摘要
在甲醇中,利用水杨醛-1H-苯并三唑-1-乙酰腙(C15H13N5O2,简称SBTH)与高氯酸镧反应,制得一新配合物,经元素分析、化学分析并结合热分析确定了其组成为La(C;。11;。N。O。)(C;。H。刀。口。)·2.SH。O 利用电导测定、红外光谱、1HNMR和TG-DTG等手段推测了配合物的结构.用微热量计测定了配合物在不同浓度(b)时的溶解焙,用计算机拟合求得该配合物的标准摩尔溶解烩(△solHm(?)=-135.62kJ·mol-1)及溶解焓(△solH)的经验公式(△solH=-135.62-11633b+3761.5b1/2),并由此分别推导出配合物的相对表观摩尔焓(φLi)、相对偏摩尔烙(Li)以及配合物稀释焓(△dilH1,2)的经验公式:φLi=-11633b+3761.5b1/2;Li=-23266b+5642.2b1/2和△dilH1,2=-11633(b2 1/2-b1 1/2)+3761.5(b2-b1)还研究了配合物的热分解过程,利用Kissinger公式计算了配合物主要分解阶段的表观活化能(Es=470.24KJ·mol-1).
A new rare earth complex La(C15H12N5O2) (C15H11N5O2). 2. 5H2O has been synthesized. Attempts have been made to ascertain its probable structure on the basis of elemental analyzes, molar conductivities, IR, 1H NMR and TG-DTG. It is suggested that the complex has a eight-coordinated configuration. The enthalpies of solution in DMF for the complex were measured by means of a microcalorimeter. The data of standard molar enthalpy of solution (Asol//m=-135.62 kJ. mol-1) and the empirical formulae of enthalpy of solution (sol H=- 135. 62 - 116336 + 3761. 5b1/2) for the complex at different concentration b (mol .kg-1) were obtained. And relative apparent molar enthalpy ( Li), relative partial molar enthalpy (L,) and enthalpy of dilution (dil H1, 2) were drawn up respectively by the data of enthalpies of solution of the complex: L1 = - 11633b + 2761.5b1/2, L,=-23266b+5642.2b1/2 and dil H1, 2=-11633(b1/21 ~ b1/21) +3761.5(b2-b1) .The second-stage decomposition reaction for the complex was studied and the apparent activation energy was obtained by the Kissinger's formulae.
出处
《物理化学学报》
SCIE
CAS
CSCD
北大核心
2002年第10期865-870,共6页
Acta Physico-Chimica Sinica
基金
陕西省自然科学基金(98H010)资助项目
陕西省教委专项基金资助项目
稀土材料化学及应用国家重点实验室开放课题