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双[3-(3,5-二叔丁基-4-羟基苯基)丙酸]三甘醇酯的合成与表征
Synthesis and Characterization of Triethylene Glycol Bis Propionate
【摘要】 以3-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯(简称3,5-甲酯)与三甘醇为原料,有机锡为催化剂,通过酯交换法在无溶剂的条件下合成了双[3-(3,5-二叔丁基-4-羟基苯基)丙酸]三甘醇酯。通过实验考察了反应温度、催化剂及催化剂用量、反应时间及物料配比等因素对反应的影响。结果表明,最佳的反应条件是:反应温度为125~135℃,催化剂为有机锡,催化剂用量为0.50g,反应时间为3.5h,3,5-甲酯与三甘醇摩尔比为2.10∶1。在此条件下,收率在94%以上,产品熔点为106~107℃,通过元素分析、红外光谱分析、核磁氢谱对产品进行了结构表征。
【Abstract】 Triethylene glycol bis propionate was prepared without solvent by transesterifying methyl-3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate with triethylene glycol in the presence of organic-tin as a catalyst. The influence of temperature, time, catalyst and the molar ratio of raw materials on the yield of the product were studied. The result shows that the optimum conditions are as follows: reaction temperature is ranged from 125~135 ℃, the catalyst is 0.5 g, reaction time is 3.5 h, the molar ratio of between methyl-3-(3,5-di-tert-butyl-4-hydroxyphenyl)- propionate and triethylene glycol is 2.10∶1. The yield of the product can be up to 94% under the optimum condition. Melting point of the product is 106~107 ℃. By means of elemental analysis, IR and 1 HNMR characterized the structure of the product.
- 【文献出处】 石油化工高等学校学报 ,Journal of Petrochemical Universities , 编辑部邮箱 ,2003年02期
- 【分类号】TQ314.24
- 【被引频次】5
- 【下载频次】159