三水硝酸镝与苯并-15-冠-5在丙酮中配合行为的研究  

Studies on Coordination Behavior Between Dy (NO_3)_3·3H_2O and Crown Ether B15C5 in Acetone

作　　者：任德厚[1] 薛鸿福 刘丽娜[1] 刘子如[2] 阴翠梅[2] 

机构地区：[1]西北大学化学系 [2]西安近代化学研究所

出　　处：《化学学报》1989年第4期372-376,共5页Acta Chimica Sinica

基　　金：国然自然科学基金

摘　　要：近年来,稀土冠醚配合物的研究迅速增多。但是,一般多采用合成的方法,King等对于稀土硝酸盐制得组成为Ln（NO₃）₃·B15C5·3H₂O·CH₃COCH₃的配合物（Ln=Sm—Lu）。而Seminara等制得的却为无水无溶剂的配合物Ln（NO₃）₃·B15C5。为了进一步弄清楚Dy（NO₃）₃·3H₂O与B15C5在丙酮中的配合行为,我们用改进的半微量相平衡方法研究了Dy（NO₃）₃·3H₂O-B15C5-CH₃COCH₃三元体系在18℃时的溶解度,并进一步分离制备配合物,研究了配合物的红外光谱、热力学等性质。The solubilities of the ternary system, Dy(NO_3)_3·3H_2O-B15C5-CH_3COCH_3 at 18℃ have been investigated through the study of phase equilibrium using the modified semimicro method. The results indicated that the solubility curve of this system consists of two branch lines, the long branch corresponds to the solid phase of the complex, Dy(NO_3)_3·B15C5·3H_2O·2CH_3COCH_3; the short one to the solid phase of B15C5. The curve of refractive indices for saturated solutions also consists of two branch lines, which corresponds to the two branch lines of solubility curve. No complex species with different Dy/crown ratio has been found. The behavior of water in the equilibrium system has been examined. The results indicate that the mole ratio, H_2O/Dy(NO_3)_3, is always 3:1 either in liquid or solid phase. The complex has been isolated and shown the composition of Dy(NO_3)_3·B15C5· 3H_2O·0.65CH_3COCH_3. The properties of this complex have been examined by infrared spectra, DTA, TG and DSC. The enthalpies of desolvent and thermal decomposition have beeo determined by DSC. The apparent activation energy of the thermal decomposition has been found to be 117.46 kJ/mol from DSC curves using Kissinger method.

关 键 词：镝配合物 冠醚 丙酮 

分 类 号：O614.342[理学—无机化学]