Glycerol
esterification with acetic acid was carried out in a continuous,
easy-to-scale-up system using toluene as the entrainer. A water separation
system was designed and coupled to an optimized continuous system.
The continuous system operated at a temperature of 100 °C, an
acetic acid-to-glycerol mole ratio of 7, a pressure of 1 bar, and
a feed flow rate of 0.5 mL min–1 over 3 g of Amberlyst
36. Under these conditions, the glycerol conversion was 100% with
43%, 44%, and 13% selectivities to monoacetin, diacetin, and triacetin,
respectively. Formation of byproducts was not observed under these
conditions. When this continuous system was coupled to the designed
simultaneous reactor and water separation system, containing 3 g of
Amberlyst 36, these values changed to 0%, 15%, and 80%, respectively.
Byproduct formation was observed with a selectivity of only 5% after
the feed was passed from the water separation system. Continuous removal
of the water formed in the reaction was done with toluene. As a result
of this process, the chemical equilibrium shifted toward the TA production.
The maximum selectivities obtained from experiments were 85% for MA,
and 65% for DA. Amberlyst 15 and Purolite PD206 also was used for
esterification reaction. Amberlyst 15 and Amberlyst 36 exhibited similar
performances. A mixture of MA and DA was obtained through esterification
of glycerol with trapped acetic acid in a Dean–Stark apparatus.