邻香兰素乙二胺合镍(Ⅱ)配合物的合成、晶体结构及热分解动力学的研究

Studies on Synthesis, Crystal Structure and Kinetics of Thermal Decomposition of o-Vanillin Ethylenediamine Nickel (Ⅱ)

X射线单晶衍射结果表明,邻香兰素乙二胺合镍(Ⅱ)(Ni-Vaniethy)C_(18)H_(18)N_2NiO_4·H_2O为正交晶系,空间群Pbna,晶胞参数a=1.1931(3)nm,b=1.5233(4)nm,c=1.9592(6)nm,V=3.561nm^3,M=403.08,Z=8,D_c=1.50g/cm^3,μ=11.23cm^(-1),F(000)=1680,最后偏离因子R=0.071.利用TG、DTG曲线对配合物进行了非等温动力学研究,得到了其热分解动力学参数.并探讨了反应的可能机理.

The crystal of o-vanillin ethylenediamine Nickel ( Ⅰ ) (Ni-Vaniethy) C18H18N2NiO4 · H2O was synthesized and its structure was determined by single crystal X-ray diffraction method. The complex belongs to the orthorhombic system, space group Pbna with cell parameters of a?1. 1931(3) nm, b=1.5233(4) nm, c=1. 9592(6) nm, V=3. 561 (nm)3, M=403. 08, Z=8, Dc = 1. 50 g/cm3, μ-11.23 cm-1, F(000) = 1680, final R=0. 071 for 1200 unique reflections [I≥3(σ)]. The kinetics of thermal decomposition reaction of the complex was studied under a non-isothermal condition by TG. The kinetic parameters were obtained from the analysis of TG, DTG curves by integral and differential methods. The functions of thermal decomposition reaction mechanism are:f(a)=2(1-a)1/2,g(a)=1-(1-a)1/2.