物理化学学报 >> 2008, Vol. 24 >> Issue (12): 2263-2267.doi: 10.3866/PKU.WHXB20081219

研究论文 上一篇    下一篇

3-硝基邻苯二甲酸锆的制备﹑热分解机理及非等温反应动力学

张衡, 赵凤起, 仪建华, 张晓宏, 胡荣祖, 徐司雨, 任晓宁   

  1. 西安近代化学研究所, 西安 710065
  • 收稿日期:2008-08-01 修回日期:2008-09-18 发布日期:2008-12-04
  • 通讯作者: 赵凤起 E-mail:npecc@163.com

Preparation, Thermal Behavior and Non-isothermal Decomposition Reaction Kinetics of Zr(3-NO2-PHT)2·2H2O

ZHANG Heng, ZHAO Feng-Qi, YI Jian-Hua, ZHANG Xiao-Hong, HU Rong-Zu, XU Si-Yu, REN Xiao-Ning   

  1. Xi’an Modern Chemistry Research Institute, Xi’an 710065, P. R. China
  • Received:2008-08-01 Revised:2008-09-18 Published:2008-12-04
  • Contact: ZHAO Feng-Qi E-mail:npecc@163.com

摘要: 用3-硝基邻苯二甲酸、氢氧化钠和硝酸氧锆为原料, 制备了3-硝基邻苯二甲酸锆, 采用元素分析、X射线荧光衍射和FT-IR对其结构进行了表征. 用TG-DTG以及变温固相原位反应池/傅里叶变换红外光谱(RSFT-IR)联用技术研究了3-硝基邻苯二甲酸锆的热分解机理, 对主分解反应的DTG峰进行了数学处理, 计算得到了动力学参数和动力学方程. 结果表明, 3-硝基邻苯二甲酸锆的分解反应总共有4个阶段, 其中主分解反应发生在第2阶段, 主分解反应的表观活化能Ea与指前因子A分别为158.84 kJ·mol-1和109.85 s-1, 主分解阶段的反应机理服从一级Mample法则, 主分解反应的动力学方程为dα/dt=109.85(1-α)e-1.91×104/T.

关键词: 3-硝基邻苯二甲酸锆, 热分解机理, 非等温反应动力学

Abstract: Zirconium 3-nitrophthalate (Zr(3-NO2-PHT)2·2H2O) was synthesized using 3-nitrophthalic acid, sodium hydroxide, and zirconyl nitrate as raw materials. Its structure was determined by elemental analysis, X-ray fluorescence and FT-IR spectra. The thermal decomposition mechanism and kinetic parameters of the decomposition reaction for Zr(3-NO2-PHT)2·2H2O were investigated by temperature-programmed TG-DTG and condensed-phase thermolysis/FT-IR techniques. A kinetic equation for the decomposition reaction was obtained. The results showed that Zr(3-NO2-PHT)2·2H2O underwent a four-stage decomposition process and that the main decomposition reaction occurred during the second process. The apparent activation energy (Ea) and pre-exponential factor (A) of the main decomposition reaction are 158.84 kJ·mol-1 and 109.85 s-1, respectively. The kinetic equation can thus be expressed as: dα/dt=109.85(1-α)e-1.91×104/T.

Key words: Zr(3-NO2-PHT)2·2H2O, Thermal decomposition mechanism, Nonisothermal reaction kinetics

MSC2000: 

  • O643