TEX色谱分析条件的建立及热稳定性研究  

Establishment of Chromatographic Conditions and Study on Thermal Stability of 4,10-Dinitro-2,6,8,12-Tetraoxa-4,10-Diazatetracyclo-[5.5.0.0^(5,9)0^(3,11)]-Dodecane(TEX)

作　　者：王瑞[1] 孟子晖[1] 薛敏[1] 徐志斌[1] 崔可建[1] 赵凤起[2] 肖立柏[2] 郭琪 

机构地区：[1]北京理工大学化工与环境学院,北京100081 [2]西安近代化学研究所燃烧与爆炸技术重点实验室,陕西西安710065 [3]西安航天化学动力厂,陕西西安710065

出　　处：《火炸药学报》2015年第4期27-30,共4页Chinese Journal of Explosives & Propellants

摘　　要：为研究4,10-二硝基-2,6,8,12-四氧杂-4,10-二氮杂四环[5.5.0.05,903,11]十二烷(TEX)的稳定性,建立了TEX的高效液相色谱(HPLC)分析方法,采用TG-DTG和DSC研究了TEX的热行为,测定了不同升温速率(5、10、15、20和25K/min)下TEX的分解峰温,用Kissinger方法计算了TEX放热分解反应的表观活化能(Ek)和指前因子(A),用热力学方程计算了TEX放热分解反应的活化熵(△S≠)、活化焓(△H≠)和活化吉布斯自由能(△G≠)。结果表明,TEX对热较稳定,其热分解反应的△S≠、△H≠和△G≠值分别为501.03J/(K·mol)、432.48kJ/mol、145.26kJ/mol。To study the stability of 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo-[5.5.0.0^5,9 0^3,11 ]-dodecane （TEX）,a high performance liquid chromatography（HPLC）analysis method for TEX was developed.The thermal behavior of TEX was studied by thermogravimetry-derivative thermogravimetry（TG-DTG）and differential scanning calorimetry（DSC）,the peak temperatures at different heating rates（5,10,15,20 and 25 K/min）were determined. The apparent activation energy（Ek ）and preexponential constant（A）of the exothermic decomposition reaction were calculated by Kissinger′s method.Activation enthalpy（△S^≠）,activation entropy（△H^≠）and activation Gibbs free energy（△G^≠）for the exothermic decomposition reaction of TEX were calculated according to thermodynamic equations.The results indicate that TEX is stable to heat.The values of △S^≠,△H^≠ and △G^≠ are 501 .03 J/（K·mol）, 432.48 kJ/mol and 145.26 kJ/mol,respectively.

关 键 词：分析化学 TEX HPLC DSC 热稳定性 热力学参数 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O657.7[理学—分析化学]