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以对氯甲基苯甲酸(CMBA)为试剂,通过Friedel-Crafts烷基化反应,将苯甲酸(BA)键合在聚砜(PSF)侧链,制得了改性聚砜BAPSF,并采用FT IR与1H NMR等方法对其结构进行了表征。通过与Tb3+配位,制得了高分子-稀土配合物BAPSF-Tb(Ⅲ),初步考察了该配合物的荧光发射特性。本文重点研究了聚砜的功能化改性反应,考察了主要因素对CMBA与PSF之间Friedel-Crafts烷基化反应的影响,分析了反应机理,优化了反应条件。实验结果表明,CMBA与PSF之间Friedel-Crafts烷基化反应顺利进行的适宜反应条件为:70℃,以N,N-二甲基乙酰胺(DMAC)为溶剂,SnCl4为催化剂。配合物BAPSF-Tb(Ⅲ)不仅发射出Tb3+的特征荧光,而且大分子配基BAPSF对Tb3+的荧光发射显示出很强的敏化作用。
The modified polysulfone BAPSF was prepared by the Friedel-Crafts alkylation reaction of benzoic acid (BA) on the side chain of polysulfone (PSF) with p-chloromethylbenzoic acid (CMBA) Its structure was characterized by IR and 1H NMR. By complexing with Tb3 +, the polymer-rare earth complex BAPSF-Tb (Ⅲ) was prepared and the fluorescence emission characteristics of the complex were investigated. This paper focuses on the functionalized polysulfone-modified reaction, investigated the impact of the main factors on the Friedel-Crafts alkylation reaction between CMBA and PSF, analyzed the reaction mechanism, and optimized the reaction conditions. The experimental results show that Friedel-Crafts alkylation reaction between CMBA and PSF is carried out at 70 ℃ with N, N-dimethylacetamide (DMAC) as solvent and SnCl4 as catalyst. The complex BAPSF-Tb (Ⅲ) not only emits the characteristic fluorescence of Tb3 +, but also the macromolecule ligand BAPSF shows strong sensitization to the Tb3 + fluorescence emission.