三炔丙基异氰尿酸酯的合成、表征及其非等温固化动力学

Synthesis,characterization and non-isothermal curing kinetics of tri-propargyl isocyanurate

以3-溴丙炔、异氰尿酸为原料,利用相转移催化剂合成了三炔丙基异氰尿酸酯(TPIC),并用FT-IR、1 H NMR对其结构进行了表征。用TGA表征了热固化后的TPIC的热性能。结果表明:热固化后的树脂在375℃开始分解,800℃的残炭率达75%。根据DSC曲线,TPIC的熔点为167℃左右,并用Kissinger、Flynn-Wall-Ozawa和Friedman-Reich-Levi法分别计算了热固化反应活化能,它们分别为46.81、48.70和40.92kJ.mol-1,热固化反应级数都接近1,并探讨了固化反应过程与机理。通过对比分析表明,这3种方法均适用于TPIC体系。

Tri-propargyl isocyanurate（TPIC）was synthesized using isocyanurate and propargyl bromide by phase transfer catalyst reaction.The chemical structure of TPIC was characterized by FT-IR,1H NMR.The analysis of TGA curve referred to the cured TPIC displayed that the preliminary thermal decomposition temperature of cured TPIC was about 375℃ and the char yield was 75% at 800℃.According to DSC curves used to investigate the thermal curing behavior of TPIC,the curing kinetic parameters were calculated by several thermo analysis methods,respectively,such as Kissinger,Flynn-Wall-Ozawa and Friedman-Reich-Levi,and the apparent activation energy was 46.81,48.70 and 40.92 kJ·mol-1 respectively.The order of curing reaction obtained by the three methods all approached 1 and the mechanism was further discussed.Based on comparative analysis of the above three methods,they all can properly simulate the thermal curing process of TPIC.