Acetin (triacetin and diacetin or monoacetin)were prepared using ethyl acetate and glycerol as raw material, cation exchange resin(NKC-9) as catalyst and with 4A zeolites as dealcohol adsorbent. The optimum reaction conditions were identified, which are n(ethyl acetate)/n( glycerol)=6.0:1; catalyst dosage 10.0% (refer to total mass of ethyl acetate and glycerol); reaction temperature78℃-85℃; reaction time 4.0 h. Content of (triacetin and diacetin or monoacetin) by the process with the analysis of SreactionSliquid by GC-MScould achieve 6.48%,54.18%,25.16%.