K(FOX-7)·H2O的合成、晶体结构和热行为

高等学校化学学报 ›› 2010, Vol. 31 ›› Issue (4): 638.

K(FOX-7)·H₂O的合成、晶体结构和热行为

徐抗震¹, 左现刚², 宋纪蓉^1,3, 王锋¹, 黄洁¹, 常春然¹

1. 西北大学化工学院, 西安 710069;
2. 河南科技学院信息工程学院, 新乡 453003;
3. 故宫博物院文保科技部, 北京 100009

收稿日期:2009-09-02 出版日期:2010-04-10 发布日期:2010-04-10
通讯作者: 徐抗震, 男, 博士, 副教授, 主要从事新型含能材料研究. E-mail: xukz@nwu.edu.cn
基金资助:
国家自然科学基金(批准号: 20803058)、陕西省自然科学基金(批准号: SJ08B10)、总装备部武器装备预研基金(批准号: 9140C3503010905)和西北大学研究生创新基金(批准号: 09YSY25)资助.

Preparation, Crystal Structure and Thermal Behavior of K(FOX-7)·H2O

XU Kang-Zhen^1*, ZUO Xian-Gang², SONG Ji-Rong^1,3, WANG Feng¹, HUANG Jie¹, CHANG Chun-Ran¹

1. School of Chemical Engineering, Northwest University, Xi′an 710069, China;
2. College of Information Engineering, Henan Institute of Science and Technology, Xin′xiang 453003, China;
3. Conservation Technology Department, the Palace Museum, Beijing 100009, China

Received:2009-09-02 Online:2010-04-10 Published:2010-04-10
Contact: XU Kang-Zhen. E-mail: xukz@nwu.edu.cn
Supported by:
国家自然科学基金(批准号: 20803058)、陕西省自然科学基金(批准号: SJ08B10)、总装备部武器装备预研基金(批准号: 9140C3503010905)和西北大学研究生创新基金(批准号: 09YSY25)资助.

摘要/Abstract

摘要：

利用1,1-二氨基-2,2-二硝基乙烯(FOX-7)和KOH在甲醇水体系中合成了一种新型有机钾盐, 并培养出K(FOX-7)·H₂O单晶. 该晶体属三斜晶系, P1空间群, 晶胞参数: a=0.7493(2) nm, b=0.9767(3) nm, c=2.0035(5) nm, α=90.017(4)°, β=97.129(4)°, γ=90.019(4)°, V=1.4548(7) nm³, D_c=1.865 g/cm³, μ=0.724 mm^-1, F(000)=832, Z=8, R₁=0.0523, wR₂=0.1082. K(FOX-7)·H₂O的热分解行为可分为一个脱水和两个放热分解过程, 且第一放热分解反应的表观活化能和指前因子分别为135.9 kJ/mol和1012.17 s^-1. 热爆炸的临界温度为212.02 ℃. 同时, 利用微量热法测定了K(FOX-7)·H₂O的比热容, 298.15 K时的摩尔热容为210.88 J·mol^-1·K^-1. 用测得的比热容方程计算了298.15 K为基础的FOX-7的热力学函数, 并得到了绝热至爆时间为15.7~16.8 s之间的某一值.

关键词: 1,1-二氨基-2,2-二硝基乙烯(FOX-7); 钾盐; 晶体结构; 热行为; 绝热至爆时间

Abstract:

A high-energy organic potassium salt of 1,1-diamino-2,2-dinitroethlyene(FOX-7) was synthesized by mixing FOX-7 and KOH in water-methanol system. Crystal structure of K(FOX-7)·H₂O was determined by X-ray diffraction analysis. The crystal belongs to triclinic crystallographic system, space group P1 and cell parameters: a=0.7493(2) nm, b=0.9767(3) nm, c=2.0035(5) nm, α=90.017(4)°, β=97.129(4)°, γ=90.019(4)°, V=1.4548(7) nm³, D_c=1.865 g/cm³, μ=0.724 mm^-1, F(000)=832, Z=8, R₁=0.0523, wR₂=0.1082. The thermal behavior of K(FOX-7)·H₂O was studied, and the apparent activation energy and pre-exponential factor of the second decomposition reaction are 135.9 kJ·mol^-1 and 1012.17s^-1, respectively. The critical temperature of thermal explosion is 212.02 ℃. The specific heat capacity of K(FOX-7)·H₂O was determined with micro-DSC method, and the molar heat capacity is 210.88 J·mol^-1·K^-1at 298.15 K. Thermodynamic functions of K(FOX-7)·H₂O, relative to the standard temperature 298.15K, were calculated through thermodynamic relationship, and the adiabatic time-to-explosion also was obtained as a certain value between 15.7—16.8 s.

Key words: 1,1-Diamino-2,2-dinitroethlyene(FOX-7); Potassium salt; Crystal structure; Thermal behavior; Adiabatic time-to-explosion

TrendMD:

徐抗震, 左现刚, 宋纪蓉, 王锋, 黄洁, 常春然. K(FOX-7)·H₂O的合成、晶体结构和热行为. 高等学校化学学报, 2010, 31(4): 638.

XU Kang-Zhen*, ZUO Xian-Gang, SONG Ji-Rong, WANG Feng, HUANG Jie, .... Preparation, Crystal Structure and Thermal Behavior of K(FOX-7)·H2O. Chem. J. Chinese Universities, 2010, 31(4): 638.

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K(FOX-7)·H₂O的合成、晶体结构和热行为

Preparation, Crystal Structure and Thermal Behavior of K(FOX-7)·H2O

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