N,N,N',N'-四(β-羟乙基)己二酰胺合成工艺的研究
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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.
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
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