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5,5′-联四唑-1,1′-二氧-1,2,4-三氮唑含能离子盐的合成、表征及热行为
作者:
作者单位:

(1. 西南科技大学四川省非金属复合与功能材料重点实验室——省部共建国家重点实验室培育基地, 四川 绵阳 621010; 2. 西安近代化学研究所, 陕西 西安 710065)

作者简介:

尚宇(1990-),男,硕士研究生,主要从事含能材料研究。e-mail: 350389174@qq.com 通信联系人: 金波(1982-),男,副教授,主要从事富勒烯化学和含能材料研究。e-mail: jinbo0428@163.com

通讯作者:

金波(1982-),男,副教授,主要从事富勒烯化学和含能材料研究。e-mail: jinbo0428@163.com

基金项目:

国家自然科学基金(51372211),西南科技大学杰出青年基金( 13zx9107)和非金属复合与功能材料重点实验室—省部共建国家重点实验室培育基地开放基金项目(14tdfk05)


Synthesis, Characterizations and Thermal Behavior of Bis-1,2,4-triazolium 1H, 1′H -5,5′-bistetrazole-1,1′-diolate
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(1. State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010, China; 2. Xi′an Modern Chemistry Research Institute, Xi′an 710065, China)

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    摘要:

    以5, 5′-联四唑-1, 1′-二羟基二水合物(BTO)、1, 2, 4-三氮唑为原料合成了一种新的5, 5′-联四唑-1, 1′-二氧-1, 2, 4-三氮唑(T2BTO)含能离子盐。采用X-射线单晶衍射、FT-IR、1H NMR、13C NMR和元素分析表征了其结构。采用差示扫描量热法(DSC)和热重-微分热重(TG-DTG)研究了其热行为。用Kissinger法和Ozawa法分别计算了其热分解动力学参数(活化能EaEO、指前因子A)。采用WL-1型撞击感度测试仪测定了其特性落高H50。用Kamlet-Jacobs经验公式计算了其爆速(D)和爆压(p)。结果表明,该晶体属于单斜晶系, C2/c空间群, 晶体学参数为a=15.2410(12)Å, b=10.5185(8)Å, c=7.7546(7)Å, V=1221.26(18)Å 3, Dc=1.688 g·cm-3, Z=8。在10 K·min-1的DSC曲线上, 其分解峰值温度为519.9 K, TG曲线上只存在一个失重阶段, 该阶段位于453.2~523.2 K, 失重为90.8%, 显示其有较好的热稳定性。EK=144.39 kJ·mol-1, EO =145.52 kJ·mol-1, ln(A/s-1)=32.99, H50>61.0 cm, D=7579 m·s-1, p=24.49 GPa。

    Abstract:

    A new energetic ionic salt bis-1, 2, 4-triazolium 1H, 1′H-5, 5′-bistetrazole-1, 1′-diolate (T2BTO) was synthesized by using 1H, 1′H-5, 5′-bistetrazole-1, 1′-diol dihydrate (BTO) and 1, 2, 4-triazole as starting materials. Its structure was characterized by X-ray single crystal diffraction, FT-IR, 1H NMR, 13C NMR and elemental analyses. Its thermal behavior was studied by differential scanning calorimetry(DSC) and thermogravimetry-derivative thermogravimetry(TG-DTG). Its kinetic parameters of thermal decomposition(activation energy EaEO and pre-exponential factor A)were calculated by Kissinger′s and Ozawa′s method. The characteristic drop height of impact sensitivity (H50) was determined by WL-1 type impact sensitivity test instrument. Its detonation velocity (D) and detonation pressure (p) were calculated by Kamlet-Jacobs empirical formula. Results show that the crystal of T2BTO is monoclinic, space group C2/c with crystal parameters of a=15.2410(12) Å, b=10.5185(8) Å, c=7.7546(7) Å, V=1221.26(18) Å 3, ρ=1.688 g·cm-3, Z=8. Its thermal decomposition temperature on DSC curve at 10 K·min-1 is 519.9 K, there is only one stage on TG curve with a mass loss of 90.8 % between 453.2 K and 523.2 K, revealing a better thermal stability. EK=144.39 kJ·mol-1, EO=145.52 kJ·mol-1, ln(A/s-1)=32.99, H50>61.0 cm, D=7579 m·s-1, p=24.49 GPa.

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引用本文

尚宇,金波,刘强强,等.5,5′-联四唑-1,1′-二氧-1,2,4-三氮唑含能离子盐的合成、表征及热行为[J].含能材料, 2016, 24(10):953-959. DOI:10.11943/j. issn.1006-9941.2016.10.005.
SHANG Yu, JIN Bo, LIU Qiang-qiang, et al. Synthesis, Characterizations and Thermal Behavior of Bis-1,2,4-triazolium 1H, 1′H -5,5′-bistetrazole-1,1′-diolate[J]. Chinese Journal of Energetic Materials, 2016, 24(10):953-959. DOI:10.11943/j. issn.1006-9941.2016.10.005.

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  • 收稿日期: 2016-03-18
  • 最后修改日期: 2016-04-12
  • 录用日期: 2016-04-27
  • 在线发布日期: 2016-10-08
  • 出版日期: 2016-10-14