金属钝化剂Nangarz XL-1合成的研究

Study on Synthesis Metal deactivator Nangarz XL-1

研究了以2,6-二叔丁基苯酚,丙烯酸甲酯,草酸二乙酯及乙醇胺为原料合成具有抗氧化及金属钝化双重功能的金属钝化剂Nangarz XL-1的合成工艺,考察了各步反应机理及影响因素。结果表明中间体(3,5-二叔丁基-4-羟基)苯基丙酸甲酯合成最佳条件为:丙烯酸甲酯与2,6-二叔丁基苯酚的质量比为1.10∶1,丙烯酸甲酯加入方式为120℃滴加0.5h,在140℃下反应4h,产率96.5%;中间体N,N′-双(羟乙基)草酰胺合成最佳条件为:乙醇胺与草酸二乙酯物质的量比2∶1,反应温度为112℃,产率95.5%;产品Nangarz XL-1合成的最佳条件为:反应温度180℃,反应时间4h,催化剂为有机锡,产率90.2%。用红外光谱和核磁共振氢谱表征了产品化学结构。

The process of synthesizing Nangarz XL-1 with 2,6-di-tert-butylphenol, ethyl oxalate and ethanolamine was studied. It is a hindered phenol with dual function of metal deactivation. The reaction mechanism and effective factors were studied through methyl acrylate, diantioxygenation and the experiment. The optimized reaction conditions are as follows. For （3,5-ditertbutyl-4-hydroxy） phenyl propionate methyl, the optimized conditions are： methyl acrylate （mol ratio） is 1.10：1, methyl acrylate is added for 0.5 h at 120℃ and reacts at 140 ℃ for 4h, yield 96.5%; for N,N＇-Bis （2-hydroxyethyl） oxamide： ethanolamine/diethyl oxalate （mole ratio） is 2：1, reacts at 112℃ for 1 h, yield 95.5%; for metal deactivator Nangarz XL-1： the organic tin is used as catalyst,reacts at 180℃ for 4 h, yield 90.2%. The chemical structure of the product was characterized by the IR and ^1HNMR methods.