The distillation process for one-step synthesis of methyl-isobutyl-ketone(MIBK) from acetone is analyzed.The existence of small amount water in the feed of MIBK light-ends column causes an unstable operation and further affects the total MIBK separation process.To solve this problem,a hybrid pervaporation/distillation process is put forward,in which the MIBK light-ends column can be eliminated.A small-scale pervaporation experiment with a zeolite NaA membrane which is prepared on the surface of α-Al2O3,is established to study the membrane separation properties.Aspen Plus software is used to simulate the hybrid pervaporation/distillation process.When the quality and recovery of MIBK product is the same,compared with the traditional distillation process,operating costs and total cost can reduce by 20% and 15%,respectively.