The effect of activated carbon fiber (ACF) on the ozonation of phenol in water in a fluid bed reactor was investigated. It was observed that this combined process could increase the yield of the oxidation process significantly for phenol and COD (chemical oxygen demand) removal, especially for the phenol removal. The efficiency of ozonation increased with an increase in the dose of ACF. Higher initial phenol concentration only caused a slight decrease of phenol and COD removal. The results of repeated use found that ozonation could efficiently regenerate ACF in situ in the reactor, which was considered easy to handle without the costly ex situ regeneration of the industrial treatment process. The Boehm titrations and FTIR studies indicate that the ozonation process in water call significantly change the composition of acidic surface oxygen-containing groups of ACF, leading to the increase of carboxylic, hydroxylic, and carbonylic groups and the slight decrease of the lactonic groups. Furthermore, this process call also increase the surface area and total pore volume of ACF. Due to the new micropore formation and some pore enlargement, the micropores became smaller, and the mesopores and macropores got bigger. (C) 2007 Elsevier Inc. All rights reserved.