氯离子桥联铜(II)配合物微/纳米结构材料的合成和表征

摘要：采用2-吡咯甲醛分别与2-（2-氨乙基）吡啶、2-氨甲基吡啶反应，制备出两种三齿席夫碱配体HL1和HL2 。在表面活性剂聚乙烯吡咯烷酮存在时，在甲醇溶液中，由配体HL1和HL2分别与三乙基胺、四氟合硼酸铜(Ⅱ)、碘及KCl作用，得到铜(II)配合物[Cu2(L3)2(-Cl)2]和[Cu2(L4)2(-Cl)2]微/纳米结构材料。对配体进行了红外光谱、核磁共振氢谱、质谱表征，对配合物微/纳米材料的结构进行了红外光谱、XRD、单晶X-射线衍射表征，对微/纳米结构材料的形貌用扫描电子显微镜（SEM）进行了表征。XRD分析表明加了表面活性剂制备得到的配合物微/纳米材料与不加表面活性剂得到的是同一种物质，且结构相同。还研究了聚乙烯吡咯烷酮的用量和反应时间对配合物微/纳米材料形貌和尺寸的影响。60908

毕业论文关键词：席夫碱，聚乙烯吡咯烷酮，铜(II)配合物，纳米材料

Abstract：Two tridentate Schiff Ligands HL1 and HL2 were obtained by reacting pyrrole-2-carboxaldehyde with 2-(2-aminoethyl)pyridine or 2-aminomethylpyridine, respectively. In the presence of polyvinylpyrrolidone as a surfactant, copper (II) complex micro/nano structural material [Cu2(L3)2(-Cl)2] was obtained by mixing ligand HL1, copper(II) tetrafluoroborate hydrate, iodine and potassium chloride, in methanol, using triethyleneamine as a base. Similarly, copper (II) complex micro/nano structural material [Cu2(L4)2(-Cl)2] was obtained by mixing ligand HL2, copper(II) tetrafluoroborate hydrate, iodine, potassium chloride, triethyleneamine and polyvinylpyrrolidone in methanol. Two ligands were characterised by IR, 1H NMR and ESI-MS. Structures of two micro/nano materials were analysed by IR, powder X-ray deffraction (XRD) and single crystal X-ray deffraction determination. Morphology of the two micro/nano materials was inspected using a scanning electron microscope. Powder X-ray analysis shows that structures of the micro/nano materials prepared by the procedure with polyvinylpyrrolidone as a surfactant are the same as those obtained from the procedure without the surfactant polyvinylpyrrolidone. Influences of the amount of surfactant and reaction time on the morphologies of the two micro/nano materials were investigated.

Keywords：Schiff base, polyvinylpyrrolidone, copper(II) complexes, nano-sized materials

1 前言 5

2 实验部分 6

2.1 仪器与试剂 6

2.1.1 仪器 6

2.1.2 药品与试剂 7

2.2 配体的合成 7

2.2.1 配体HL1的合成 7

2.2.2 配体HL2的合成 8

2.3 配合物的合成 8

2.3.1 配合物[Cu2(L3)2(-Cl)2] 微/纳米结构材料的合成 8

2.3.2 配合物[Cu2(L4)2(-Cl)2] 微/纳米结构材料的合成 9

3 结果与讨论 10

3.1 配体HL1和HL2的合成及表征 10

3.1.1 HL1的合成 10

3.1.2 HL2 的合成 11

3.2 配合物[Cu2(L3)2(-Cl)2]和[Cu2(L4)2(-Cl)2] 微/纳米结构材料的合成和结构表征 12

3.2.1 配合物的合成 13

3.2.2 配合物微/纳米结构材料的红外表征 13

3.2.3 配合物微/纳米结构材料的XRD表征 14 氯离子桥联铜(II)配合物微/纳米结构材料的合成和表征:http://www.751com.cn/huaxue/lunwen_66466.html