Using EMT zeolite grains as seeds, NaY membranes were synthesized by secondary hydrothermal reaction method. The effect of alkalinity and the amount of Al in the secondary growth sol on the microstructure of the membranes was investigated. The effect of the concentration of the feed mixture and the pervaporation temperature on the separation performance was investigate when the membranes were applied to separate MeOH/DMC mixture. The stability of the membrane was also investigated. The results show that, when the molar ratio of n(SiO2)/n(Na2O) = 1/1.4 and n(SiO2)/n(Al2O3)=10in the secondary growth sol, the membrane was of the highest quality in all the membranes we prepared. The separation performance was effected by the composition of feed mixture and pervaporation temperature. At 50℃, with the increase of feed mixture concentration(20%~80%),the separation factor decreased from 34.1to 5.2,the flux increased from 114.7to 135.5g/(m2·h));with the increase of pervaporation temperature(20~80 ℃),for the feed mixture with 50% methanol, the separation factor decreased from 29.8to 2.8and the flux increased from 96.3to 180.8g/(m2·h).The membrane was stable. Within 14 h pervaporation period, no change on the separation factor and flux was observed