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为研究中间体C,N-二甲基-C-(3-吡啶基)硝酮合成的热风险性,采用绝热加速量热仪(ARC)研究硝酮合成反应原料及产物的热分解情况,再通过反应量热仪(RC1)分析试验,得到硝酮合成反应动力学方程。结果表明,N-甲羟胺硫酸盐的分解温度为378.15 K,硝酮的分解温度为373.15 K,分解过程有气体放出。合成反应为放热反应,反应放热量Δr H m为-46.17 kJ/mol,绝热温升ΔT ad为27.10 K。热失控条件下,体系最高反应温度(MTSR)为336.60 K,低于体系沸点和N-甲羟胺硫酸盐和硝酮分解温度,合成工艺热危险性较小。合成反应对主要中间体3-乙酰基吡啶的反应级数为0.62。
In order to study the thermal risk of the synthesis of intermediate C, N-dimethyl-C- (3-pyridyl) nitrone, the thermal decomposition of nitrone synthesis reaction raw materials and products was studied by adiabatic accelerated calorimeter (ARC) Then through the reaction calorimeter (RC1) analysis of the experiment, the nitrone reaction kinetics equation. The results showed that the decomposition temperature of N-hydroxylamine sulfate was 378.15 K, the decomposition temperature of nitrone was 373.15 K, and gas was released during decomposition. The synthesis reaction was an exothermic reaction, the reaction exotherm Δr H m was -46.17 kJ / mol and the adiabatic temperature increase ΔT ad was 27.10 K. Thermal runaway conditions, the system maximum reaction temperature (MTSR) of 336.60 K, lower than the system boiling point and N-hydroxylamine sulfate and nitrone decomposition temperature, synthesis of thermal risk less. The reaction order of the synthesis reaction to the main intermediate 3-acetylpyridine was 0.62.