FOX-7合成工艺优化及中间体热分解特性  

Synthesis Process Optimization of FOX-7 and Study on Thermal Decomposition Characteristics of Intermediate

作　　者：何文祥 郭子超 陈利平[1] 刘峰 HE Wen-xiang;GUO Zi-chao;CHEN Li-ping;LIU Feng(School of Chemistry and Chemical Engineering,Nanjing University of Science and Technology,Nanjing 210094,China)

机构地区：[1]南京理工大学化学与化工学院,江苏南京210094

出　　处：《火炸药学报》2023年第9期788-796,I0001,共10页Chinese Journal of Explosives & Propellants

基　　金：江苏省基础研究计划(自然科学基金)(No.BK20200495)。

摘　　要：为了安全合成1,1-二氨基-2,2-二硝基乙烯(FOX-7),对其合成过程的硝化反应工艺进行优化,提出了分步合成的新方法;利用差示扫描量热仪(DSC)研究FOX-7合成过程的中间体2-甲基-4,6-二羟基-5-硝基嘧啶(物质2)的热分解特性;运用模型拟合法,选用自催化模型同时对DSC等温和动态两种量热模式的实验数据进行动力学计算,获取准确的动力学参数,建立其热分解动力学模型,基于该模型对TMR ad和T D24进行预测:结合硝化机理,利用反应量热仪(RC1e)研究不同工艺条件下反应体系的放热特性。结果表明,物质2稳定性好,可将其作为原料进行硝化反应;使用新工艺合成FOX-7,硝化反应的反应热降低35%左右,绝热温升由98.7 K降至65 K左右,降低了热风险失控的严重度。To synthesize 1,1-diamino-2,2-dinitroethylene(FOX-7)safely,the nitration reaction process was optimized and a new stepwise method was proposed.The thermal decomposition characteristics of 2-methyl-4,6-dihydroxy-5-nitropyrimidine(Compound 2),an intermediate in the synthesis of FOX-7,were studied by differential scanning calorimeter(DSC).Using the model fitting method,the autocatalytic model was chosen to perform kinetic calculations on the experimental data of both DSC isothermal and dynamic calorimetric modes.The accurate kinetic parameters were obtained,and its thermal decomposition kinetic model was established.Based on this model,the TMR ad and T D24 values were predicted.Combined with the nitration mechanism,the exothermic characteristics of the reaction system under different process conditions were studied by reaction calorimeter(RC1e).The results show that the intermediate is stable and can be used as raw material for nitration reaction.The synthesis of FOX-7 under new process results in a significant reduction of about 35%on the heat of reaction,makes the adiabatic temperature decrease from 98.7 K to 65 K,and reduces the possibility of uncontrolled thermal risk.

关 键 词：物理化学 FOX-7 2-甲基-4 6-二羟基-5-硝基嘧啶 工艺优化 热分解动力学 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] TQ564[化学工程—炸药化工]