酚酞型氰酸酯的合成与表征

Synthesis and characterization of phenolphthalein cyanate ester

采用卤化氰-酚合成法制备了酚酞型CE(氰酸酯),并采用红外光谱(FT-IR)法、质谱法、核磁共振氢谱(1H-NMR)法、毛细管法和差示扫描量热(DSC)法等对酚酞型CE的结构和性能进行了表征和分析,同时对其热性能和热解动力学行为进行了研究。结果表明:酚酞型CE的合成条件为"-15℃搅拌反应1 h→升温至5℃搅拌反应4 h→5℃保温反应2 h";目标产物失重5%温度为435℃,最大失重速率温度为453℃,表观活化能为222.49 kJ/mol,指前因子为1013.97s-1;将酚酞型CE加入到胶粘剂的基础配方中,相应胶粘剂的综合性能略高于基础配方胶粘剂。

The phenolphthalein CE （cyanate ester） was prepared by halogenated cyanide-phenol synthesis method,and its structure and properties were characterized and analysed by FT-IR （infrared spectroscopy）, mass spectrum, proton nuclear magnetic resonance spectroscopy （IH-NMR）, capillary method, DSC （differential scanning calorimetry） and other methods, at one time,the thermal property and pyrolysis-kinetic behavior of phenolphthalein CE were investigated. The results showed that the synthesis conditions of phenolphthalein CE were ＂mix round and reaction at -15 ℃ for 1 h--mix round and reaction at 5 ℃ for 4 h→reaction at 5℃ for 2 h. The 5% weight loss temperature,maximal weight loss rate temperature,apparent activation energy and pre-exponential factor of target product were 435℃ ,453℃ ,222.49 kJ/mol and 10^13＇97 s-1 respectively. The combination property of corresponding adhesive made from basic formula and phenolphthalein CE ,was slightly higher than those of adhesive made from basic formula.