The catalytic wet peroxide oxidation (CWPO) of phenol from wastewater using Mg-Al LDH and calcined LDH at 500 º C was investigated. The LDH was synthesized by co-precipitation and was characterized by XRD, FTIR, SEM, EDS, and BET. XRD results indicated that during the calcination of LDH at 500 º C, LDH decomposed to the mixed oxide. The SEM images approved Mg-Al LDH comprised of flakes and the calcined LDH comprised of spherical nanoparticles. BET results indicated the specific surface area of 100. 2 and 86. 3 m2. g-1 for pure LDH and calcined LDH, respectively. The process was optimized by one factor at a time method and considering four process factors i. e. reaction temperature, peroxide dosage, initial phenol concentration, and reaction time. The optimum conditions resulted at initial phenol concentration of 100 ppm, reaction temperature of 60 º C, with peroxide volume of 3 mL and time on stream of 45 min over calcined LDH with maximum 85% removal of phenol. On the pure LDH, the maximum phenol removal (79%) resulted in a peroxide volume of 2. 5 mL at 55 min. The study concluded that the calcined Mg-Al LDH due to the synergistic effect of MgO and Mg-Al mixed oxide showed higher catalytic activity despite a relatively low surface area.