Supercritical carbon dioxide was used as a benign and environmentally friendly solvent for both synthesis and separation of glycerol acetates. Therefore, at the first step, the effect of important variables on the esterification reaction such as pressure (65-300) bar, temperature (100-150) °C, molar ratio of acetic acid to glycerol (1.5-40), solvent and substrates flow rates, reactor geometry and catalyst reusability have been investigated using Amberlyst 15 ® as a solid acidic catalyst. Moreover, the esterification reaction was studied over three catalysts of silica sulfuric acid, zeolite H-ZSM-5(x), and methyl imidazolium hydrogen sulfate as an ionic liquid at the optimized variables of the above reaction. The feasibility of partially selective extraction of triacetin from a mixture of triacetin, diacetin, and monoacetin with a molar ratio of 1:2:1 using a semi-continuous setup. At the best conditions of 109 bar, 56 °C, 0.86 mL·min -1 , and 61 min) the percent extraction was about 62.6% triacetin accompanied by only 16.8% diacetin and no monoacetin detected. Then a continuous fractionation setup equipped with a glass-bead packed column kept under a thermal gradient of 56 to70 °C was carried out based on the results of continuous recovery of triacetin from the acetins mixture with acetic acid.
