多胺合金属配合物的固相合成表征及性质测定

要：分别以氯化铜、醋酸锌和尿素为原料、通过室温固相合成法得到了二氯化四尿素合铜(II) {Cu{OC(NH2) 2}4Cl2和二醋酸四尿素合锌(II) {Zn[OC(NH2)2]4}(C4H6O4)两种固相配合物．采用化学分析方法、IR、TG—DSC，DSC等手段对其组成、结构、热稳定性等性能进行了表征．结果表明，Cu(Ⅱ)与尿素的物质的量之比为1:4，分子式为{Cu{OC(NH2) 2}4Cl2，配位原子为羰基氧原子，尿素与铜形成配合物后热稳定性增加，二氯化四尿素合铜(II)的熔融焓为52.36J/g，熔融温度为98.51℃，二氯化四尿素合铜(II)中第二个分解过程反应的Ea=178.28 kJ/mol，k0=1.52*1018mol/(min*L)；配合物中Zn(Ⅱ)与尿素的物质的量之比为1:4，分子式为{Zn[OC(NH2)2]4}(C4H6O4) ，配位原子为羰基氧原子，尿素与锌形成配合物后，热稳定性减小，二醋酸四尿素合锌(II)的熔融焓为84.49J/g，熔融温度为111.14℃，二醋酸四尿素合锌(II)中分解过程反应的Ea=167.97kJ/mol，k0=5.86*1020mol/(min*L)。7145
关键字：室温固相合成；固相合成；二氯化四尿素合铜(II)；二醋酸四尿素合锌(II)；尿素
Solid State Synthesis and Characteristies of the Polyamine Metal Complexes in Room Temperature
Abstract：{Cu{OC(NH2) 2}4Cl2和{Zn[OC(NH2)2]4}(C4H6O4) were synthesized by the room tempreature solid state synthesis with the material of copper chloride, zinc acetate and urea. Their composition, structure, and thermostability were characterized by the chemical analysis, IR, and TG—DSC, DSC. The results showed that the mole ratio of copper salt and urea was 1:4, the molecular formula is {Cu{OC(NH2) 2}4Cl2, the coordination bond is the oxygen of the carbonyl, the thermostability of coordinated urea was lifted, the enthalpy during melting down is 52.36J/g, the melting point is 98.51℃, Ea=178.28 kJ/mol, k0=1.52*1018mol/(min*L) in the second decomposition period. the mole ratio of zinc salt and urea was 1:4, the molecular formula is{Zn[OC(NH2)2]4}(C4H6O4), the coordination bond is the oxygen of the carbonyl, the thermostability of coordinated urea was reduced, the enthalpy during melting down is 84.49J/g, the melting point is 111.14℃, Ea=167.97kJ/mol，k0=5.86*1020mol/(min*L) in the decomposition period.
KeyWords： solid state synthesis in room temperature; solid state synthesis; copper(II) dichloride tetracarbamide complex; zinc(II) diacetate tetracarbamide complex; urea

目录

1 前言   1
1.1 开题依据   1
1.2 文献综述   1
1.2.1组合化学   1
1.2.2固相合成法   2
1.2.3室温固相合成   4
1.2.4室温固相合成法在合成多胺合金属配合物的进展   8
1.3 本课题研究的方向和内容   10
2 实验   12
2.1 主要仪器与试剂   12
2.1.1 实验仪器   12
2.1.2 实验试剂   12
2.2 配合物的合成   13
2.2.1 二氯化四尿素合铜(II)配合物的合成   13
2.2.2 二醋酸四尿素合锌(II)配合物的合成   13
2.3 配合物的组成分析   13
2.3.1 原子吸收法测定铜、锌的含量测定   13
2.3.2 尿素合铜(II)中Cl元素的含量测定   15
2.3.3 用元素分析仪测定C、H、O元素的含量   15
2.4 配合物的热稳定性分析   15
2.4.1 尿素的热稳定性分析   15
2.4.2 尿素合铜(II)的热稳定性分析   16
2.4.3尿素合锌(II)的热稳定性分析   16
2.4.4尿素合铜(II)的DSC分析   16
2.4.5尿素合锌(II)的DSC分析   17
2.5 配合物的结构分析   17 多胺合金属配合物的固相合成表征及性质测定:http://www.youerw.com/huaxue/lunwen_4949.html