闫宇民,陈丽珍,王建龙. N-硝基吡唑合成过程中的热安全性[J]. 科学技术与工程, 2020, 20(30): 12403-12408.
YAN Yu-min,CHEN Li-zhen.Study on Thermal Safety in the Process of Synthesis Reaction of N-nitropyrazole[J].Science Technology and Engineering,2020,20(30):12403-12408. |
| N-硝基吡唑合成过程中的热安全性 |
| Study on Thermal Safety in the Process of Synthesis Reaction of N-nitropyrazole |
| 投稿时间：2019-10-19 修订日期：2020-08-04 |
| DOI： |
| 中文关键词: N-硝基吡唑 硝化反应 反应热 绝热分解 冷却失效 |
| 英文关键词:N-nitropyrazole nitration reaction heat adiabatic decomposition cooling failure |
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| 中文摘要: |
| 为解决N-硝基吡唑安全生产问题，利用反应量热仪EaysmaxHFCal测定N-硝基吡唑合成过程中的放热速率、传热系数、比热容等热力学数据，结果表明：加料过程中平均放热速率为6.72 W，保温过程中平均放热速率为0.11 W，理论绝热温升为111.19 ℃。采用绝热加速量热仪ARC测定硝化液的热稳定性，结果表明：硝化液绝热分解分为三个阶段，后两个阶段为其主要热分解阶段。主要的热分解在78.8 ℃开始，整体绝热分解过程较为缓慢。计算了第二段热分解过程的活化能及指前因子，分别为118.81 kJ·mol-1、6.94×1013 s-1。反应液到达最大反应速率用时24 h所对应的的温度TD24=48.11 ℃，通过冷却失效情形法，确定其危险度等级为2级，反应过程的热危险较低。 |
| 英文摘要: |
| In order to solve the safety production problem of n-nitropyrazole, EasymaxHFCal was used to measure the heat release rate, heat transfer coefficient, specific heat capacity and other thermodynamic data in the synthesis process of n-nitropyrazole. The result shows that the average heat release rate of nitration reaction in feeding is 6.72 W and in the finish period is 0.11 W. The theoretical adiabatic temperature rise is 111.19 ℃. The thermal decomposition behavior of the nitrate solution in the reaction process was studied by ARC. Based on the experiment rasult, the adiabatic decomposition can be divided into three stages and the last two stages are the main thermal decomposition. The adiabatic decomposition of n-nitropyrazole is slow with the initial decomposition temperature begin at 78.8 ℃. The activation energy and pre-exponential factor of thermal decomposition in the second stage were calculated, which are 118.81 kJ·mol-1, 6.94×1013 s-1, respectively. The temperature corresponding to the reaction of the reaction solution to reach the maximum thermal decomposition rate of 24 hours is TD24=48.11 ℃. The risk level is determined as level 2 by the cooling failure situation method. The thermal runway risk of this reaction is low. |
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