杂化多硫代钼酸铵的合成及表征

SYNTHESIS AND CHARACTERIZATION OF HYBRID AMMONIUM POLYTHIOSULFATE

采用水-乙醇混合溶液为溶剂,将三氧化钼与氨水、硫化铵、硫置于压力釜中,通入氮气保护,通过水热合成方法。制备得到杂化多硫代钼酸铵。通过红外光谱、热重分析表征,用X-射线衍射测定了化合物的单晶结构。单晶解析表明:分子量:740.68,晶胞参数:a=1.161 8(3)nm,b=1.645 0(4)nm,c=0.571 8(13)nm,α=90°,β=117.288(6)°,γ=90°,V=96.954 nm,Z=2。R1=0.045 9,wR2=0.123 6。

By hydrothermal synthesis method,with the solvent of mixed solution of water and ethanol,molybdenum oxide,sulfur,ammonia,ammonium sulphide were dissolved in autoclave,and bubbled into nitrogen. A novel hybrid ammonium polythiosulfate was synthesized and characterized by IR and TGA. Its crystal structure analysis reveals that the compound was determined by single crystal X-ray diffraction. The crystal structure is orthorhombic in the space group Cmca. Crystallographic data are as follow： Mr = 740. 68,a = 1. 161 8（ 3） nm,b = 1. 645 0（ 4） nm,c = 0. 571 8（ 13） nm,α = 90°,β = 117. 288（ 6） °,γ = 90°,V = 96. 954 nm,Z = 2,R1 = 0. 045 9,wR2 = 0. 123 6.