size, the dispersion of the metal or metal oxide on the support, the metal loading and the electronic properties of the NP in the material. In addition, NP have the additional advantage of their recyclability and reuse. These are essential and desired properties in many applications of these nanomaterials in catalysis [12,15], sensors [15,16] and even in the field of medicine [12]. There are several methods for the preparation of NP. Some of them include conventional physic-chemical methodologies of impregnation/reduction and coprecipitation [13,15,17], precipitation/deposition [13,15,17,18]. Nowadays more innovating methods have appeared such as photochemical deposition [13,15,17], ultrasonic deposition [13,15,17,18], use of laser treatment [13,15,17], supercritical fluids [13,15,17,19], plasma [13,15,17] or microwave irradiation [13,15,17,20,21].The mechanochemistry is a novel procedure for the production of NP. It consists on the melting, deformation and fracture of a mixture of reactants, normally solid, in a repetitive way during grinding. This reaction takes place at the interface of nanosized particles, those which are being continu...