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摘要异辛醇与硝硫混酸反应生产硝酸异辛酯（EHN）的过程为强放热过程，伴随着较大的反应热危险性。在化工生产中一旦发生热失控，反应釜内温度、压力急剧上升，最终导致很严重的安全生产事故。国内曾发生过两起异辛醇硝化工艺的安全事故，故有必要分析异辛醇硝化工艺的热危险性。
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本毕业论文首先通过全自动反应量热仪（RC1e）测试了该工艺在不同温度、加料速率、搅拌速率下的热力学数据，并计算出MTSR、ΔTad等参数。然后通过差示扫描量热仪（DSC）和加速度量热仪（ARC）研究了EHN的分解特性，并算出诱导期为24h所对应的温度TD24。利用高效液相色谱对反应产物进行浓度分析，得到EHN的产率，并用来修正相关热力学参数。最后结合MTSR、ΔTad、TD24等相关数据，利用失控情景分析法对该工艺危险性进行评估。结果表明：该工艺在低温条件下，热失控危险等级为2级。而在25℃、30℃时，反应体系发生二次分解反应，危险等级为5级。20259
关键词：硝酸异辛酯（EHN），硝化反应，反应量热仪（RC1e），加速度量热仪（ARC），差示扫描量热仪（DSC），热失控危险等级。
毕业设计说明书（论文）外文摘要
Title Thermal hazard research on nitration of
iso-octyl alcohol
Abstract
It is a strong exothermic process of producing 2-Ethylhexyl nitrate (EHN) by dosing iso-octyl alcohol into nitric acid-sulfuric acid mixture. And this reaction is of great thermal hazard. The temperature and pressure in the reactor would increase sharply if thermal runaway happens during the reaction, and it may result in serious consequence finally. There have been two accidents related to this reaction in our country, so it is necessary to analyze the thermal risk of iso-octyl nitration process.
Firstly, Reaction Calorimeter (RC1e) was used to evaluate the thermal behavior of this reaction, and the parameters such as adiabatic temperature rise (ΔTad), Maximal Temperature attainable by runaway of the desired Synthetic Reaction (MTSR) were calculated based on RC1 data. Then Differential Scanning Calorimeter (DSC) and Accelerating Rate Calorimeter (ARC) were used to study the decomposition characteristics of the final products, and to obtain the relationship between induction period and temperature. Based on this relationship, the important temperature TD24 corresponding to the induction period of 24h was calculated. After that, High performance liquid chromatography (HPLC) was used to analyze the concentration of the desired product. Then the yield of EHN was obtained, and was used to correct the relevant thermodynamic parameters. Finally, based on the parameters of MTSR, ΔTad and TD24, the thermal runaway hazard was evaluated. The result showed that the thermal runaway risk of this reaction was of the criticality index 2 at low temperature; While at 25℃ and 30℃, the secondary decomposition was initiated, which made the thermal runaway criticality index increase to 5.
Key words: EHN, nitration, RC1e, ARC, DSC, criticality index of thermal runaway
目录
1 绪论 1
1.1 研究意义和应用前景 1
1.2 国内外研究概况 1
1.3 本论文的主要工作 3
2 失控情景评估方法 4
2.1 典型失控情形 4
2.2 工艺危险度评估 4
3 RC1e实验 6
3.1 实验原理 6
3.2 试剂 7
3.3 实验过程及实验条件 7
3.4 实验结果分析 9
4 EHN的热稳定性分析 13