聚正己基三苯乙炔基硅烷树脂的合成及其热稳定性能  

Synthesis and Thermal Stability of N-hexyl-tri(phenylethynyl) Silane

作　　者：汪猛[1] 谭德新[1] 疏瑞文[1] 徐远[1] WANG Meng;TAN De-xin;SHU Rui-wen;XU Yuan(School of Chemical Engineering,Anhui University and 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7期494-497,502,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：以正己基三氯硅烷、镁条、溴乙烷和苯乙炔为原料,通过Grignard反应合成单体正己基三苯乙炔基硅烷(NTPES),其结构经~1H NMR,^(13)C NMR,29Si NMR和FT-IR表征,采用非等温差热扫描量热法(DSC)研究了其热固化行为。通过热聚合合成了聚正己基三苯乙炔基硅烷树脂(PNTPES),运用热重分析(TG)技术研究了固化树脂的热稳定性。结果表明:树脂在氮气气氛中质量损失5%的温度高于445℃,800℃残存率大于60%,具有较好的热稳定性。N-hexyl-tri（phenylethynyl） silane monomer（NTPES） was synthesized by Grignard reaction using n-hexyltrichlorosilane,magnesium rod,ethyl bromide and phenylacetylene as the starting materials. The structure was characterized by^1H NMR,^13C NMR,29 Si NMR and FT-IR. Its thermal curing behavior was studied by non-isothermal differential scanning calorimetry（DSC）. Ploy-N-hexyl-tri（phenylethynyl） silane monomer（PNTPES） was synthesized by thermal polymerization and the thermal stability of resin was studied by thermogravimetric analysis（TG）. The temperature of 5% weight loss was up to 445 ℃ under N2 atmosphere and the residue of resin at 800 ℃ was exceeding 60%. That indicated the resin presented excellent thermal stability.

关 键 词：正己基三苯乙炔基硅烷 Grignard反应 合成 非等温法DSC 固化工艺 热稳定性 

分 类 号：TQ322.41[化学工程—合成树脂塑料工业]