以硫酸铁铵为催化剂,采用微波辐射的方法催化合成乙酸正丁酯。讨论了微波辐射的功率、反应时间、酸醇摩尔比、催化剂的用量以及分水因素对酯化反应的影响。通过单因素实验确定合成乙酸正丁酯的最佳反应条件为:微波辐射功率为240 W,辐射时间为15 m in,催化剂用量为1.3 g,酸醇比为1.2:1.0,酯化率为98.2%。本方法具有反应时间短、反应条件温和、后处理简单且环保无污染等特点。
On the basis of 2,6-bisbenzoylactyl pyridine(L1), 2,6-bis[(3-pyrazoleyl) -5-phenyl]pyridine (L2)and2,6-bis[(3-pyrazoleyl)-3,5-bisphenyl]pyridine(L3) are synthesized. With the synthesized organic compounds as organic ligands, corresponding terbium(Ⅲ) complexes are prepared .The composition of these new compounds are confirmed by 1H-NMR, EA , IR spectrum , UV spectrum and MS .The properties of the complexes are characterized by EA,IR spectrum ,UV spectrum,TG-DTA and fluorescence spectra. Photoluminescence measurements indicate that the effective energy transfer from the organic ligand L2 to the central Tb(Ⅲ) ions occurs in the complexe, and strong and characteristic green mission appears due to the 5D4- 7F5 transitions of the 4f electrons of the central Tb(Ⅲ) ions. The fluorescence spectra shows that the fluorescence emission intensity of Tb(L2) 3·3H2O is stronger than that of Tb2(L1) 3·4H2O,but the property of TG-DTA is not so good as we expected. It cannot be the best material for fabrication of organic light-emitting devices.
