LLM-105合成新方法反应热分析  

Reaction heat analysis of new method for synthesis of LLM-105

作　　者：常佩[1] 王锡杰[1] 胡建建[1] 李亚南[1] 贾思媛[1] 王伯周[1] Chang Pei;Wang Xijie;Hu Jianjian;Li Yanan;Jia Siyuan;Wang Bozhou(Xi’an Modern Chemistry Research Institute,Xi’an 710065,China)

机构地区：[1]西安近代化学研究所,陕西西安710065

出　　处：《化学推进剂与高分子材料》2020年第2期33-37,共5页Chemical Propellants & Polymeric Materials

摘　　要：利用反应量热仪测定了2,6–二氨基–3,5–二硝基吡啶–1–氧化物(LLM-105)新合成方法的反应过程的反应热释放速率曲线及反应体系的比定压热容等热力学数据。结果表明:亚硝化合成N–亚硝基亚氨基二乙腈(NIDA)阶段,加料温度为15、20℃时的最大放热速率分别为121.60、142.05 W,反应体系的绝热温升分别为19.547、21.357 K;环化合成2,6–二氨基吡嗪–1–氧化物(DAPO)阶段,加料温度为5、10℃时的最大放热速率分别为53.47、94.54 W,反应体系的绝热温升分别为66.329、108.450 K;硝化氧化合成LLM-105阶段的最大放热速率为12.17 W,反应体系的绝热温升为61.421 K。这表明新方法合成LLM-105反应放热平稳,工艺过程安全,以此工艺可以开展放大制备。The reaction heat release rate curve of the reaction process and the thermodynamic data including the specific heat capacity at constant pressure,etc.of the reaction system for the new synthesis method of 2,6-diamino-3,5-dinitropyridine-1-oxide(LLM-105)were determined by using the reaction calorimeter.The results show that during the nitrosation synthesis stage of the N-nitrosoiminodiacetonitrile(NIDA),when the feeding temperature is 15℃and 20℃respectively,the maximum exothermic rate is 121.60 W and 142.05 W respectively,and the adiabatic temperature rise of the reaction system is 19.547 K and 21.357 K respectively.During the cyclization synthesis stage of the 2,6-diaminopyrazine-1-oxide(DAPO),when the feeding temperature is 5℃and 10℃respectively,the maximum exothermic rate is 53.47 W and 94.54 W respectively,and the adiabatic temperature rise of the reaction system is 66.329 K and 108.450 K respectively.During the nitration oxidation synthesis stage of the LLM-105,the maximum exothermic rate is 12.17 W,and the adiabatic temperature rise of the reaction system is 61.421 K.It shows that the synthesis of LLM-105 by using the new method has the stable reaction heat release and safe process,therefore this process can be enlarged.

关 键 词：2 6-二氨基–3 5-二硝基吡啶–1-氧化物 LLM-105 合成 反应热 

分 类 号：TQ254[化学工程—有机化工]