文献类型：期刊文献

中文题名：全内炔型含硅聚三唑树脂的制备与性能

英文题名：Preparation and Properties of Total Internal Acetylene Silicon-Containing Polytriazole Resin

作者：李圆梦[1];万里强[1];舒达[1];罗文梅[1];黄发荣[1]

机构：[1]华东理工大学特种功能高分子材料及相关技术教育部重点实验室,上海200237

年份：2019

卷号：32

期号：3

起止页码：360

中文期刊名：功能高分子学报

外文期刊名：Journal of Functional Polymers

收录：CSTPCD;;北大核心:【北大核心2017】；CSCD:【CSCD_E2019_2020】；

基金：中央高校基本科研业务费专项资金(222201717001)

语种：中文

中文关键词：聚三唑;热性能;贮存稳定性;复合材料

外文关键词：polytrizole;thermal properties;storage stability;composite material

摘要：采用格氏试剂法制备了苯乙炔封端型含硅芳炔(PTPSA),并采用傅里叶转换红外光谱(FT-IR)、核磁共振氢谱(~1 H-NMR)和差示扫描量热法(DSC)表征了其结构。以PTPSA和1,3,5-三叠氮甲基-2,4,6-三甲基苯(TAMIMB)为原料,制备了新型全内炔型含硅聚三唑树脂(P-PTA3)。利用FT-IR、DSC、动态力学分析(DMA)和热重分析(TGA)研究了树脂的固化行为及热性能,通过测试凝胶时间随贮存时间的变化研究了树脂溶液的贮存稳定性。结果表明:树脂固化物的玻璃化转变温度(Tg)可达304℃,失重率5%时的温度(Td5)达330℃以上。P-PTA3树脂溶液在35℃和25℃下贮存时间分别超过20d和40d。单向碳纤维T700/P-PTA3复合材料常温下的弯曲强度为1 875MPa,弯曲模量为135.5GPa,180℃下弯曲强度保留率为75%。
Silicon-containing arylacetylene terminated by phenylacetylene (PTPSA) was synthesized by Grignard reaction, and the molecular structure was characterized and confirmed by Fourier transform-infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy ( 1H-NMR) and differential scanning calorimeter (DSC). A novel polytriazole (P-PTA3) resin was further synthesized through 1,3-dipolar cycloaddition reaction between PTPSA and 1,3,5-tris(azidomethyl)-2,4,6-trimethylbenzene (TAMTMB). The unidirectional T700 carbon fiber reinforced P-PTA3 resin composite (T700/P-PTA3) was prepared by compression molding. The curing behaviors of the resin were monitored by FT-IR and DSC. The effects of molar ratio of monomers on the thermal properties of P-PTA3 resin were studied by dynamic thermos mechanical analysis (DMA) and thermogravimetric (TG) analysis. The storage stability of the resin and its tetrahydrofuran(THF) solution were evaluated by measuring the variation of the gel time against storage time. The gel time was measured under 90 ℃. The results show that the glass transition temperature ( T g) of the cured P-PTA3 resin is 304 ℃ and 5% weight loss temperature ( T d5 ) is 341 ℃ as tested in nitrogen atmosphere (the molar ratio of the alkynyl and triazo is 1.1∶1.0), and T d5 of the samples with different molar ratios of the cured P-PTA3 resins is higher than 330 ℃. The P-PTA3 resin and its THF solution can be stored for more than 20 d and 40 d at 35 ℃ and 25 ℃, respectively. Correspondingly, the gel time of the resins at 90 ℃ is 24 min and 42 min, respectively, which presents a better storage stability than the currently existing polytriazole resin solution at the same storage temperature. The flexural strength and flexural modulus of T700/P-PTA3 composite at room temperature was 1 875 MPa, and 135.5 GPa, respectively, while the retention rate of bending strength was 75% under 180 ℃.