The objective of this study is to prepare a pelletized adsorbent to remove volatile organic compounds (VOC) from the municipal solid waste incinerator (MSWI) fly ash in Korea. The fly ash sample was sieved to particle size of 75-150㎛, and then a hydrothermal processing was carried out. The pelletized adsorbent was prepared from hydrothermal treated fly ash by mixing it with coal tar pitch and K2CO3 as a carbon source and activating agent, and activating them. The optimum condition to derive maximum iodine adsorptivity and BET surface area was the mixing ratio of hydrothermal treated fly ash, coal tar pitch and K2CO3 of 40/40/20 wt.% at the activation temperature of 800°C. Under this condition, the iodine adsorptivity and BET surface area for prepared adsorbent were 455 mg/g and 325 m2/g, respectively.