聚酰亚胺与钐的微波辐射固相配位及其性能研究

Study on the Solid Phase Coordination Synthesis of Samarium and Polyimide under Microwave Radiation and its Characterization

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。

Solid phase coordination reaction of samarium ion (Ⅲ) (Sm3+) and the resultant of polycondensation and imidization of benzoguanamine (BGA) and pyromellitic dianhydride (PMDA) under microwave radiation were studied. The effects of microwave radiation time (power), the composition of two reactants and the reaction temperature on the yield and Sm content in the complexes were investigated. The complex was studied by Fourier transform infrared spectrum (FTIR), Fourier transform Roman spectrum (FTRR), scanning electron microscope (SEM), 13C solid state nuclear magnetic resonance spectrometry and X-ray powder diffraction, respectively, and the content of Sm3+ in the complex was measured. The possible structure of the complex was inferred. The fluorescent emission intensity of the complex coordinated under microwave radiation was measured by fluorescent emission spectrum and was compared with the emission intensity of the complex with conventional thermal coordination. The magnetic susceptibilities were measured by magnetic curve. The results showed that the complex only emit quit weak fluorescent peak of characteristic fluorescent of Sm3+, which illustrated that the first excitation level of Sm3+ and that of the complexant can not match very well. The experimental results also showed that the fluorescent emission intensity increased with increasing of Sm content in the complex, which illustrated that Sm3+ was dispersed uniformly in the complex, and that the complex showed good magnetic property of the rare earth ion.