N_2O_5/HNO_3硝解TAIW一步法制备ε-HNIW  

Synthesis of ε-HNIW by One-pot Nitrolysis of TAIW with N_2O_5/ HNO_3

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作  者:丁伟兴 胡小玲[2] 董波[2] 吴秋洁[2,3] 钱华[2,3] 

机构地区:[1]武进开放大学,江苏常州213000 [2]南京理工大学化工学院,江苏南京210094 [3]国家民用爆破器材质量监督检验中心,江苏南京210094

出  处:《爆破器材》2015年第4期15-18,共4页Explosive Materials

基  金:国家自然科学基金(21406116);第六批南京理工大学"卓越计划""紫金之星"项目资助

摘  要:针对硝硫混酸硝解-转晶两步法制备ε-HNIW的现状,本文采用绿色硝化剂N2O5/HNO3硝解2,6,8,12-四乙酰基-2,4,6,8,10,12-六氮杂四环-[5,5,0,03,11,05,9]十二烷(TAIW)一步法直接制备ε-HNIW,并采用NMR、MS、XRD对其结构及晶型进行鉴定。ε-HNIW得率82.72%,纯度98.24%。该方法不仅避免硫酸的使用,减轻了废酸污染,而且在硝化液中直接转晶,简化了工艺路线,具有较强的应用前景。ε-HNIW was synthesized by one-pot nitrolysis of 2, 6, 8,12-tetraacetyl-2, 4, 6, 8, 10, 12-hexaazatetracyclo[ 5, 5, 0, 0^3,11 ,0^5,9] dodecane (TAIW) with N2O5/HNO3 as the nitrating agent, which overcame the drawbacks of mix acid-nitrolysis and two step-crystal transformation. Structure and crystal form of ε-HNIW were characterized by NMR, MS and XRD. Yield of ε-HNIW is 82.72% , and its purity is 98.24%. By the use of new nitrating agent, the reaction eliminated the use of concentrated sulfuric acid and was eco-friendly. Moreover, ε-HNIW was directly transformed in the solution. The simplified process route shows good prospect in industry.

关 键 词:N2O5/HNO3 ε-HNIW 绿色合成 TAIW CL-20 

分 类 号:O62[理学—有机化学] TQ56[理学—化学]

 

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