Chloranil was prepared by quinol hydrogen peroxide with hydrochloric acid using hydrochloric acid and acetic acid (2∶3,v/v) as a solvent, programmed heat up, and intermittently adding hydrogen peroxide. Chloranil was synthesized by chloridization in situ, reaction was proceed on three phase according to reactive temperature 45、70、95 ℃. The yield and purity of chloranil reached over 97%. It provided a new measure for preparing chloranil.