高纯和低可水解氯含量环氧树脂的制备

Preparation of High Pure Epoxy Resin with Low Hydrolyzable Chlorinity Content

以双酚A和环氧氯丙烷为原料,通过两步法制备了液态双酚A型环氧树脂,再与NaH反应进行后处理精制,除去环氧树脂的可水解氯,制得高纯、低可水解氯含量的环氧树脂;考察了溶剂种类及其用量、NaH用量、反应时间等工艺条件对环氧树脂性能的影响。实验结果表明,在同样溶剂用量的情况下,以四氢呋喃(THF)为溶剂比以二氧六环和乙醚为溶剂的脱氯效果好;随THF用量的增加,可水解氯含量降低,环氧基团含量基本不变;在无水THF的用量为200mL、NaH用量为0.12g、反应时间为3.5h的条件下,所得环氧树脂中可水解氯的质量分数低于0.005%,达到微电子工业的使用要求。

Epoxy resins with low hydrolyzable chlorinity content for usage in microelectronic equipments were prepared from bisphenol A and epichlorohydrin by using a two - step - reaction first and then by post - treating with sodium hydride to remove hydrolyzable chlorine. Effects of solvent type, sodium hydride dosage, and reaction time on hydrolyzable chlorine content in epoxy resin were studied. Tetrahydrofuran （THF）was a better solvent than dioxane and diethyl ether for removing hydrolyzable chlorine from the resin. Hydrolyzable chlorine content in the resin decreased with increasing of Nail dosage, while epoxide content remained unchanged. Mass fraction of hydrolyzable chlorine in epoxy resin could be reduced to lower than 0.005% under optimal conditions： reaction time 3.5 h. Nail 0.12 g and THF without water 200 mL.