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出 处:《高分子学报》2011年第12期1382-1389,共8页Acta Polymerica Sinica
基 金:山西省自然科学基金(基金号201002100843)资助项目
摘 要:通过高分子反应法研究制备了高分子化的8-羟基喹啉铝发光材料.首先使用自制的氯甲基化试剂1,4-二氯甲氧基丁烷(BCMB),制备了5-氯甲基-8-羟基喹啉(CHQ);通过聚苯乙烯(PS)与CHQ之间的Friedel-Crafts烷基化反应,制得侧链键合有8-羟基喹啉(HQ)的改性聚苯乙烯HQ-PS;再使HQ-PS与二配体的8-羟基喹啉铝配合物Alq2发生配位反应,制得了含8-羟基喹啉铝配合物的聚苯乙烯发光材料Alq3-PS,即实现了8-羟基喹啉铝配合物Alq3的高分子化;并采用红外光谱(FTIR)、核磁共振氢谱(1H-NMR)、紫外光谱(UV)及热失重分析(TGA)等方法对其结构和性能作了表征,还测定了该发光材料的光致发光性能.重点考察了各种反应条件对在PS侧链键合8-羟基喹啉的影响规律,优化了反应条件.实验结果表明,5-氯甲基-8-羟基喹啉与聚苯乙烯之间的Friedel-Crafts反应可顺利进行,适宜的反应条件为70℃,以N,N-二甲基甲酰胺(DMF)为溶剂,以SnCl4为催化剂.高分子化的8-羟基喹啉铝配合物Alq3-PS具有Alq3的荧光发射光谱,且具有比聚苯乙烯更高的热稳定性.5-Chloromethyl-8-hydroxyquinoline(CHQ) was first prepared through the reaction between HQ and chloromethylation reagent 1,4-bichloromethoxy-butane(BCMB).The Friedel-Crafts alkylation reaction was carried out between CHQ and polystyrene(PS),and HQ was bounded onto the side chains of PS,obtaining the modified polystyrene HQ-PS.And then,the coordination reaction between HQ-PS and 8-hydroxyquinoline aluminum complex Alq2 that have two HQ ligands was conducted,and the luminous material Alq3-PS,on which 8-hydroxyquinoline aluminum complex Alq3 is attached chemically,was achieved,namely,the polymeric Alq3 was prepared.In order to fully characterize the chemical structure and properties of Alq3-PS,several characterization means were employed such as FTIR,1H-NMR,UV-Vis absorption spectrum and thermogravimetric analysis(TGA),and its luminous performance was determined.In this work,the effects of the main factors on the Friedel-Crafts alkylation reaction were investigated,and the reaction conditions were optimized.The experimental results show that the Friedel-Crafts alkylation reaction between PS and CHQ can proceed successfully,and the suitable reaction conditions are as follows: a temperature of 70℃,with N,N-dimethylformamide(DMF) as solvent,and using SnCl4 as Lewis catalyst.The Alq3-containing polystyrene,Alq3-PS,possesses the fluorescence-emission spectrum of Alq3 and has higher thermostability than polystyrene.
关 键 词:8-羟基喹啉铝 聚苯乙烯 FRIEDEL-CRAFTS烷基化反应 荧光发射
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