1,2-环氧丙醚基芳香酮紫外线吸收剂的微波合成和表征 - 化学通报.PDF

化学通报 2014 年 第 77 卷 w2014016 研究论文 1,2-环氧丙醚基芳香酮紫外线吸收剂的微波合成和表征 张明政 李 然 黄 丹* (江南大学生态纺织教育部重点实验室 无锡 214122) 摘 要 以 2,4-二羟基二苯甲酮、4-羟基苯乙酮(HAP)为原料分别和环氧氯丙烷反应，经微波辐照合成了 两种反应性紫外线吸收剂 2-羟基-4-缩水甘油醚基二苯甲酮(HEPBP)和 4-缩水甘油醚基苯乙酮(EPAP) 。结构采 用红外光谱、核磁和质谱表征。最佳合成条件为：n(羟基芳香酮):n(环氧氯丙烷)=1:3 ，微波功率400W ，于 90℃ 反应 15min，收率分别是 52.6%和 58.3% 。与常规合成方法比较，微波合成法能降低反应温度、大大地缩短反 应时间。产物中环氧丙烷基团的引入能提高芳香酮类紫外线吸收剂的紫外吸收性能。 关键词 微波合成 反应性紫外线吸收剂 2,4-二羟基二苯甲酮 4-羟基苯乙酮 环氧氯丙烷 Microwave Syntheses and Characterization of 1,2-Epoxy Propyl Ether Aromatic Ketone UV Absorbents Zhang Mingzheng, Li Ran, Huang Dan* (Key Laboratory of Eco-textiles, Jiangnan University, WuXi 214122) Abstract Two reactive UV absorbents, 2-hydroxy-4(2,3-epoxypropoxy)benzophenone and 4(2,3- epoxypropoxy)acetophenone were synthesized by reaction of hydroxylated aromatic ketone (2,4-dihydroxybenzophenone and 4-acetophenone) and epichlorohydrin under microwave radiation and characterized by IR, NMR, MS and UV-Vis spectra. The optimal reaction condition was as follow: molar ratio of hydroxylated aromatic ketone and epichlorohydrin was 1:3, microwave power was 400 W in sodium hydroxide solution at 90℃ for 15min. The yield was 52.6% and 58.3% under this condition. Comparing with the conventional synthesis process, microwave synthesis can reduce the reaction temperature, greatly shorten the reaction time. The UV absorption properties of aromatic ketone ultraviolet absorbents were improved significantly as the introduction of epoxy propane groups. Keywords Microwave synthesis, UV absorbers with react