十二烷基芳炔硅烷单体的合成及固化动力学研究  

Synthesis and Curing Kinetics of Dodecyl-tri (phenylethynyl) Silane Monomer

作　　者：汪猛[1] 疏瑞文[1] 谭德新[1] 徐远[1] WANG Meng;SHU Rui-wen;TAN De-xin;XU Yuan(School of Chemical Engineering,Anhui University of Science ＆ Technology,Huainan 232001,China)

机构地区：[1]安徽理工大学化学工程学院,安徽淮南232001

出　　处：《合成化学》2018年第8期582-586,共5页Chinese Journal of Synthetic Chemistry

基　　金：国家自然科学基金资助项目(51507003);安徽理工大学博士启动基金资助项目(ZY537)

摘　　要：以十二烷基三氯硅烷、镁条、溴乙烷和苯乙炔为原料,通过格利雅反应首次合成了十二烷基三苯乙炔基硅烷单体(DTPES),其结构经~1H NMR,^(13)C NMR,^(29)Si NMR和FT-IR表征。采用非等温差示扫描量热法(DSC)对单体的热固化动力学进行了研究,并运用Kissinger、Ozawa和Flynn-Wall-Ozawa法计算了DTPES的固化反应活化能,Friedman法推测了固化机理和固化动力学模型。结果表明:DTPES的固化过程符合自催化动力学模型。固化反应的表观活化能为160.10 k J·mol^(-1),反应级数n和m的平均值分别为0.83和0.30,指前因子lnA平均值为29.48 s^(-1)。Dodecyl-tri（ phenylethynyl） silane monomer（ DTPES） was synthesized for the first time by Grignard reaction,using dodecyltrichlorosilane,magnesium rod,ethyl bromide and phenylacetylene as materials. The structure was characterized by ~1H NMR,^（13）C NMR,^（29）Si NMR and FT-IR. The thermal curing kinetics of DTPES was studied by non-isothermal differential scanning calorimetry（ DSC）. The activation energy of curing reaction was analyzed by the Kissinger,Ozawa and Flynn-Wall-Ozawa methods. The curing mechanism and curing kinetics model were speculated by the Friedman method. The results showed that the curing process of DTPES followed the autocatalytic kinetic model. The average activation energy was 160. 10 k J·mol^（-1） and the reaction orders n,m and per-exponential factor ln A were 0. 83,0. 30 and 29. 48 s^（-1）,respectively.

关 键 词：十二烷基三苯乙炔基硅烷 格利雅反应 合成 固化机理 固化动力学 

分 类 号：TQ322.4[化学工程—合成树脂塑料工业] O62[理学—有机化学]