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Synthesis and Properties of a Novel Energetic Salt 3,5-diamino-4-nitro-1H-pyrazol-2-ium Pentazolate
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School of Chemistry and Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China

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    Abstract:

    A novel energetic non-metallic pentazolate salt, 3,5-diamino-4-nitro-1H-pyrazol-2-ium pentazolate (3), was synthesized by a metathesis reaction of 3,5-diamino-4-nitropyrazole hydrochloride with sodium pentazolate. The structure of 3 was characterized by nuclear magnetic resonance (NMR), single crystal X-ray diffraction analysis (SC-XRD), Fourier infrared spectroscopy (IR) and elemental analysis (EA). The study on thermal behavior of 3 by using differential scanning calorimetry (DSC) and thermogravimetry (TG) show that its onset decomposition temperature is 119.5 ℃, which is higher than most non-metallic pentazolate salts. The apparent activation energies were calculated based on DSC curves at different heating rates. Based on the measured density at room temperature (1.71 g·cm-3) and calculated enthalpy of formation (503.3 kJ·mol-1), the detonation performances of 3D=8483 m·s-1p=26.4 GPa) were calculated by Explo5 V6.05.02 software. The impact sensitivity and friction sensitivity of 3 are 10 J and 216 N, respectively.

    表 3 化合物3的理化性质及爆轰性能Table 3 Physiochemical properties and detonation performances of compound 3
    表 1 化合物3的晶体结构数据和精修参数Table 1 Crystal data and structure refinement details for compound 3
    图1 化合物3的(a) 晶体结构; (b) 分子平面性; (c) 三维堆积图; (d) 二维氢键网络图Fig.1 (a) Crystal structure of 3; (b) Molecular planarity of 3, (c) 3D supramolecular structure of 3, (d) 2D hydrogen bond network in 3
    图2 化合物3的(a)Hirshfeld表面; (b)二维指纹图; (c)原子间相互作用的比例Fig.2 (a) Hirshfeld surfaces of compound 3, (b) 2D fingerprint plot in crystal stacking of compound 3, (c) Pie graph for individual atomic contact percentage of compound 3
    图3 化合物3的TG-DSC曲线(N2气氛,5 ℃·min-1)Fig.3 TG-DSC curves of compound 3 under N2 at a heating rate of 5 ℃·min-1
    图4 化合物3的DSC曲线Fig.4 DSC curves of 3 under N2 at different heating rates
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喻儒靖,刘雨季,曾志伟,等.3,5-二氨基-4-硝基吡唑五唑新型含能离子盐合成和性能[J].含能材料,2022,30(3):222-227.
YU Ru-jing, LIU Yu-ji, ZENG Zhi-wei, et al. Synthesis and Properties of a Novel Energetic Salt 3,5-diamino-4-nitro-1H-pyrazol-2-ium Pentazolate[J]. Chinese Journal of Energetic Materials,2022,30(3):222-227.

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History
  • Received:December 06,2021
  • Revised:December 28,2021
  • Adopted:January 07,2022
  • Online: March 17,2022
  • Published: March 25,2022