2-Methylpyridine-N-oxidation runaway studies

Calorimetry has been used in order to identify the runaway behavior of 2-methylpyridine-N-oxidation (2-picoline-N-oxidation). Experiments were performed in an Automatic Pressure Tracking Adiabatic Calorimeter (APTAC), employing 2-methylpyridine-N-oxide (2-picoline-N-oxide) with or without catalyst, 2-methylpyridine-N-oxide, hydrogen peroxide, 2-methylpyridine (2-picoline) and catalyst, and 2-methylpyridine, hydrogen peroxide and catalyst. Approximately 16.5 g of aqueous solutions were used in 100 ml closed glass cells in all but one measurement. Measurements were performed isothermally or employing the Heat-Wait-Search (HWS) technique. During reaction runaway, any excess of hydrogen peroxide and the produced 2-methylpyridine-N-oxide decompose releasing non-condensable gases and raising the pressure. It was found that the reaction runaway is condition-sensitive. Catalyst, the presence of 2-picoline and/or its N-oxide, affect hydrogen peroxide and/or 2-picoline-N-oxide decomposition rates. Further research accompanied by analytical measurements of the gas and liquid phase would provide indications in regard to the decomposition mechanisms followed in those cases.