双醛淀粉-苯胺希夫碱的合成

The Synthesis of Dialdehyde Starch-Aniline Schiff-base

摘要:

在以二甲基亚砜为溶剂的均相反应体系中，以双醛淀粉和苯胺为底物，乙酸为催化剂，N2保护下，合成了双醛淀粉-苯胺希夫碱。详细研究了反应条件，得到的最佳反应条件为：以二甲基亚砜为溶剂，双醛淀粉质量浓度为100 g/L，体系中乙酸含量3%(体积)，反应温度50 ℃，醛基与氨基的摩尔比为2:1，反应时间12h。在最佳条件下，以双醛含量为5%的双醛淀粉（DAS5）为底物的苯胺利用率为94%；以双醛含量为20%的双醛淀粉（DAS20）为底物的苯胺利用率为55%。通过FT-IR、NMR和XRD对双醛淀粉-苯胺希夫碱的结构进行了表征。 关键词：双醛淀粉；苯胺；均相；希夫碱

Abstract:

Dialdehyde starch-aniline Schiff-base (DAS-AN) was synthesized with dialdehyde starch (DAS) and aniline as reactants, and acetic acid as catalyst in dimethyl sulfoxide (DMSO) homogeneous system under N2 atmosphere. The synthesis conditions of DAS-AN were studied and the optimum conditions were as follows: the mass concentration of DAS is 100 g/L in DMSO, the dosage of acetic acid is 3% (volume), reaction temperature is 50℃, the molar ratio of aldehyde group to amino group is 2:1, and reaction time is 12h. Under the optimum conditions, the utilization ratio of aniline is 94% with DAS5 (the dialdehyde content is 5%) as reactant, and that is 55% with DAS20 (the dialdehyde content is 20%) as reactant. The structure of DAS-AN is characterized by FT-IR, NMR and XRD.