Biomass valorization strategies, including the preparation of materials and the synthesis of high-added value chemicals from platform molecules have been explored within this work. Biomass wastes were employed for the synthesis of carbonaceous samples, which were further used for the deposition of iron oxide nanoparticles. The incorporation of such entities in 1, 5 and 10 wt.% was carried out through mechanochemical procedures, avoiding the use of solvents and additional reagents. The catalysts were fully characterized by XRD, XPS and TEM analyses. Moreover, the catalytic performance of the samples was investigated in the oxidation of vanillyl alcohol into vanillin, either using by conventional methods or microwave-assisted protocols. Remarkably, after 30 min of reaction under microwave irradiation, conversion values of ca. 70% were achieved for the catalyst modified with 10% of iron oxide.