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Preparation of MNX from DPT Through Nitrolysis-nitrosolysis Reaction in CH3NH2∙HCl/Fuming Nitric Acid System
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1.School of Chemical Engineering, Nanjing University of Science and Technology, Nanjng 210094, China;2.Gansu Yin Guang Chemical Industry Group Co. Ltd., Baiyin 730900, China

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    Abstract:

    CH3NH2·HCl was used to replace NH4NO3 as an additive in the reaction of 3,7-dinitro-1,3,5,7-tetraazabicyclo[3.3.1]nonane (DPT) in fuming nitric acid, and the effect of CH3NH2·HCl on the formation of 1-nitroso-3,5,7-trinitro-1,3,5,7-tetraazacyclooctane (MNX) was investigated. The process of preparing MNX by CH3NH2·HCl promoting the reaction of DPT with fuming nitric acid was studied. The effects of loading amounts of fuming nitric acid and CH3NH2·HCl, reaction temperature and reaction time on the reaction were investigated. Results show that the optimum reaction conditions determined by orthogonal experiments are: n (DPT)∶n(CH3NH2·HCl)=1∶2.5,reaction time 10 min and reaction temperature -25 ℃. Under the optimum reaction conditions, the yield of MNX is 78.5%. This method avoids using NaNO2 solution and N2O4 as nitroso resource and simplifies the preparation process of MNX. The waste liquid is easy to be treated. The recovery of nitric acid is 75%. CH3NH2·HCl can promote the reaction of DPT with fuming nitric acid more significantly than NH4NO3. A possible mechanism of promoting the reaction of DPT and fuming nitric acid via decomposing CH3NH2·HCl (or NH4NO3) into CH3NH2 (or NH3) as a Lewis base catalyst is proposed, which involves the process of nitrous acid formation from nitric acid through a redox reaction as nitroso resource.

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张宇,徐子帅,阮健,等.甲胺盐酸盐/发烟硝酸体系中DPT硝解-亚硝解反应制备MNX[J].含能材料,2019,27(2):119-124.
ZHANG Yu, XU Zi-shuai, RUAN Jian, et al. Preparation of MNX from DPT Through Nitrolysis-nitrosolysis Reaction in CH3NH2∙HCl/Fuming Nitric Acid System[J]. Chinese Journal of Energetic Materials,2019,27(2):119-124.

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History
  • Received:June 05,2018
  • Revised:September 13,2018
  • Adopted:August 14,2018
  • Online: September 06,2018
  • Published: February 25,2019