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研究了钐离子(Ⅲ)与苯代三聚氰胺与均苯四酸二酐缩聚并亚酰化后的产物聚酰亚胺的固相配位反应。考察了微波辐射时间(功率)、稀土离子和聚合物的配比以及温度等因素对配合物产率及配合物中钐离子含量的影响; 测量了配合物的红外光谱、拉曼光谱、扫描电镜、13C固体核磁共振及X射线粉末衍射等,并推测了配合物可能的结构。用络合滴定法测定了配合物中钐离子的含量, 通过荧光发射光谱测量了配合物的荧光发射强度,考察了荧光发射强度和配合物中钐离子含量之间的关系,并与相应的常规加热配位进行比较。通过磁化曲线测量了配体和配合物的磁性能。实验结果表明:此类配合物只表现出较弱的钐离子的特征荧光峰,说明钐离子的第一激发态能级和配体的三重态能级之间不能很好地匹配, 但是荧光发射强度随配合物中钐离子含量的增加而增强, 说明钐离子在配合物中是均匀分布的。另外配合物显示出稀土离子优良的磁性能。
The solid-phase coordination reaction of the polyimide with samarium (Ⅲ) and the product of polycondensation and acylation of benzoguanamine and pyromellitic dianhydride was studied. The effect of microwave irradiation time, power, rare earth ion and polymer ratio and temperature on the yield of complex and the content of samarium in the complex were investigated. The infrared spectrum, Raman spectrum, SEM, 13C solid state nuclear magnetic resonance and X-ray powder diffraction, and speculated that the possible structure of the complex. The complexation titration method was used to determine the content of samarium in the complex. The fluorescence emission intensity of the complex was measured by fluorescence emission spectroscopy. The relationship between the fluorescence emission intensity and the content of samarium ion in the complex was investigated. Heating coordination for comparison. The magnetic properties of ligands and complexes were measured by magnetization curves. The experimental results show that the complexes show only the weak characteristic peak of samarium ions, indicating that the first excited state of samarium ions and the triplet energy of the ligand do not match well, but the fluorescence emission The intensity increases with the increase of the content of samarium ions in the complex, indicating that the samarium ions are uniformly distributed in the complex. In addition the complex shows excellent magnetic properties of rare earth ions.