摘要
为了改善FOX-7的性能,采用喷雾重结晶法制备了细化FOX-7,研究了溶剂与非溶剂种类、药液质量浓度及搅拌速率对重结晶细化FOX-7晶体形貌的影响,确定了最佳工艺条件;采用扫描电子显微镜(SEM)及粒度分析软件对细化FOX-7进行了粒径形貌表征;采用X射线粉末衍射系统(XRD)、傅里叶变换红外光谱仪(FT-IR)、差示扫描量热仪(DSC)、12型落锤仪及WM-1型摩擦感度仪对微米级FOX-7晶体进行表征及性能测试。结果表明,最佳工艺条件为:溶剂-非溶剂为NMP-H2O,药液质量浓度为0.4g/mL,搅拌速率为450r/min,可获得平均粒径为1.81μm的微米级FOX-7晶体;微米级FOX-7晶型与原料FOX-7相比未发生改变;微米级FOX-7表观活化能比原料FOX-7提高了88.74kJ/mol,热爆炸临界温度提高了19℃,特性落高从82.3cm提升至136.1cm,摩擦感度从12%降至0;表明微米级FOX-7比原料FOX-7具有更好的热安定性及更低的机械感度。
In order to improve the performance of FOX-7,the refined FOX-7 was prepared by the spray recrystallization method.The effects of solvent and non-solvent types,liquid mass concentration and stirring rate on the crystal morphology of refined FOX-7 were studied,and the optimal process conditions for the refined FOX-7 were determined.The morphology and particle size of the refined FOX-7 was characterized by using the scanning electron microscope(SEM)and particle size analysis software.The properties of micron FOX-7 were characterized and tested by using X-ray powder diffraction system(XRD),Fourier transform infrared spectrometer(FT-IR),differential scanning thermometer(DSC),type 12 drop hammer instrument and WM-1 friction sensitivity meter.The results showed that the optimal process conditions for obtaining the refined FOX-7 are as follows:solvent-nonsolvent is NMP-H2O,the liquid mass concentration is 0.4g/mL,the stirring rate is 450 r/min,and the micron FOX-7 crystals with an average particle size of 1.81μm can be obtained.The crystal form of micron FOX-7 has no change compared to the raw FOX-7.The apparent activation energy of micron FOX-7(88.74kJ/mol)is higher than that of the raw FOX-7,and the critical temperature of the thermal explosion is increased by 19℃.The characteristic drop height is increased from 82.3cm to 136.1cm,and the friction sensitivity decreased from 12%to 0.It shows that the micron FOX-7 has better thermal stability and lower mechanical sensitivity than that of the raw FOX-7.
作者
李小东
杨武
刘慧敏
宋昌贵
孙红燕
田健安
LI Xiao-dong;YANG Wu;LIU Hui-min;SONG Chang-gui;SUN Hong-yan;TIAN Jian-an(School of Environment and Safety Engineering, North University of China, Taiyuan 030051, China;Science and Technology on Electromechanical Dynamic Control Laboratory, Xi′an 710065, China)
出处
《火炸药学报》
EI
CAS
CSCD
北大核心
2020年第6期662-668,共7页
Chinese Journal of Explosives & Propellants
基金
国防科工局基础产品创新科研项目。
关键词
物理化学
FOX-7
喷雾重结晶
晶体粒径
热动力学分析
机械感度
physical chemistry
FOX-7
spray recrystallization
crystal size
thermal kinetic analysis
mechanical sensitivity
