Pre-press article
Parametric Study of Reaction Parameter for Glycerol Acetylation and Reusability of Sulfated-Titania Catalyst
https://doi.org/10.47836/pjst.34.4.04KeywordsAcetins, acetylation, glycerol, parametric study, solid acid catalyst, sulfated-titania, triacetin
Article content
Abstract
A parametric study of the reaction parameter for glycerol acetylation was conducted using a highly active sulfated-titania catalyst to determine the ideal conditions for achieving higher TA selectivity and glycerol conversion (GLC). The catalyst was prepared by impregnating titania with a 15% sulfuric acid solution, followed by calcination under CO2 for 2 hours and denoted as the 15SA catalyst. The catalyst was subsequently analysed using TGA, XRD, BET, XPS, NH3-TPD, and SEM-EDX. The characterisation results revealed that the 15SA catalyst possesses a sufficient surface area (1.9 m2g-1), a high density of acidic sites (342.6 μmolg−1) and good porosity. The study then examined the effects of several reaction parameters, including temperature (100 °C – 140 °C), molar ratio of glycerol (Gly) to acetic acid (Ac) (1:3 w/v – 1:15 w/v), catalyst loading (0.1 g – 0.9 g) and reaction time (1 h – 5 h). The catalyst was then reused for five successive cycles to evaluate its reusability. The results demonstrated that a higher density of acidic sites, sufficient BET surface area and pore volume of the catalyst may enhance the formation of GLC and TA in the glycerol acetylation by facilitating the diffusion of the glycerol molecules on the catalyst’s surface. Therefore, optimal conditions for glycerol acetylation yielded a higher TA selectivity of 55 % and glycerol conversion of 97 % at a molar ratio of 1:6 w/v of Gly: Ac and a catalyst loading of 0.5 g at 130 °C for a 2 h reaction time. The reusability study showed that the 15SA catalyst can attain a higher GLC exceeding 97 % and a higher DA+TA selectivity of 85 % after five cycles. In contrast, the selectivity of TA reduced after five cycles due to the leaching of the acidic site from the catalyst, as proven by the EDX analysis.
