Chinese Journal of Chemical Engineering, Vol.28, No.1, 158-164, 2020
Solventless ketalization of glycerol to solketal with acetone over the ionic liquid [P(C4H9)(3)C14H29][TsO]
The ketalization of glycerol with acetone was conducted over an ionic liquid [P(C4H9)(3)C14H29][TsO] (ETPT) in a batch reactor. A scheme to obtain the purified product using TTPT as a homogeneous catalyst is proposed and a maximum solketal yield of 86% is achieved at acetone/glycerol molar ratio of 6/1, reaction time of 0.5 h, reaction temperature of 303 K, catalyst amount of 5 wt% of glycerol:1117 was recycled and reused for ten times without obvious losses in terms of quantity and activity. Furthermore, effects of various experimental parameters (stirring speed, catalyst loadings, temperature and reactant composition) on the reaction kinetics are investigated. In terms of kinetics modeling, K-gamma is fitted by reactant composition at the temperature range 298 K-323 K, which was a concise strategy that showed good precision in the kinetics fitting. The activation energy for this ketalization reaction was evaluated to be 282 kJ. mol(-1) In addition, the kinetics of the reaction at a temperature exceeding the boiling point of acetone were also studied. We believe that all the results are important for further development of a technology for the continuous synthesis of solketal. (C) 2019 The Chemical Industry and Engineering Society of China, and Chemical Industry Press Co., Ltd All rights reserved.