(172h) Reaction Calorimetry as Means for Process Intensification of the Epoxidation of Methyl Oleate

Summary Reaction calorimetry proved a powerful tool for the solvent-free epoxidation of technical grade methyl oleate with in situ generated peracetic acid [1]. The results obtained from the calorimetric studies could be successfully transferred to 25 L scale. STY could be increased without a change in selectivity and yield. Results In a heat flow reaction calorimeter the isothermal solvent-free epoxidation of methyl oleate (technical grade, 70%) was performed [2]. This reaction is investigated within the CRC 442 (Environmentally friendly tribosystems by coatings and fluids from renewable sources) to optimise the synthesis of the biodegradable lubricant HISM from renewable sources and to characterise the lubricant in terms of lubrication behaviour, toxicity and biodegradability [3], [4]. In our studies conversion and selectivity of the products as well as the kinetics of the reaction were systematically investigated as function of reaction temperature as well as stirring speed. We found out that the reaction is strongly dependent on temperature and stirring speed. The reaction time could be decreased from 18h at 60°C (state of the art of the production at our institute) to 4h at 80°C. Selectivity and conversion were comparable. The results from the calorimetric studies could be succesfully transferred to a 25 L scale pilot plant. The obtained results and the yielded product were comparable to the 1 L scale calorimeter. Thus the productivity of the pilot plant could be increased 4 fold. Results of the calorimetric measurements of the epoxidation of methyl oleate as well as of the process intensification for the pilot plant will be presented. References [1] Swern, D.; Billen, G. N.; Findley, T. W.; Scanlan, J. T. J. Am. Chem. Soc. 1947,67, 1787. [2] Zogg, A.; Stoessel, F.; Fischer, U.; Hungerbuehler, K. Thermochimica Acta 2004,419, 1-17. [3] www.sfb442.rwth-aachen.de [4] Wagner, H.; Luther, R.; Mang, T. Appl. Cat. A 2001, 221, 429-442.