摘要
采用两步升温法,合成了N,N,N',N'-四(β-羟乙基)己二酰胺(HAA)类固化剂。并探讨了原料配比、反应温度、反应时间和结晶溶剂对产品收率的影响。试验结果表明:在Na OH和CH3ONa复合催化剂条件下,n(己二酸二甲酯)∶n(二乙醇胺)=1∶2.3,采用两步升温法,减压状态下75℃反应1 h,95℃反应3 h,混合结晶溶剂m(甲醇)∶m(丙酮)=1∶3,产品收率和纯度分别为95%和99%。并借助液相和红外光谱进行了表征。
The curing agent of N,N,N',N'-tetra-(β-hydroxyethyl) adipamide were prepared by two-step method. The influences of raw material ratio, reaction temperature, reaction time and crystal solvent on product yield were tested. Test results showed that molar ratio of dimethyladipate to ethanolamine at 1∶2.3, sodium methoxide and sodium hydroxide as catalysts, first step reaction temperature at 75 ℃, first step reaction time by 1.5 h, the second step reaction temperature at 95 ℃, the second step reaction time by 3 h, crystal solvent of methoxide and acetone by the ratio of 1∶3, the product yield was 95% and the purity of product reached 99%. The product was characterized by liquid chromatography and IR.
引文
[1]慕春明,史铁钧,史先磊.H2O2环氧化TAIC制备TGIC[J].应用化学,2008,25(9):1 090-1 094
[2]黄逸东,陈丰.TGIC中总氯含量的测定和分析[J].涂料工业,2012,42(8):54-56
[3]KIM D.S.,HAN M.J.,LEE J.R..Cure behavior and properties of an epoxy resin modified with a bismaleimide resin[J].Polymer Engineering and Science,1995,35(17):1 353-1 358
[4]赵良燕,史铁钧,钱金明.新型固化剂β-羟烷基酰胺的合成与表征[J].热固性树脂,2009,24(2):19-22
[5]童乃斌,王申生,孙毅.β-羟烷基酰胺(SA552)的合成及其应用[J].涂料工业,1995,25(2):20-22
[6]丰巍伟,杨敬梅,方志杰.二步法合成N,N,N',N'-四(β-羟乙基)己二酰胺[J].化学试剂,2009,31(8):652-654
[7]邹菁,刘安昌,金焰.新型固化剂四羟乙基己二酰胺制备工艺的研究[J].武汉工程大学学报,2007,29(2):20-22