The catalytic performance of transition metal (Fe2+ or Cu2+) containing nano-sized hollow core mesoporous shell carbon (HCMSC) heterogeneous catalysts for the hydroxylation of phenol with hydrogen peroxide (H2O2) in water was investigated in a batch reactor. The metal-containing HCMSC catalyst showed higher activity than the same metal ion-exchanged zeolites. The nature of the metal and its content in the HCMSC had remarkable influence on the reaction results under the typical reaction conditions (PhOH/H2O2=3, reaction temperature=60 oC). Fe2+ containing HCMSC catalyst showed high catalytic activity with phenol conversion of 29%, selectivity to catechol (CAT) and hydroquinone (HQ) about 85%, H2O2 effective conversion about 70% and selectivity to benzoquinone (BQ) below 1% in the batch system.