Synthesis, crystal structure and thermal behavior of 4-amino-3,5-dinitropyrazole potassium salt
Synthesis, crystal structure and thermal behavior of 4-amino-3,5-dinitropyrazole potassium salt
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4-氨基-3,5-二硝基吡唑钾盐的合成、晶体结构及热行为
DOI：
10.1016/j.ica.2013.03.005
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发表时间：
2013-08-24
影响因子：
2.8
通讯作者：
An, Ting
中科院分区：
文献类型：
--
作者：
Wang, Ying-Lei;Zhao, Feng-Qi;An, Ting
首次合成了一种新型含能阻燃剂4-氨基-3,5-二硝基吡唑钾盐(ADNPK)，收率86.26%。通过IR和元素分析证实了ADNPK的结构。通过单晶X射线衍射仪测定了ADNPK的晶体结构。它在单斜晶系中结晶，空间群 P2(1)/n，晶体参数 a = 12.706(3) 埃，b = 9.3334(18) 埃，c = 13.792(3) 埃，beta = 102.513(3) 度，V = 1596.8(5) 埃(3)，Z = 2，mu = 0.675 mm(-1)，F(000) = 928，D-calc = 1.907 g cm(-3)。利用差示扫描量热法(DSC)研究了ADNPK的热行为和非等温分解反应动力学。采用基辛格法得到ADNPK放热分解反应的表观活化能和指前因子分别为2373 kJ mol(-1)和10(18.74) s(-1)。 ADNPK放热分解反应的机理方程为：d alpha/dT = 10(18.74)/beta 2(1 - alpha)(3/2) exp(-2.37310(5)/RT) (C) 2013 Elsevier B.V. 版权所有。
A novel energetic flame suppressant, 4-amino-3,5-dinitropyrazole potassium salt (ADNPK), was firstly synthesized with a yield of 86.26%. The structure of ADNPK was confirmed by IR and elemental analysis. The crystal structure of ADNPK was determined by single crystal X-ray diffractometer. It crystallizes in a monoclinic system, space group P2(1)/n with crystal parameters a = 12.706(3) angstrom, b = 9.3334(18) angstrom, c = 13.792(3) angstrom, beta = 102.513(3)degrees, V = 1596.8(5) angstrom(3), Z = 2, mu = 0.675 mm(-1), F(000) = 928, and D-calc = 1.907 g cm(-3). The thermal behavior and non-isothermal decomposition reaction kinetics of ADNPK were studied by means of Differential Scanning Calorimetiy (DSC). The apparent activation energy and pre-exponential factor of the exothermic decomposition reaction of ADNPK obtained by the Kissinger method are 2373 kJ mol(-1) and 10(18.74) s(-1). And the mechanism equation for the exothermic decomposition reaction of ADNPK is:d alpha/dT = 10(18.74)/beta 2(1 - alpha)(3/2) exp(-2.37310(5)/RT) (C) 2013 Elsevier B.V. All rights reserved.