基于甲基三苯乙炔基硅烷的新型聚三唑树脂的制备与性能

首先采用格氏试剂法合成了甲基三苯乙炔基硅烷(MTPES),通过傅里叶变换红外光谱(FT-IR)、核磁共振氢谱(1 H-NMR)对其结构进行了表征。然后以MTPES和4,4’-二叠氮甲基联苯(BAMBP)为原料制备了新型聚三唑树脂(MPTA)。利用FT-IR和差示扫描量热(DSC)研究了MPTA树脂的固化行为,通过动态力学热分析(DMA)和热重分析(TG)研究了炔基与叠氮基配比对树脂热性能的影响,并通过测试凝胶时间随贮存时间的变化研究了树脂及其四氢呋喃(THF)溶液的贮存稳定性。结果表明,固化后的树脂玻璃化转变温度(Tg)达到236℃,在氮气中的5%热失重温度(T_(d5))在320℃左右。MPTA树脂在35℃和25℃下分别贮存7d和20d后,100℃下树脂的凝胶时间分别为40min和25min,MPTA树脂的THF溶液在同样条件下贮存28d后,凝胶时间分别为54min和61min,具有比现有聚三唑树脂更好的贮存稳定性。单向T700碳纤维-MPTA复合材料常温下的弯曲强度为1 660 MPa,弯曲模量为129 GPa,150℃下的弯曲强度保留率为70%。

Preparation and Properties of a Novel Polytriazole Resin Based on Methyl Tri(phenylethynyl) Silane

Methyl-tri (phenylethynyl) silane(MTPES) was first synthesized with ethyl bromide, methyl trichlorosilane, and phenyl acetylene by Grignard reaction and characterized by Fourier Transform-Infrared spectroscopy(FT-IR) and Nuclear Magnetic Resonance spectroscopy(1H-NMR).A novel polytriazole(MPTA) resin was further synthesized from 4,4''-biphenyl dibenzyl azide(BAMBP) and MTPES via 1,3-dipolar cycloaddition.The curing behaviors of the resin were traced by FT-IR and Differential Scanning Calorimeter(DSC).The effects of mole ratio of monomers on thermal properties of MPTA resin were studied by the Dynamic Thermo Mechanical analysis (DMA) and Thermogravimetric analysis (TG).The storage stability of the resin and tetrahydrofuran (THF) solution was studied by measuring the gel time and the storage time.The results show that the glass transition temperature (Tg) and 5% mass loss temperature (Td5) of a cured MPTA resin reached 236 ℃ and 320 ℃ in nitrogen atmosphere, respectively.After 28 d storage of MPTA resin solution at 35 ℃ and 25 ℃, the gel time of the resin is still 54 min and 61 min at 100 ℃, respectively.MPTA resin stored for 7 d and 20 d under the same conditions, the gel time is still 40 min and 25 min, respectively, which is better than the existing polytriazole in storage stability.Unidirectional T700 carbon fiber reinforced MPTA composite (T700-MPTA) was prepared through compression molding.The composite has good mechanical property, and the bending strength of T700-MPTA composite achieve to 1 660 MPa.The retention rate of bending strength is 70% at 150 ℃.