Fly ash, a coal combustion residue produced by Termotasajero in Colombia, has been hydrothermally treated after an alkaline fusion to produce zeolite without addition of silicon or aluminum. The starting material was thoroughly mixed with NaOH, in a 1:1.2 mass ratio, to obtain a homogeneous mixture that was heated to 100 °C during different times (6, 8, and 10 h) and three zeolite samples were produced. The samples were characterized by XRD, SEM, XRF, Mössbauer spectroscopy, and N₂ physisorption. According to characterization results (high surface area and appropriate morphological properties including crystallinity) and synthesis time, zeolitic catalyst synthesized with 8 h of hydrothermal treatment was selected to perform further analysis. This sample consisted of a mixture of zeolite X and zeolite A of high surface area (301 m² g^-1) and a Fe content of 6% wt/wt. The zeolite was used as a catalyst for the Fenton oxidation of Orange II. Experiments were performed in a laboratory batch reactor at 70 °C and constant pH = 3, using different concentrations of H₂O₂. When the stoichiometric amount of H₂O₂ was used, good mineralization (X_TOC = 45%), complete discoloration, and oxidant consumption were obtained after 240 min of reaction. The sample retained activity after 16 h of usage. The presence of Fe in the reaction media was always detected and a homogeneous Fenton mechanism induced by surface-leached iron is suggested.