间苯二酚缩甲醛四缩水甘油醚的合成

Synthesis of methylene-bis(1,3-benzenediol)-tetra-glycidyl ether

采用间苯二酚、甲醛合成甲撑二间苯二酚后,再环氧化合成四官能团的甲撑二间苯二酚四缩水甘油醚环氧树脂.研究了不同催化剂用于酚醛缩合、采用不同醚化反应温度、改变醚化反应时间、环化加碱量等条件对产品质量的影响,确定了合成条件.结果表明其最优化合成条件为：采用盐酸作催化剂合成甲撑二间苯二酚,环氧醚化温度为95 ℃,醚化时间8 h,实际用碱量为理论用碱量的1.1倍.产品改性邻甲酚醛环氧聚合物固化体系时能显著提高其玻璃化温度,改善耐热性能,玻璃化温度可达180～190 ℃,比邻甲酚醛环氧体系提高了30 ℃以上.

The methylene- bis（1, 3 - benzenediol）, prepared by condensation of 1.3 - benzendiol with formaldehyde, was glycidyl etherated with epichlorohydrin to prepare methylene- bis（1.3 - benzenediol） - tetra glycidyl ether, the effect of different catalyst used for phenol - formaldehyde condensation, etherification reaction temperature, etherification time, the base use level in cyclization on the products quality was discribed. In this paper, test showed that the optimum synthetic conditions were below： hydrochloric acid was used as catalyst for 1, 3 - benzenediol- formaldehyde condensation, etherification temperature was 95 degrees, etheri- fication time was 8 h, practical use level of base in cyclization reaction was 1.1 times of theoretical level. The products obtained might be used to modify cresol resin and the glass transition temperature and heat- resistance of eresol resin modified with the synthetie tetrafunetional epoxy resin were inereased so that it was as high as 180 - 190 degrees which was increased 30 degrees more than common cresol resin system.