3,4-双(4'-硝基呋咱-3'-基)氧化呋咱合成、表征与性能研究

Study on Synthesis,Characterization and Properties of 3,4-Bis(4'-nitrofurazano-3'-yl)furoxan

采用丙二腈为原料,经亚硝化、重排、肟化、脱水环化、分子间缩合环化以及氧化等反应合成含能化合物3,4-双(4'-硝基呋咱-3'-基)氧化呋咱(DNTF),总收率为43%,并采用红外光谱、核磁共振光谱、INADEQUATE谱、质谱和元素分析等进行了结构表征.开展了DNTF物化与爆轰性能研究,其密度1.937 g/cm3,熔点109～110℃,爆速8930 m/s(ρ=1.870 g/cm3),摩擦感度44%～60%(90°摆角),撞击感度80%～96%(10 kg,25 cm),特性落高H50为38.9 cm(5 kg),爆发点315～340℃,爆热5789 J/g(ρ=1.83 g/cm3),威力168.4%TNT当量,真空安定性(5 g样品,100℃,40 h)放气量1.09 mL.采用DSC法和TG-DTG法测定了DNTF的热稳定性,利用真空安定法研究了DNTF同1,3,5-三硝基-1,3,5-三氮杂环己烷(RDX),1,3,5,7-四硝基-1,3,5,7-四氮杂环辛烷(HMX),2,4,6-三硝基甲苯(TNT)及推进剂含能组分的相容性,结果表明:DNTF具有较好的热稳定性,其分解温度为253.56℃;良好的相容性,可与常用含能材料(RDX,HMX,TNT)相容.DNTF能量较高、熔点较低、机械感度适中,安定性好,可作为新一代熔铸混合炸药的液相载体.

An energetic material 3,4-bis（4＇-nitrofurazano-3＇-yl）furoxan was synthesized using dicyanopropane as starting material through nitrosation,rearrangement,oximation,dehydration cyclization,dimerization and oxidation etc.steps with total yield of 43%.Its molecular structure was confirmed by IR,1H NMR,13C NMR,15N NMR,INADEQUATE,MS and elemental analysis.The properties of DNTF had been tested in our experiments,the results showed that density was 1.937 g/cm3,melting point was 109～110 ℃,detonation velocity was 8930 m/s（ρ=1.870 g/cm3）,friction sensitivity was 44%～60%（90°）,impact sensitivity was 80%～96%（10 kg,25 cm）,H50 was 38.9 cm,explosion point was 315～340 ℃,explosion heat was 5789 J/g（ρ=1.83 g/cm3）,explosion strength was 168.4% of TNT,and deflation volume was 1.09 mL（5 g,100 ℃,40 h） in vacuum stability test.Its thermal stability was identified by DSC and TG techniques,and compatibility was investigated by vacuum stability test.The experimental results showed that DNTF had better thermal stability and its thermal decomposition was 253.56 ℃（peak）,the compatibility of DNTF was better and might be compatible with some general energetic materials,such as 1,3,5-trinitro-1,3,5-triazinane（RDX）,1,3,5,7-tetranitro-1,3,5,7-tetrazocane（HMX）,2-methyl-1,3,5-trinitrobenzene（TNT） etc.Because of its high energy,low melting point,moderate mechanical sensitivity and good compatibility,DNTF could be used as an effective liquid-phase carrier in melt-cast explosives.