Catalytic Wet Air Oxidation of an Aqueous Phenol Solution over Fe-Al Pillared Catalyst Was Conducted in a Stirred Tank and Packed Bed Reactor. Semi-Batch Experiments in the Stirred Tank Reactor Were Designed to Investigate the Effects of Temperature, Air Pressure, Initial Phenol Concentration, Catalyst Loading, and Catalyst Size on the Conversion of Total Organic Carbon. the Catalyst Exhibited an Important Activity in Degrading Total Organic Carbon at Mild Conditions. its Internal Mass Transfer Resistance Was Assessed over Different Catalyst Sizes Via a Chosen Criterion. Packed Bed Runs Were Conducted under Selected Temperature and Pressure (170 °C, 3.2 MPa) over a Long Duration (240 H). Various Characterization Methods Were Employed for Fresh and Aged Pillared Clay Catalysts. Occurrence of Catalyst Deactivation by Carbonaceous Deposits during the Packed Bed Operation Was Observed through Scanning Electron Microscopy (SEM) and Elemental Analysis. Insignificant Metal Leaching Was Observed Because Trace Amounts of Metal Elements Were Detected in the Hot Acidic Liquid Solution. © 2005 Elsevier B.V. All Rights Reserved.