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双醛淀粉-苯胺希夫碱的合成

Synthesis of Dialdehyde Starch-aniline Schiff-base

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【作者】 王晓娟具本植张淑芬

【Author】 WANG Xiao-juan,JU Ben-zhi,ZHANG Shu-fen(State Key Laboratory of Fine Chemicals,Dalian University of Technology,Dalian 116024,Liaoning,China)

【机构】 大连理工大学精细化工国家重点实验室

【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。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,体系中乙酸体积分数3%,反应温度50℃,醛基与氨基的摩尔比为2:1,反应时间12 h。在最佳条件下,以双醛摩尔分数为5%的双醛淀粉(DAS5)为底物的苯胺利用率为94%;以双醛摩尔分数为20%的双醛淀粉(DAS20)为底物的苯胺利用率为55%。通过FTIR、NMR和XRD对双醛淀粉-苯胺希夫碱的结构进行了表征。

【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 in 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 fraction),reaction temperature is 50 ℃,the molar ratio of aldehyde group to amino group is 2∶ 1,and reaction time is 12 h.Under these optimum conditions,the utilization ratio of aniline is 94% with DAS5(the dialdehyde molar fraction is 5%) as reactant,and 55% with DAS20(the dialdehyde molar fraction is 20%) as reactant.The structure of DAS-AN is characterized by means of FTIR,NMR and XRD.

【基金】 国家自然科学基金重点基金(20836001)~~
  • 【文献出处】 精细化工 ,Fine Chemicals , 编辑部邮箱 ,2012年06期
  • 【分类号】O636.12
  • 【被引频次】4
  • 【下载频次】299
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