苯酚-亚联苯型环氧树脂的合成及其在环氧模塑料中的应用

Synthesis of Epoxy Resin with Biphenylene Structure and Its Application in Epoxy Molding Compound

以自制苯酚-亚联苯型酚醛树脂、环氧氯丙烷为主要原料,采用固体碱作为醚化阶段催化剂,合成了一种苯酚-亚联苯型环氧树脂。借助红外光谱(FTIR)、核磁共振光谱(1 H NMR和13C NMR)、凝胶渗透色谱(GPC)分别对产物的结构、组成和分子量进行了表征,结果成功制备了苯酚-亚联苯型环氧树脂,相对分子质量为870,环氧当量为274g/eq。此外,将所得苯酚-亚联苯型环氧树脂用于环氧模塑料中,并与市售环氧树脂所得的模塑料进行比较,借助热失重分析仪(TGA)、热机械分析仪(TMA)等对模塑料的主要性能进行研究,结果表明含有苯酚-亚联苯型环氧树脂的模塑料具有较长的凝胶时间和流动长度,具有较高的Tg(142℃)以及较高的初始降解温度(413℃),完全可以满足无铅焊料的加工工艺要求,并具有较好的弯曲强度和弯曲模量。

Epoxy resin with biphenylene structure was synthesized by the reaction between elf-prepared phe- nol-biphenylene resin and epichlorohydrin using solid sodium hydroxide as etherization catalyst. The prod- uct was characterized by Fourier Transform Infrared Spectroscopy（FTIR）, Nuclear Magnetic Resonance Spectroscopy （1H NMR and laC NMR） and Gel Permeation Chromatography（GPC）, respectively, and the results showed that phenol-biphenylene epoxy resin was successfully synthesized, and its molecular weight was 870 as well as the epoxy equivalent 274g/eq. Furthermore, the epoxy resin with biphenylene structure was applied in epoxy molding compound （EMC）, and the curred EMC was characterized by thermogravitric analyzer（TGA）, thermomechanical analyzer （TMA）, and electronic universal testing ma- chine, respectively. Compared with the commercial epoxy resins, the EMC containing self-prepared epoxy resin with biphenylene structure showed longer gelation time and flowing length, and had higher Tg （142℃）and initial degradation temperature （413℃）, which can meet the processing requirement of lead- free solder. Additionally, the EMC had better flexural strength and flexural modulus.