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机构地区:[1]河北工程大学科信学院,邯郸056038 [2]河北工程大学理学院,邯郸056038
出 处:《中国食品添加剂》2013年第3期132-136,共5页China Food Additives
基 金:邯郸市科学技术研究与发展计划项目(1223108086-5);河北省科技计划项目(12206808D)
摘 要:以没食子酸和正丙醇为原料,硫酸氢钠为催化剂,采用微波辐射成功合成了没食子酸丙酯。通过熔点测定、红外光谱分析和元素分析对产品进行结构表征;通过单因素考察了没食子酸和正丙醇的物质的量比、催化剂的用量、微波时间、微波功率等因素对反应的影响,在单因素实验的基础上,采用正交试验法优化确定了最佳合成条件,结果表明最佳反应条件为:没食子酸用量为0.025mol,没食子酸与正丙醇的物质的量比为1∶15,催化剂量为3g,微波功率为500W,微波时间为45min,不加带水剂,在此条件下,没食子酸丙酯的收率可达82.58%。实验证明硫酸氢钠具有较好的催化活性和重复使用性能;与热催化酯化反应相比,微波辐射可缩短反应时间,降低能耗。该方法实现了绿色合成食品抗氧化剂没食子酸丙酯。Propyl gallate(PG) was synthesized by 1-propyl alcohol and gallic acid with sodium bisulfate as catalyst under microwave irradiation.The reaction products were structurally identified by means of melting point measurement,Infrared(IR) spectral analysis and elemental analysis.The effects of molar ratio of gallic acid to 1-propyl alcohol,catalyst dosage,microwave time and microwave power were studied.On the basis of single facter tests,the optimal conditions were optimized by the orthogonal experiments as follows: 0.025 mol gallic acid,molar ratio of gallic acid to 1-propyl alcohol 1 ∶ 15,dosage of catalyst 3.0g,microwave power 500 W,for 45min,with no water-carrying reagent.Under the above conditions,the yield of propyl gallate could reach up to 82.58%.The experiments indicated that NaHSO4 has good catalytic activity and could be used repeatedly.Over the heating esterification,microwave radiation could reduce reaction time and lower energy consumption under the same conditions.The green synthesis food antioxidant Propyl gallate was realized.
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