In this study, we studied to find the most suitable condition for the preparation of adsorbent by hydrothermal treatment of fly ash from the municipal solid waste incinerator (MSWI). There are many variables that affect the adsorptive characteristics in our study. With the variation of which discussed the effect such as the concentration of NaOH, reaction temperature, reaction time, solid/liquid ratio, and so on. The phase of adsorbent, its morphology and cation exchange capacity (CEC) were analyzed to evaluate their effects. The phase of adsorbent after treatment was identified by X-ray diffraction (XRD), the morphology was examined by scanning electron microscopy (SEM), and the CEC was analyzed by the ammonium acetate method. The maximum CEC value was obtained under the condition of 3N NaOH, 100°C of reaction temperature, 12 hr of reaction time, and 1:10 of solid/liquid ratio. The CEC was 68 meq/100g in this condition, which was 8 times the amount of raw fly ash.