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首先以二乙醇胺和丙烯酸甲酯为原料,通过Michael加成反应制备A2B型前驱单体N,N-二羟乙基-3-氨基丙烯酸甲酯,然后以三羟甲基丙烷为反应中心核,采用有核准一步法合成羟端基超支化聚(胺-酯)(HPAE);最后利用二茂铁甲酸对HPAE进行端基改性,得到了二茂铁端基修饰的超支化聚(胺-酯)(HPAE-Fc)。HPAE-Fc的合成条件:w(催化剂)=2.5%(相对于反应物总质量),反应温度为140℃,反应物投料比n(OH)∶n(二茂铁甲酸)为1∶0.8,反应时间为4 h。采用FTIR、1HNMR、UV-vis、DSC和羟值等手段对HPAE-Fc的结构进行了表征,表明二茂铁基团成功地接枝到了HPAE分子表面,接枝率达70%。
First, with diethanolamine and methyl acrylate as raw materials, the A2B precursor monomer N, N-dihydroxyethyl-3-aminoacrylate was prepared by Michael addition reaction, and then trimethylolpropane was used as the reaction center. Hydroxyl terminated hyperbranched poly (amine-ester) (HPAE) was synthesized by approved one-step method. Finally, the ferrocene-terminated HPAE was modified with ferrocenecarboxylic acid to obtain the hyperbranched poly (amine- Ester) (HPAE-Fc). The synthesis conditions of HPAE-Fc: w (catalyst) = 2.5% (relative to the total mass of the reactants), reaction temperature 140 ° C, reactant feed ratio n (OH) The reaction time is 4 h. The structure of HPAE-Fc was characterized by means of FTIR, 1HNMR, UV-vis, DSC and hydroxyl value. The results showed that the ferrocene group was successfully grafted onto the surface of HPAE and the grafting rate reached 70%.