木质素模型化合物香草醛Mannich反应及其产物化学结构表征.PDFVIP

木质素模型化合物香草醛Mannich反应及其产物 化学结构表征 * 聂明才,孔振武 ,霍淑平,吴国民,陈健 (中国林业科学研究院林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局林产 化学工程重点开放性实验室;江苏省生物质能源与材料重点实验室, 江苏 南京 210042) 摘摇 要:摇 以木质素模型化合物香草醛、二乙醇胺及多聚甲醛为原料,1,4-二氧杂环己烷为溶剂,通 过Mannich反应合成了香草醛胺基多元醇,研究了物料配比、反应温度、时间及溶剂用量等因素对 NIE Ming鄄cai摇 摇 Mannich反应的影响。 实验结果表明:反应物料按物质的量比n(香草醛)颐n(甲醛)颐n(二乙醇胺) 1颐1颐1,甲醛与二乙醇胺60 益 反应2h生成1,3-氧氮杂环戊烷,再将其滴入香草醛中,80 益 反应3h,二氧六环溶剂用 量为100mL/ mol(以香草醛的物质的量计),二乙醇胺的转化率最高可达到84.92%。 采用HPLC、LC-MS、FT-IR及 1HNMR表征了香草醛胺基多元醇的化学结构,相对分子质量269。 关键词:摇 木质素模型化合物;香草醛;Mannich反应;胺基多元醇 中图分类号:TQ35摇 摇 摇 摇 摇 摇 文献标识码:A摇 摇 摇 摇 摇 摇 文章编号:0253-2417(2012)03-0013-06 Mannich Reaction of Lignin Model Compound Vanillin and Chemical Structure Characterization of Its Product NIE Ming鄄cai,KONGZhen鄄wu,HUO Shu鄄ping,WU Guo鄄min,CHENJian (Instituteof Chemical Industry of Forest Products,CAF;National Engineering Lab.for Biomass Chemical Utilization;Key and Open Lab.of Forest Chemical Engineering,SFA;Key Lab.of BiomassEnergy and Material,Jiangsu Province,Nanjing210042,China) Abstract:Vanillin aminated polyol(VAP) was prepared by vanillin,diethanolamine and paraformaldehyde in 1,4鄄dioxane by Mannich reaction. The effects of material ratio,reaction temperature,reaction time and solvent dosage on the Mannich reaction were investigated. Itwasobservedthehighest conversionrateof diethanolaminewasupto84.92% by dropping 1,3鄄oxazolidine whichwasthereactionproduct of formaldehyde and diethanolamine at60益 for2 h,intovanillin andreacting at80 益 for3h in the molar ratio of n(vanillin)颐n(formaldehyde)颐n(diethanolamine) as 1颐1颐1 in 1,4鄄dioxane of 100 mL/ mol vanillin. The 1 chemical structure of vanillin aminated polyol was character