N-甲基-2-[4-二甲基氨基]苯基-3,4-富勒烯基吡咯烷微米片控制合成研究

Controllable synthesis and characterization of N-methyl-2-[4-dimethyl-amido] phenyl-3,4-fulleropyrrolidine derivative microflake structure

以富勒烯C60、4-(N,N-二甲基氨基)苯甲醛为原料,通过1,3-偶极环加成反应合成了N-甲基-2-[4-二甲基氨基]苯基-3,4-富勒烯基吡咯烷。首次采用表面活性剂协助自组装的方法制得C60衍生物的微米片结构。结果表明,N-甲基-2-[4-二甲基氨基]苯基-3,4-富勒烯基吡咯烷结晶态形貌为片状结构,形貌和晶体结构受溶剂种类、溶液浓度、醇与溶剂体积配合比、表面活性剂浓度的影响。当甲苯为溶剂,溶液浓度为1.0mg/mL,异丙醇与甲苯体积配合比为3∶1,表面活性剂十六烷基三甲基溴化铵(CTAB)浓度为5.0mmol/L时,N-甲基-2-[4-二甲基氨基]苯基-3,4-富勒烯基吡咯烷结晶态形貌为宽度约3μm、厚度约50nm规则的正方形片状结构。

N-methyl-2-[4-dimethyl-amido]phenyl-3,4-fulleropyrrolidine was synthesized by [60]fullerene and4-（N,N-dimethylamino）benzaldehyde with 1,3-dipolar cycloaddition reaction,different morphologies of micro structure were fabricated for the first time using the surfactant assisted self-assembly method.The crystalline structure was characterized by scanning electron microscopy（SEM）,thermal gravimetric analysis（TGA）and photoluminescence（PL） spectroscopy.The morphology and crystal structure of N-methyl-2-[4-dimethyl-amido]phenyl-3,4-fulleropyrrolidine was flakes,and controlled by using different solvents,concentration,volume ratio of alcohol and solvent,as well as surfactant concentration.When toluene was used as solvent,the concentration was 1.0 mg/mL,the volume ratio of isopropyl alcohol and toluene was 3∶1,the concentration of surfactant cetyltrimethylammonium bromide（CTAB）was 5.0 mmol/L,the width of about 3μm and the thickness of about 50 nm regular square flakes of N-methyl-2-[4-dimethyl-amido]phenyl-3,4-fulleropyrrolidine were obtained and can be controlled.