Abstract: Cyclohexanone glycol ketal was synthesis from cyclohexanone and ethylene glycol in the presence of a late-model catalyst, which was prepared with fly ash as raw material. The catalysts were characterized by means of XRD, TG and FTIR. Various reaction parameters, such as the molar ratio of cyclohexanone to ethylene glycol, amount of catalyst, reaction time, water-carrying reagent and other factors influencing the synthesis were discussed and the optimum conditions was established. The results showed that molar ratio of cyclohexanone to ethylene glycol was 1∶1.4, the amount of catalyst was 2% cyclohexanone, amount of cyclohexane was 10 mL, the reaction time 2 h, the yield of cyclohexanone ethylene ketal reached 99.6% under the optimum condition. The catalyst had a higher activity with respect to condensation reaction and can be used repeatedly.