A continuous and selective method for monoacetin synthesis was developed. Effects of the process parameters including reaction temperatures (100–140 °C), acetic acid to glycerol mol ratios (1–3), feed flow rates (0.2–0.6 mL min−1), and pressures (1–160 bar) on the glycerol conversion and the monoacetin selectivity were studied. At the optimum conditions of 100 °C, acetic acid to glycerol mol ratio of 1, feed flow rate of 0.6 mL min−1, and 1 bar, the glycerol conversion and monoacetin selectivity was, respectively, 53% and 93%. The effect of water amount in the feed (3–15%)was also studied at the optimum conditions.