氯丙基三苯乙炔基硅烷的制备及其固化分析

Preparation and curing kinetics analysis of CPTPES

以苯乙炔、镁条、氯丙基三氯硅烷和溴乙烷为原料,通过Grignard反应成功制备氯丙基三苯乙炔基硅烷(CPTPES)单体。利用傅里叶变换红外光谱仪和核磁共振波谱仪(1H-NMR、13C-NMR)对单体进行结构表征;通过差示扫描量热仪(DSC)确定单体的固化工艺,采用Kissinger法、Ozawa法、Flynn-Wall-Ozawa法和Friedman法探究单体的固化特性,并预测固化反应机理。实验结果表明:CPTPES的熔点为75℃,反应活化能Ea为146.75kJ/mol,指前因子lnA为26.33,反应级数m为0.47,n为1.61,固化机理与自催化反应机理相符。

Chloropropyl(triphenylethynyl)silane(CPTPES)monomer was synthesized via Grignard reaction of phenylacetylene,magnesium,chloropropyltrichlorosilane and ethylbromide.Its chemical structure was characterized by Fourier transform infrared spectroscopy(FT-IR)and nuclear magnetic resonance spectroscopy(1H-NMR,13C-NMR).Its curing process was obtained by differential scanning calorimetry(DSC)and the curing kinetic parameters were discussed by four well-known kinetic methods,i.e.,Kissinger,Ozawa,Flynn-Wall-Ozawa and Friedman methods.Results shown that the melting was 75℃,the reaction activation energy Ea was 146.75 kJ/mol,the pre-exponential factor lnA was 26.33 and the reaction order m and n were 0.47 and 1.61 respectively.The curing mechanism was in accordance with autocatalytic reaction.