posted on 2018-06-06, 16:27authored byClaudia
E. Berdugo, Andrea Suaza, Miguel A. Santaella, Orlando A. Sánchez, Gerardo Rodríguez, Alvaro Orjuela
In
this work, diethyl citrate (DEC) was synthesized and isolated
for further physicochemical characterization and phase equilibria
study. The synthesis was performed via partial esterification of citric
acid with ethanol, and the final product was separated from the resulting
mixture using a pH-controlled solvent extraction method. Characterization
using 1H NMR and 13C NMR spectroscopy confirmed
the presence of both DEC isomers with few impurities. Results indicate
that a 6:5 molar ratio of the symmetric to the nonsymmetric ester
structures was attained during synthesis. Thermogravimetric analysis
and differential scanning calorimetry allowed us to measure, for the
first time, glass transition temperature (228 K) and decomposition
temperature (493 K) of diethyl citrate. Additionally, P–x data for the vapor–liquid equilibrium of the binary mixtures
diethyl citrate + ethanol and diethyl citrate + water were collected
at 308 K using an accurate dynamic device. Data were regressed to
generate binary interaction parameters for the UNIQUAC equation. The
regressed model shows good agreement with experiments, and it can
be used for further process design in the esterification of citric
acid.