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甲胺盐酸盐/发烟硝酸体系中DPT硝解-亚硝解反应制备MNX
Preparation of MNX from DPT Through Nitrolysis-nitrosolysis Reaction in CH3NH2∙HCl/Fuming Nitric Acid System
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中文摘要:
      用CH3NH2·HCl代替NH4NO3作为3,7-二硝基-1,3,5,7-四氮杂双环[3.3.1]壬烷(DPT)与发烟硝酸反应的添加剂,考察了CH3NH2·HCl对生成1-亚硝基-3,5,7-三硝基-1,3,5,7-四氮杂环辛烷(MNX)的影响。研究了CH3NH2·HCl促进DPT与发烟硝酸反应制备MNX的工艺,考察了发烟硝酸和CH3NH2·HCl的加入量、反应时间和反应温度对反应的影响。结果表明,通过正交实验确定的最佳反应条件为:n(DPT)∶n(CH3NH2·HCl)=1∶2.5,反应时间10 min,反应温度-25 ℃。在最优反应条件下MNX的收率为78.5%。本方法避免使用NaNO2溶液和N2O4作为亚硝基来源,简化了MNX的制备工艺,且反应废液容易处理,硝酸回收率为75%。CH3NH2·HCl对DPT与发烟硝酸反应的促进作用比NH4NO3的显著,提出了CH3NH2·HCl(或NH4NO3)分解成CH3NH3(或NH3)作为Lewis碱催化剂促进DPT与发烟硝酸反应的可能机理,其中涉及到硝酸通过氧化还原反应生成亚硝酸作为亚硝基来源的过程。
中文关键词: 3,7-二硝基-1,3,5,7-四氮杂双环[3.3.1]壬烷(DPT)  1-亚硝基-3,5,7-三硝基-1,3,5,7-四氮杂环辛烷(MNX)  硝酸铵  甲胺盐酸盐  Lewis碱催化剂  硝解反应  亚硝解反应
英文摘要:
      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.
英文关键词: 3,7-dinitro-1,3,5,7-tetraazabicyclo[3.3.1]nonane (DPT)  1-nitroso-3,5,7-trinitro-1,3,5,7-tetraazacyclooctane (MNX)  NH4NO3  CH3NH2·HCl  Lewis base catalyst  nitrolysis  nitrosolysis
DOI:10.11943/CJEM2018148
投稿日期:2018-06-05
最后修改日期:2018-09-13
网络出版日期:2018-09-06
书版出版日期:2019-02-25
基金项目:人才工程:江苏省“青蓝工程”资助
引用文献: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(Hanneng Cailiao),2019,27(2):119-124.
作者单位E-mail
张宇 南京理工大学 化工学院 zhangyu@njust.edu.cn 
徐子帅 甘肃银光化学工业集团有限公司  
阮健 甘肃银光化学工业集团有限公司  
王小龙 甘肃银光化学工业集团有限公司  
张路遥 甘肃银光化学工业集团有限公司  
罗军 南京理工大学 化工学院 luojun@njust.edu.cn 
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