以1H，4H-6-硝基吡唑[4，3-c]并吡唑-3-羧酸为起始原料，经过一步脱羧硝化反应得到1H，4H-3，6-二硝基吡唑[4，3-c]并吡唑（DNPP），收率76．7％，然后与硝酸铅、3，6-二肼基-1，2，4，5-四嗪反应合成了 DNPP 碱式铅盐（Pb-DNPP）与 DNPP 的3，6-二肼基-1，2，4，5-四嗪含能离子盐（DHT-DNPP）。采用红外光谱、1 H NMR、13 C NMR、质谱及元素分析等对其结构进行了表征，利用 DNPP 质谱裂解碎片信息，探讨了热解反应机理，揭示了其裂解微观反应过程。采用 DSC 和 TG-DTG 法研究了 DNPP 及其两种盐的热行为。结果表明，DNPP、Pb-DNPP 和 DHT-DN-PP 的放热分解峰分别为256．4、319．1和174．3℃，显示 Pb-DNPP 比 DNPP 和 DHT-DNPP 有更好的热稳定性。%Using 1H,4H-6-nitropyrazolo[4,3-c]pyrazole-3-carboxy as primary material,1H,4H-3,6-dinitropyrazolo [4,3-c]pyrazole (DNPP)was synthesized via one step reaction of decarboxylation and nitration with a yield of 76.7%.Then the basic lead salt of DNPP (Pb-DNPP)and the 3,6-dihydrazine-1,2,4,5-tetrazine energetic ionic salt of DNPP (DHT-DNPP)were firstly obtained by the reaction of DNPP with lead nitrate and 3,6-dihydrazine-1,2,4, 5-tetrazine,respectively.Their structures were characterized by IR,1 H NMR,13 C NMR ,MS and elemental analyses.The pyrolysis reaction mechanism and cleavage reaction pathways of DNPP were investigated by MS (EI) fragmentation information.The thermal behaviors of DNPP,Pb-DNPP and DHT-DNPP were studied by differential scanning calorimetry (DSC)and thermogravimetry (TG)-derivative thermogravimetry (DTG).Results show that the peak temperatures of the exothermic decomposition reaction of DNPP,Pb-DNPP and DHT-DNPP are 256.4, 319.1 and 174.3℃,respectively,revealing that Pb-DNPP has better thermal stability than DNPP and DHT-DNPP.
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