Synthesis and Thermal Properties of Ethynyl Phenyl Azo Phenol-biphenylene Resin
Synthesis and Thermal Properties of Ethynyl Phenyl Azo Phenol-biphenylene Resin
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DOI：
10.1021/acsomega.8b01590
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发表时间：
2019-01-01
期刊：
影响因子：
4.1
通讯作者：
Gu, Xiaohong
中科院分区：
文献类型：
--
作者：
Li, Zhihua;Li, Yujing;Gu, Xiaohong
通过重氮偶联反应在联苯酚醛树脂（BN）上引入乙炔基苯基，合成了一种新型加成固化乙炔基苯基偶氮苯酚-联苯树脂（EPABN）。提出了其合成反应和固化机理。傅里叶变换红外光谱和核磁共振氢谱分析表明，乙炔基苯基基团成功地连接到BN分子链上。通过差示扫描量热分析，确定EPABN树脂的固化过程为150 ℃/2 h + 172 ℃/2 h + 203 ℃/4 h + 255 ℃/4 h + 300 ℃/4 h。凝胶渗透色谱和元素分析表明，乙炔基苯基的引入提高了EPABN的数均分子量和重均分子量。热重分析表明，在最佳工艺条件下合成的EPABN树脂具有优异的耐热性、耐烧蚀性和力学性能。固化的EPABN树脂的耐热性的TdS和T-d（10）分别为463和531 ℃，并且其在700和1000 ℃下的残炭率分别为78.2%和72.1%。
A novel addition curing ethynyl phenyl azo phenol- biphenylene resin (EPABN) was synthesized by introducing ethynylphenyl group into biphenyl novolac resin (BN) through diazo coupling reaction. Its synthesis reaction and curing mechanism were also proposed. Fourier transform infrared spectroscopy and H-1 NMR spectroscopic analysis showed that the ethynylphenyl group was successfully linked to the BN molecular chain. By differential scanning calorimetry analysis, the curing process of EPABN resin was determined to be 150 degrees C/2 h + 172 degrees C/2 h + 203 degrees C/4 h + 255 degrees C/4 h + 300 degrees C/4 h. Gel permeation chromatography and elemental analysis showed that the introduction of ethynylphenyl group increased the numberaverage molecular weight and weight- average molecular weight of EPABN. Thermogravimetric analysis showed that the EPABN resin synthesized under the obtained optimum conditions has excellent heat resistance, ablation resistance, and mechanical properties. TdS and T-d(10) of heat resistance of the cured EPABN resin are 463 and 531 degrees C, respectively, and its residual char yield at 700 and 1000 degrees C is 78.2% and 72.1%, respectively.