为改善环氧树脂固化物柔韧性差的缺点,从固化剂结构设计着手,合成一种新型环氧树脂固化剂中间体四[(对-乙酰氨基苯氧基)甲基]甲烷.该中间体以季戊四醇四苯磺酸酯和对乙酰氨基酚为原料,通过Williamson醚化反应得到.采用单因素试验和正交实验研究了反应时间、反应温度以及反应物料配比对中间体四[(对-乙酰氨基苯氧基)甲基]甲烷收率的影响,结果表明:最佳反应时间为16 h,反应温度为170℃,反应物投料比为1:5,目标产物收率高达76.2%.用红外、核磁等手段对中间体结构进行表征,红外谱图中3297 cm-1和1659 cm-1处出现酰胺的特征峰,核磁氢谱中δ9.73(s,1H)表明了酰胺基团的存在,最终确认合成了纯净的四[(对-乙酰氨基苯氧基)甲基]甲烷且产率较高.%To improve the poor flexibility of cured epoxy resin,a new curing agent intermediates of tetrakis [(p-acetamidophenoxy) methyl] methane were synthesized based on curing agent structure design. The intermediates were prepared by etherification reaction method using pentaerythritol tetrabenzenesulfonate and acetaminophen as raw materials. The effects of reaction time,reaction temperature and the ratio of reaction materials on the yield of tetrakis [(p-acetamidophenoxy) methyl] methane were explored by single factor experiment and orthogonal experiment. The results show that the yield of the tetrakis[(p-acetamidophenoxy) methyl]methane reaches 76.2%at the optimum reaction time of 16 h,reaction temperature of 170℃,reactant ratio of 1:5. The structure of the intermediates was characterized by Fourier transform infrared spectroscopy and nuclear magnetic resonance hydrogen spectroscopy. Infrared spectrum shows the characteristic peaks of amide appears at 3297 cm-1 and 1659 cm-1,nuclear magnetic resonance hydrogen spectroscopy shows the presence of amide at δ 9.73 (s,1H). Both of test methods above confirm the synthesis of pure tetrakis [(p-acetamidophenoxy)methyl]methane with high yield.
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