This work presents a continuous,
easy-to-scale-up esterification
system with 100% conversion of glycerol in acetic acid with a high
selectivity to DA and TA and no byproducts under industrially applicable
reaction conditions. The main emphasis is to obtain TA from glycerol
esterification in acetic acid without using any acetic anhydride or
harsh conditions. The effects of reaction parameters, including the
acetic acid-to-glycerol mole ratio (1–9), temperature (66–134
°C), and pressure (1–199 bar) with a 0.5 mL·min–1 feed flow rate, on the glycerol conversion and selectivities
to monoacetin, diacetin, triacetin, and byproducts were investigated.
Under the optimum conditions of an acetic acid-to-glycerol mole ratio
of 7, a temperature of 100 °C, and a pressure of 1 bar, over
3 g of Amberlyst 36, the glycerol conversion and monoacetin, diacetin,
and triacetin selectivities reached 100%, 43%, 44%, and 13%, respectively.
The formation of byproducts was not detected under these optimum conditions.
Amberlyst 36 remained stable after 25 h on-stream. The recovered catalyst
was reused with no significant deactivation after three cycles. This
continuous system also can be used for monoacetin synthesis with 85%
selectivity and 95% glycerol conversion with an acetic acid-to-glycerol
mole ratio of 1, a temperature of 100 °C, and a pressure of 100
bar.
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