三(3-乙炔基苯胺)-苯基硅烷改性含硅芳炔树脂的性能

摘要

以苯基三氯硅烷、3-氨基苯乙炔为原料,通过胺解反应合成了三(3-乙炔基苯胺)苯基硅烷(SZTA),并通过傅里叶变换红外光谱(FT-IR)和核磁共振氢谱(1H-NMR)表征了其结构.随后通过熔融共混的方法制备了不同配比的改性含硅芳炔树脂(PSA/SZTA),借助黏度计、流变仪、差示扫描量热仪(DSC)、电子万能试验机、热重分析仪(TG)等考察了改性树脂的工艺性能、固化特性、弯曲性能、热稳定性能和热解动力学等.结果显示,引入SZTA后,改性PSA树脂的黏度降低62%;改性PSA树脂固化物的弯曲强度最高达到34.6 MPa,比未改性的PSA树脂提高了约54%;且改性树脂固化物在N2中的5%热失重温度(Td5)均高于500 ℃,保持了良好的耐热性能;PSA/SZTA-20固化物的热解表观活化能(Ea)的平均值为249 kJ/mol.%Tri(3-acetylenephenylamino)phenylsilane (SZTA) was synthesized by aminolysis reaction using phenyl trichlorosilane and 3-aminophenylacetylene as raw materials.The structure of SZTA was characterized by Fourier Transform Infrared spectroscopy (FT-IR) and proton Nuclear Magnetic Resonance spectroscopy (1H-NMR).The modified resins (PSA/SZTA) were prepared by melt blending silicon-containing arylacetylene (PSA) resin and SZTA in different ratios.The properties of the modified resins such as the process property,curing reaction,flexural property, thermal stability,and the pyrolysis dynamics were investigated by viscometer, rheometer, Differential Scanning Calorimetry (DSC),electronic universal testing machine, and Thermogravimetric analysis (TG).The results show that the viscosity of the modified PSA resin decreases by 62% after introducing SZTA.The flexural strength of the cured PSA/SZTA is up to 34.6 MPa,higher than that of PSA by 54%.The modified PSA resins maintain good heat resistance as the degradation temperatures at 5% mass loss (Td5) in N2 is above 500 ℃.The average degradation apparent activation energy (Ea) of the cured PSA/SZTA-20 is 249 kJ/mol based on Ozawa method.