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Thermal hazard assessment for synthesis of 3-methylpyridine-N-oxide
Institution:1. Safety Engineering Institute, Nanjing Tech University, Nanjing 210009, Jiangsu, China;2. Jiangsu Key Laboratory of Dangerous Chemical Safety and Control, Nanjing 210009, Jiangsu, China;1. Japan National Institute of Occupational Safety and Health, 1-4-6 Umezono Kiyose, Tokyo 204-0024, Japan;2. Yamaishi Metal Co., LTD., 791 Kimagase, Noda, Chiba 270-0222, Japan;3. Technology Institution of Industrial Safety, 2-16-26 Hirosedai, Sayama-shi, Saitama 350-1328, Japan;1. Department of Mathematics and Informatics, Chiba University, 1-33 Yayoi-cho, Inage, Chiba, Japan;2. School of Information Science, Japan Advanced Institute of Science and Technology, Nomi 923-1292, Japan;1. Center for Surface Science and Nanotechnology, University Politehnica of Bucharest, 313 Splaiul Independentei, 060042 Bucharest, Romania;2. Department of Physics and Materials Science, City University of Hong Kong, 83 Tat Chee Ave, Kowloon, Hong Kong, China
Abstract:The exothermic oxidation of 3-methylpyridine with hydrogen peroxide was analyzed by Reaction Calorimeter (RC1e) in semi-batch operation. Heat releasing rate and heat conversion were studied at different operating conditions, such as reaction temperature, feeding rate, the amount of catalyst and so on. The thermal hazard assessment of the oxidation was derived from the calorimetric data, such as adiabatic temperature rise (ΔTad) and the maximum temperature of synthesis reaction (MTSR) in out of control conditions. Along with thermal decomposition of the product, the possibility of secondary decomposition under runaway conditions was analyzed by time to maximum rate (TMRad). Also, risk matrix was used to assess the risk of the reaction. Results indicated that with the increase of the reaction temperature, the reaction heat release rate increased, while reaction time and exotherm decreased. With the increase of feeding time, heat releasing rate decreased, but reaction time and exotherm increased. With the amount of the catalyst increased, heat releasing rate increased, reaction time decreased and exothermic heat increased. The risk matrix showed that when the reaction temperature was 70 °C, feeding time was 1 h, and the amount of catalyst was 10 g and 15 g, respectively, the reaction risk was high and must be reduced.
Keywords:3-Methylpyridine  Reaction Calorimeter (RC1e)  Semi-batch reaction  Thermal hazard
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