Green syntheses of levulinate esters using ionic liquid 1-Methyl imidazolium hydrogen sulphate [MIM][HSO4] in solvent free system

Add time:08/20/2019    Source:sciencedirect.com

In the present work, n-butyl levulinate is synthesized by esterification of levulinic acid (LA) with n-butanol using Brønsted acidic ionic liquid [MIM][HSO4] as a catalyst in a solvent free condition. The prepared IL was characterized by FT-IR, 13C‐NMR and 1H–NMR. For optimization study, central composite design (CCD) method was employed. Design of experiments and statistical analysis is performed using Design Expert 11 software. The highest yield 89.6% and selectivity 98.1% of n-butyl levulinate were achieved at 90 °C. Biphasic layers of product and IL were observed resulting in self-separation of product. Effects of changes in variable parameters on conversion like LA: n-butanol molar ratio, LA:IL molar ratio and temperature were studied. Arrhenius plot was obtained and Activation energy (Ea) was calculated as 53.16 KJ/mol. Substrate study was performed on sec-, iso-, and tert-butanol and 1-Pentanol and n-Hexanol giving high yield and selectivity of corresponding levulinate esters. Catalyst was reused five times without significant decrease in yield.

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