间乙炔基苯偶氮联苯酚醛树脂的合成及性能

Synthesis and Properties of m-Ethynylbenzene Azobiphenyl Phenolic Resin

通过重氮偶合反应在联苯酚醛树脂(BN)中引入乙炔基苯基,合成了新型的加成固化型间乙炔基苯偶氮联苯酚醛树脂(EPABN)。采用傅里叶变换红外光谱、聚合物称量、流变测试、差示扫描量热分析(DSC)、热重分析和吸附法等表征了EPABN的结构、溶解性能、流变性能、热性能及树脂炭化产物的致密性。溶解性能测试表明,EPABN树脂能溶于丙酮、四氢呋喃等溶剂。流变性能测试表明,EPABN树脂在120~150℃有1个低黏度加工窗口。DSC结果分析表明,EPABN可行的固化工艺为140℃/2 h+161℃/2 h+192℃/4 h+231℃/4 h+280℃/4 h。EPABN树脂的T_(d)^(5)和T_(d)^(10)分别为479.7℃和545.1℃,700℃和1000℃的残碳率分别为80.96%和77.26%。树脂炭化产物的氮吸附测试及密度测试表明,随着炭化温度升高,炭化物的致密度和炭化密度均增加。EPABN固化物具有优异的热稳定性、高残碳率及碳化物具高致密性。

A addition-curing m-ethynylbenzene azobiphenyl phenolic resin(EPABN)was synthesized from biphenol phenolic resin(BN).The structure,dissolution properties,rheology,thermal properties and density of the EPABN were characterized by Fourier infrared spectroscopy(FT-IR),polymer weighing,rotating rheometer,differential scanning calo-rimeter(DSC),thermogravimetry(TG)and adsorption instrument.The solubility research shows that EPABN resin is soluble in acetone,tetrahydrofuran et al.The rheological test studies show that the EPABN resin has a low viscosity processing window at 120~150℃.DSC results show that the feasible curing process of the EPABN is 140℃/2 h+161℃/2 h+192℃/4 h+231℃/4 h+280℃/4 h.The T_(d)^(5)and T_(d)^(10)of the EPABN are 479.7℃,545.1℃,700℃and 1000℃are 80.96%and 77.26%,respectively.The nitrogen adsorption and density of resin carbide products show that the carbide density and carbide density increase as the carbide temperature increases.The results show that EPABN curing material has a excellent heat resistance,high carbon residual rate and high carbon density,and the EPABN is expected as structural and heat resistant material in aviation and aerospace fields.