In this work, an iron-rich residue, which is widely obtained as a by-product in the iron mining industry, and macauba endocarp, waste from the extraction of vegetable oil for the production of biofuels, were used in the preparation of different composites based on iron and carbon. The composites were obtained by manual grinding of the calcined iron residue and activated carbon prepared by the macauba endocarp followed by thermal treatment under nitrogen atmosphere. The effect of the thermal treatment was analyzed by Mössbauer spectroscopy and X-ray diffraction and showed that the increase in the treatment temperature promoted the formation of different reduced iron phases in the final composite, such as Fe3O4, FeO, and Fe0. These composites were used in a combined adsorption/oxidation process through photocatalysis to remove up to 93% of amoxicillin from aqueous phase. The formation of possible reaction intermediates was monitored by electrospray ionization mass spectrometry (ESI-MS) and a mechanism of amoxicillin degradation was proposed. Afterward, the Fe/C composites were conducted to evaluate the impact of several parameters on phosphate adsorption processes and showed a maximum adsorption capacity of 40.3mgg-1. The adsorption capacity obtained for all the materials were greater than those found in the literature.