CHINESE JOURNAL OF ENERGETIC MATERIALS
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1,1′-二羟基-5,5′-联四唑-二氨基乙二肟 (DAGBTO)富氮含能盐的合成、晶体结构及热性能
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作者单位:

(北京理工大学爆炸科学与技术国家重点实验室, 北京 100081)

作者简介:

张至斌(1992-),男,硕士研究生,主要从事含能材料的合成与性能研究。e-mail: bitZYRY@163.com 通信联系人: 张建国(1974-),男,教授,博士生导师,主要从事含能材料的理论与应用研究。e-mail: zjgbit@bit.edu.cn

通讯作者:

张建国(1974-),男,教授,博士生导师,主要从事含能材料的理论与应用研究。e-mail: zjgbit@bit.edu.cn

基金项目:

爆炸科学与技术国家重点实验室基金资助(YBKT16-04)


Synthesis,Crystal Structure and Thermal Behavior of Nitrogen-riched Energetic Salt of Diaminoglyoxinium 1H,1′H-5,5′-bitetrazole-1,1′-diolate
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(State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China)

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    摘要:

    以二氨基乙二肟(DAG)和1, 1′-二羟基-5, 5′-联四唑(BTO)为起始原料合成了新型富氮含能盐—1, 1′-二羟基-5, 5′-联四唑-二氨基乙二肟(DAGBTO)。用元素分析、傅里叶变换红外光谱、核磁和质谱对其结构进行了表征。培养了目标化合物的单晶, 并通过X-射线单晶衍射仪测定了其晶体结构, 结果表明其属于单斜晶系, C2/c空间群, 晶胞参数为: a=11.3121(11) Å, b= 6.4480(4) Å, c=15.3202(16) Å, β=105.990(2)°, V=1074.23(17) Å3, Z=4, Dc=1.782 g·cm-3, F(000)=592。通过差示扫描量热分析仪(DSC)研究其热分解行为, 并对其非等温反应动力学参数和热安全性参数进行计算, 其反应活化能为210.6 kJ·mol-1(Kissinger法)和207.9 kJ·mol-1 (Ozawa-Doyle法), 二者一致性较好, 热分解温度高于190 ℃, 热爆炸临界温度Tbp为200.7 ℃。

    Abstract:

    A novel energetic salt of diaminoglyoxinium 1H, 1′H-5, 5′-bitetrazole-1, 1′-diolate (DAGBTO) was synthesized by using diaminoglyoxime(DAG) and 1H, 1′H-5, 5′-bitetrazole-1, 1′-diol(BTO) as raw materials, and its structure was characterized by elemental analysis, Fourier transform infrared spectroscopy(FT-IR) spectroscopy, 1H NMR, 13C NMR and mass spectrometry. The single crystal of DAGBTO was obtained and its structure was determined by X-ray single-crystal diffractometer. Results show that DAGBTO belongs to monoclinic space group C2/c with a density of 1.782 g·cm-3, and the cell parameters are as follows: a=11.3121(11) Å, b=6.4480(4) Å, c=15.3202(16) Å, β=105.990(2) °, V=1074.23(17) Å3, F(000)=592. The thermal decomposition behavior was investigated by differential scanning calorimetry(DSC) technology, and non-isothermal kinetic parameters were also calculated. Results indicate that it has a good thermal stability with the decomposition temperature above 190 ℃. The apparent activation energy are 210.6 kJ·mol-1 (Kissinger) and 207.9 kJ·mol-1(Ozawa-Doyle), respectively, and the critical temperature of thermal explosion is 200.7 ℃.

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引用本文

张至斌,张建国,秦涧,等.1,1′-二羟基-5,5′-联四唑-二氨基乙二肟 (DAGBTO)富氮含能盐的合成、晶体结构及热性能[J].含能材料, 2016, 24(5):421-426. DOI:10.11943/j. issn.1006-9941.2016.05.001.
ZHANG Zhi-bin, ZHANG Jian-guo, QIN Jian, et al. Synthesis, Crystal Structure and Thermal Behavior of Nitrogen-riched Energetic Salt of Diaminoglyoxinium 1H,1′H-5,5′-bitetrazole-1,1′-diolate[J]. Chinese Journal of Energetic Materials, 2016, 24(5):421-426. DOI:10.11943/j. issn.1006-9941.2016.05.001.

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  • 收稿日期: 2015-08-24
  • 最后修改日期: 2015-09-29
  • 录用日期: 2015-10-15
  • 在线发布日期: 2016-05-05
  • 出版日期: 2016-05-20