愈创木酚胺基多元醇的合成及表征

Synthesis and Characterization of Guaiacol Aminated Polyol

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.