Continuous synthesis of glycerol acetates in supercritical carbon dioxide using Amberlyst 15?

Green Chemistry Pub Date: 2009-02-18 DOI: 10.1039/B815674C

Abstract

Continuous esterification of glycerol with acetic acid was investigated in supercritical carbon dioxide (scCO2) using Amberlyst 15? as a heterogeneous catalyst. The effect of pressure at (65–300) bar on the substrate conversion and the reaction yield and selectivity was studied. With increasing pressure, the percent of total yield and conversion remain almost unaffected and the selectivity of monoacetin synthesis increases while the selectivity for triacetin stays relatively unchanged. The effect of temperature on the yield, conversion, and the selectivity at (100–150) °C was also investigated. With increasing temperature from 100 to 140 °C, the selectivity for monoacetin decreases while for tri- and diacetin slightly increases. In contrast, with further increase in temperature, from 140 °C to 150 °C, the selectivity of monoacetin synthesis increases while that of diacetin decreases. By increasing the molar ratio of acetic acid to glycerol to 24, a selectivity of 100% was achieved for 2 h while the yield was 41% for the continuous triacetin synthesis in scCO2. When neat scCO2 as solvent with no catalyst was used, only monoacetin with 29% conversion was synthesized. The catalyst durability was also studied by monitoring the reaction for 25 h. The results show that the catalyst retains its activity even for 25 h but the selectivity for triacetin synthesis declines from 100% to about 60%.

Graphical abstract: Continuous synthesis of glycerol acetates in supercritical carbon dioxide using Amberlyst 15?
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