Synthesis Process And Particle Size Control Of Several Energetic Compounds

2,5,7,9-tetranitro-2,5,7,9-tetraazabicyclo[4,3,0]nonanone-8-one?K-56?and[2,2?-bi?1,3,4-oxadiazole?]-5,5?-dinitramide?ICM-101?are two kinds of elementary energetic materials with excellent properties.In this paper,their synthesis processes are optimized respectively,the optimal synthesis process conditions were obtained and a100-gram amplification experiment was completed.Hexanitrostilbene?HNS?is a widely used low-sensitivity heat-resistant explosive.In this paper,the crystallization of HNS was carried out,and crystal particles with a particle size of about 100³00?m were obtained.?1?The optimal process conditions for the synthesis of K-56 were:1 g K-56precursor,8 ml acetic anhydride,7.5 ml fuming nitric acid,nitrification temperature 25?,nitrification time 4 h,the yield under this condition was 76.4%with the purity was 99%.The liquid phase analysis method of K-56 was as follows:the detection wavelength was285 nm,and the flow ratio was acetonitrile/methanol=30/70,and the flow rate was 1.5ml·min^-1.K-56 was characterized by micro melting point instrument,infrared spectrometer,nuclear magnetic resonance spectrometer and single crystal X-ray diffractometer.The crystal structure was analyzed and discussed.?2?The optimal process for synthesizing ICM-101 precursor were:0.56g oxalic acid dihydrazide,1.05g KHCO₃,30ml water,1.13g 97%BrCN,reaction time 2h,reaction temperature 25?,the yield under these conditions was 93.7%.The optimal process conditions for the synthesis of ICM-101 were:0.5g ICM-101 precursor,4ml fuming nitric acid,nitrification temperature 30?,nitrification time 12h,and the yield under this condition was 87.3%.ICM-101 was characterized by micro melting point instrument,infrared spectrometer and nuclear magnetic resonance spectrometer,and its crystal structure was analyzed and discussed.?3?Crystallization of HNS by cooling crystallization method with N,N-dimethylformamide and fuming nitric acid as the solvent,the initial cooling temperature was 90?,seeding temperature was 80?,natural cooling start temperature was 40?,by changing the stirring rate and the temperature decreasing rate in the crystallization process,HNS crystal particles with an average particle size of about 100?m,200?m,and 300?m was be obtained.