硝镁法制吉纳过程中物料热稳定性分析  

Analysis on the Thermal Stability of Materials During the Synthesis of DINA by Magnesium Nitrate Method

作　　者：周鹏[1] 朱伊娜 陈利平[1] 陈网桦[1] ZHOU Peng;ZHU Yi-na;CHEN Li-ping;CHEN Wang-hua(Nanjing University of Science and Technology,Jiangsu Nanjing 210094,China)

机构地区：[1]南京理工大学化工学院

出　　处：《当代化工》2019年第10期2292-2296,2300,共6页Contemporary Chemical Industry

摘　　要：硝镁法合成吉纳的过程中存在很高的反应热失控风险.为了进一步辨识并降低这种风险,对反应过程中物料的反应进程及热稳定性进行了研究.在实验室规模下通过两种不同的路径合成了吉纳,利用傅里叶变换红外光谱仪研究了反应过程中反应体系官能团的变化情况,并得到了各步反应的反应方程式.利用差示扫描量热仪(DSC)测试了各阶段产物的热稳定性,发现在两种合成路径中反应体系的热稳定性都较差,且发现吉纳合成过程中最不稳定的反应阶段为发烟硝酸与二乙醇胺的酯化产物体系,其起始分解温度最低在70 ℃左右,比放热量为1 500 J/g.提出了通过混合加料的方式来合成吉纳,这种方法一方面可以使反应在较低的温度下平稳进行,另一方面可以降低物料在不稳定状态下存在的时间.In order to understand the thermal runaway risk of the reaction in the process of synthesizing DINA by the magnesium nitrate method,the variation process and thermal stability of the materials in the reaction process were studied.DINA was synthesized by two different paths in the laboratory scale,and the Fourier transform infrared spectrometer was used to study the change of the functional group of the reaction system during the process.The reaction equation of each step was obtained according to the results of FTIR.The thermal stability of the products at each stage was tested by differential scanning calorimetry(DSC),and it was found that the thermal stability of the reaction system was poor in both two synthetic routes.The most unstable substance in the synthesis of DINA was the esterification product of fuming nitric acid and diethanolamine(DEA),whose initial decomposition temperature was about 70°C and the specific heat release was around 1 500 J/g.In addition,a mixed feed method was proposed to synthesize DINA that can both conduct the reaction at a lower temperature and improve the thermal stability of the reaction system.

关 键 词：吉纳 合成路径 热稳定性 混合加料 

分 类 号：X937[环境科学与工程—安全科学] TQ226.1[化学工程—有机化工]