双酚芴双胺型苯并嗯嗪树脂的合成、结构及热性能

以9-芴酮、苯酚为原料,以质量分数为98%的浓硫酸为催化剂,2-巯基丙酸为助催化剂,合成了双酚芴[9,9-双(4-羟苯基)芴],再用其与乙二胺和多聚甲醛反应,合成了线性双酚芴双胺型苯并噁嗪树脂(BF-eda树脂).采用FTIR,'H NME和<'13>C NMR等分析手段对双酚芴和BF-eda树脂的化学结构进行了表征;...

Synthesis, Structure and Thermal Properties of Bisphenol Fiuorene Diamine Benzoxazine

9,9-bis(4-hydroxyphenyl)-fluorene (Bisphenol Fluorene，BHPF) was synthesized from phenol and 9-fluorenone using 98% sulfuric acid as catalyst and 2-mercaptopropionic as promoter, and then a liner BHPF-diamine benzoxazine (BF-eda resin) was synthesized using BHPF, ethylenediamine and paraformaldehyde. Chemical structure of the BF-eda resin were verified by Fourier transform infrared spectroscopy (FT-IR), 1H and 13C nuclear magnetic resonance spectroscopies(NMR). The GPC analysis presents the number average molecular weight of BF-eda resin is 4690，and the polydispersity index (PDI) is 2.93. The curing behavior of BF-eda resin was studied by differential scanning calorimetry (DSC) and the thermal stabilization of polybenzoxazine was evaluated with thermogravimetric analysis (TGA).The ring-opening polymerization temperature of BF-eda resin is about 253℃, the thermal decomposition temperature of polybenzoxazine is 344℃, the temperature at 5% weight loss is 357℃, and the char yield ratio is 51% at 900℃.