丙烯酰二茂铁基乙醇酯的制备及表征  

The Preparation and Characterization of Acroloyl Ferrocenyl Ethyl Ester

作　　者：柯爱茹[1] KE Airu

机构地区：[1]黎明职业大学党政办公室,福建泉州362000

出　　处：《黎明职业大学学报》2016年第2期70-76,共7页Journal of LiMing Vocational University

基　　金：福建省教育厅中青年教师教育科研项目(JA13428);福建省自然科学基金项目(2014J01386)

摘　　要：以二茂铁为原料,通过酰基化、羟基化、酯化制备丙烯酰二茂铁基乙醇酯(AFc EE),采用红外光谱、核磁共振以及紫外光吸收对产物进行表征,探讨单体配比、反应温度、投料顺序对AFc EE产率的影响。红外谱图显示,1 631 cm-1处出现C=C特征吸收峰,1 720 cm-1处出现C=O特征吸收峰;核磁氢谱图显示,AFc EE的端位烯烃位号3与位号5的质子共振吸收峰由于共轭作用,向低场发生位移,分别出现在6.0与7.26处;紫外光谱图显示,277 nm处出现α,β-不饱和羧酸酯吸收带。AFc EE的最佳制备条件为,n(丙烯酰氯)∶n(二茂铁基乙醇)=1.2∶1,将丙烯酰氯投入二茂铁基乙醇、三乙胺混合液中,先在冰浴条件下使其充分混合,再缓慢升温至室温,最后升温至50℃,Afc EE的产率可达71%。Acroloyl Ferrocenyl Ethyl Ester( AFc EE) was prepared with ferrocene as raw materials,through acylation,hydroxylation and esterification. The preparation condition including monomer ratio,reaction temperature,feeding order were discussed by using FTIR,H- NMR and UV / vis to study the structure of AFc EE.FTIR results indicate that the peak at 1 631cm- 1comes from C = C,the peak at 1720 cm- 1comes from C = O; HNMR results show that the absorption of H witch is at No. 3 and No. 5 occurred at 6. 0 and 7. 26;UV / vis results suggest that AFc EE belongs to α,β- unsaturated carboxylic acid ester. The best preparation condition in which the yield of AFc EE reaches 71% is that: n( acryloyl chloride) ∶ n( ferrocene ethanol) =1. 2 ∶ 1,The process is as follows: firstly acryloyl chloride is put into the mixture of ferrocenyl ethanol and triethylamine,secondly this miscible liquid is thoroughly mixed under ice- cooling,then it is slowly warmed to room temperature,and finally warmed to 50 ℃ 。

关 键 词：二茂铁 乙酰基二茂铁 二茂铁基乙醇酯 丙烯酰二茂铁基乙醇酯 

分 类 号：TQ314.22[化学工程—高聚物工业]