Boonlert-Uthai Tossapol, Samthong Chavakorn, Somwangthanaroj Anongnat
Department of Chemical Engineering, Faculty of Engineering, Chulalongkorn University, Bangkok 10330, Thailand.
Polymers (Basel). 2019 Sep 23;11(10):1545. doi: 10.3390/polym11101545.
The hyperbranched epoxy resins (HBE) composed of bisphenol A (BPA) and polyethylene glycol (PEG) as reactants and pentaerythritol as branching point were successfully synthesized via A + B polycondensation reaction at various BPA/PEG ratios. The C NMR spectra revealed that the synthesized HBE mainly had a dendritic structure as confirmed by the high degree of branching (DB). The addition of PEG in the resin enhanced degree of branching (DB) (from 0.82 to 0.90), epoxy equivalent weight (EEW) (from 697 g eq to 468 g eq) as well as curing reaction. Adding 5-10 wt.% PEG in the resin decreased the onset and peak curing temperatures and glass transition temperature; however, adding 15 wt.% PEG in the resin have increased these thermal properties due to the lowest EEW. The curing kinetics were evaluated by fitting the experimental data of the curing behavior of all resins with the Šesták-Berggren equation. The activation energy increased with the increase of PEG in the resins due to HBE's steric hindrance, whereas the activation energy of HBE15P decreased due to a large amount of equivalent active epoxy group per mass sample. The curing behavior and thermal properties of obtained hyperbranched BPA/PEG epoxy resin would be suitable for using in electronics application.
以双酚A(BPA)和聚乙二醇(PEG)为反应物、季戊四醇为支化点,通过A + B缩聚反应成功合成了不同BPA/PEG比例的超支化环氧树脂(HBE)。碳核磁共振光谱表明,合成的HBE主要具有树枝状结构,这一点通过高支化度(DB)得到了证实。树脂中PEG的加入提高了支化度(DB)(从0.82提高到0.90)、环氧当量(EEW)(从697 g/eq提高到468 g/eq)以及固化反应。在树脂中加入5 - 10 wt.%的PEG降低了起始固化温度、峰值固化温度和玻璃化转变温度;然而,在树脂中加入15 wt.%的PEG由于最低的EEW而提高了这些热性能。通过将所有树脂固化行为的实验数据与Šesták - Berggren方程拟合来评估固化动力学。由于HBE的空间位阻,树脂中随着PEG含量的增加活化能升高,而HBE15P的活化能由于每质量样品中大量的等效活性环氧基团而降低。所获得的超支化BPA/PEG环氧树脂的固化行为和热性能适用于电子应用。