Synthesis And Theoretical Study Of 2,4,6,8-tetrachitro-2,4,6,8-tetraazabicyclic [3.3.0] Octane

2,4,6,8-tetra-nitro-2,4,6,8-tetra-heterocyclic [3.3.0] octane,also known as bicyclic HMX,has good detonation performance,so it has good research significance and application prospects.However,there are not too many reports about its synthetic route.The "three-step" synthetic route,which starts from methylene diacetyl ammonia to synthesize bicyclic HMX,is expensive and has low yield,limiting industrial production and large-scale application of bicyclic HMX.Therefore,the development of a new synthesis process of bicyclic-HMX and the realization of efficient,green,and low-cost manufacturing of bicyclic-HMX have significant application value and practical significance for expanding the application scenarios of bicyclic-HMX,promoting the development of modern aerospace industry,and promoting the advancement of the current weapon system.In this paper,the detonation performance parameters of bicyclic-HMX and its derivatives are described from the theoretical calculation.Secondly,the new synthesis route of double cyclo-HMX is explored as follows: Using potassium sulfamate,37% formaldehyde,40%glyoxal as raw material,deionized water as a solvent,organic acid as an acid catalyst,the intermediate parent ring potassium sulfamate was prepared by mannish condensation reaction and hydroxyl aldehyde condensation reaction and then fuming nitric acid-acetic anhydride as nitrification system.2,4,6,8-tetranitro-2,4,6,8-tetraazabicyclic [3.3.0] octane was synthesized by reflux at 40 ℃ water bath;Finally,the optimal reaction conditions were screened for2,4,6,8-tetraazabicyclic [3.3.0] octane sulfonate and the final product,2,4,6,8-tetrachitro-2,4,6,8-tetraazabicyclic [3.3.0] octane.The following conclusions were obtained:1.Preparation of synthetic intermediate parent ring 2,4,6,8-tetraazabicyclic [3.3.0] octane sulfonate potassium salt the best synthesis route is: at 25 ℃ reaction temperature,input raw potassium sulfamate 3.3 mmol and N(glyoxal): N(formaldehyde)= 1.6,adding 0.5 m L deionized water,reaction time 12 h,adding 0.075 mmol formic acids as the acid catalyst is the best reaction conditions.2.Nitration of 2,4,6,8-tetraazabicyclic [3.3.0] octane sulfonate potassium salt to obtain the target product 2,4,6,8-tetrachitro-2,4,6,8-tetraazabicyclic [3.3.0] octane,its synthesis of the best process route is: Under the condition of nitrification temperature of 40 ℃,the intermediate 2,4,6,8-tetraazabicyclic [3.3.0] octane sulfonic acid potassium salt was put in,and then the best nitrification agent was added to smoke nitric anhydride system,and the mole ratio was 1.3:1.The nitrification reaction was held for 3 h.At this time,the yield of dicyclic HMX reached 66%.