愈创木酚胺基多元醇的合成及表征  

Synthesis and Characterization of Guaiacol Aminated Polyol

作　　者：聂明才[1] 孔振武[1] 霍淑平[1] 吴国民[1] 陈健[1] 

机构地区：[1]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

出　　处：《生物质化学工程》2011年第3期15-20,共6页Biomass Chemical Engineering

基　　金：国家林业局948技术引进项目(2008-4-77)

摘　　要：以木质素模型化合物愈创木酚、二乙醇胺及多聚甲醛为原料,通过Mannich反应合成了愈创木酚胺基多元醇,研究了物料滴加顺序、物料配比、反应温度及时间等因素对Mannich反应的影响。实验结果表明:反应物料按物质的量比n(愈创木酚)∶n(甲醛)∶n(二乙醇胺)1∶1∶1,甲醛与二乙醇胺60℃反应2 h生成1,3-氧氮杂环戊烷,再将其滴入愈创木酚中,80～90℃反应3～4 h,二乙醇胺的转化率最高可达到90.71%。并采用HPLC、LC-MS及FT-IR表征了愈创木酚胺基多元醇的化学结构。The Mannich reaction was applied to prepare guaiacol aminated polyol（GAP） from guaiacol,diethanolamine and paraformaldehyde.The effects of main reaction factors,i.e.,ingredients drop-charging order,ratio of raw materials,reaction temperature and reaction time on the Mannich reaction were investigated.The results showed that the conversion rate of diethanolamine was the highest up to 90.71 % by dropping 1,3-oxazolidine into guaiacol and reacting at 80-90 ℃ for 3-4 h in the molar ratio n（guaiacol）∶n（formaldehyde）∶n（diethanolamine） as 1∶1∶1.The 1,3-oxazolidine was obtained from the reaction of formaldehyde with diethanolamine at 60 ℃ for 2 h.The chemical structure of guaiacol aminated polyol was characterized by HPLC,LC-MS and FT-IR.

关 键 词：木质素模型化合物 愈创木酚 MANNICH反应 胺基多元醇 

分 类 号：TQ352.1[化学工程]