Dy(NO_3)_3·3H_2O与B15C5在无水乙醇中配合行为的研究

Studies on Coordination Behavior between Dy(NO_3)_3·3H_2O and Crown Ether BI5C5 in Absolute Alcohol

用改进的半微量相平衡方法研究了Dy(NO_3)_3·3H_2O—B15C5一C_2H_5OH三元体系在18℃时的溶解度,测定了该体系在18℃各饱和溶液的折光率。结果表明,该体系中只有一种化学计量为Dy(NO_3)8·B15C5·3H_2O·2.5C_2H_5OH的配合物生成,配合物与冠醚B15C5的共饱和点组成为:Dy(NO_3)_3·3H_2O 19.04％;B15C5 28.42％;C_2H_5OH 52.54％.考查了相平衡过程中水的行为。经分离、洗涤及浓硫酸干燥恒重后,配合物的组成变为:Dy(NO_3)_3·B15C5·3H_2O·0.65C_2H_5OH.通过化学分析、紫外与红外光谱分析、DTG,TG及DSC研究了配合物的组成和性质。测定了配合物的脱溶剂、热分解过程的热效应。在常量情况下,考查了配合物的热失重情况。

The solubilities of the ternary system, Dy(NO_3)_3·3H_2O-B15C5-C_2H_5OH, at 18℃have been investigated by the modified semimicro method to study phase equilibrium. The refractive indices for satuated solutions at 18℃have been determined for this system. The results indi- cated that there is only one stoichiometry complex formed in the ternary system. The eutonic point of complex and crown ether B15C5 occurs at 19.04% Dy(NO_3)_3H_2O, 28.42% B15C5, 52.54% C_2H_5OH. The behavior of water for this system in equilibrium has been examined. The complex has been isolated, washed and dried in a dessicator charged with concentrated. salphric acid until constant weight was attained. The dried samples have the composition of Dy(NO_3)_3·B15C5·3H_2O.0.65C_2H_5OH. The properties of this complex have been investigated by chemical analysis, UV-spectra, infrared spectra, DTG and TG. The enthalpies of desolvent and decomposition have been determined by DSC. The weightless processes of the complex have also been examined with the dried samples of 100～200mg.