六次甲基四胺合锶配合物的合成与表征

摘要

Strontium-hexamine complex was prepared by using liquid phase synthesis method.The products were tested by using fourier transform infrared spectrometer(FTIR),thermogravimetry-differential thermal analysis(TG-DTA) and X-radiffraction(XRD).The contents of Sr2+,NO-3 and C6H12N4 were analyzed by adopting chemical analysis method.The results show that the best experimental conditions are that the molar ratio of strontium nitrate and hexamethylene tetramine is 1∶2,at 85℃ heated in a water bath,stirring speed of 180r/min,the reaction time is 60min.The yields of the strontium-hexamine complex are not less than 63%.Based on the analysis curves of TG-DTA,the three endothermic peaks respectively represent complex dissociation and the sublimation of hexamethylene tetramine between 79.25℃ and 220.39℃.Its total mass loss is-55.7%.The endothermic peak between 510.6℃ and 658.6℃ is the thermal decomposition of strontium nitrate.Its mass loss is-22.9%.The residue content of strontium oxide is 21.4%.The chemical analysis results of the product component are Sr2+ 17.3%,NO-3 25.5%,C6H12N4 57.3%.The possible formula of the strontium-hexamine complex is [Sr(C6H12N4)2](NO3)2.%以硝酸锶与六次甲基四胺为原料,利用液相合成法制备六次甲基四胺和锶的配合物.基于正交试验探讨合成反应最佳条件,利用傅立叶变换红外光谱仪、X射线衍射仪及热重-差热分析对产物进行表征,通过化学分析测试Sr2+、NO-3和C6H12N4的含量.结果表明:硝酸锶与六次甲基四胺的摩尔比为1∶2,在85℃的水浴中加热,搅拌速度为180r/min,反应60min条件下,目标产物的产率不低于63%.六次甲基四胺合锶配合物在79.25~220.39℃出现三个吸热峰,失重率为-55.7%,此阶段主要是配合物的解离和六次甲基四胺的蒸发过程;在510.6~658.6℃之间的吸热峰为硝酸锶的热分解过程,失重率为-22.9%,残渣量为21.4%,主要为氧化锶.产物成分化学分析的结果是Sr2+ 17.3%、NO-325.5%、C6H12N4 57.3%.并推测出该配合物产物分子式可能为[Sr(C6H12N4)2](NO3)2.