水热条件下金属—有机配位聚合物的合成
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摘要
金属-有机配位聚合物是由金属中心离子与有机配体自组装而形成的。金属-有机配位聚合物新颖的多样结构导致其许多特殊的性能。
本文通过水热法合成了一系列具有新型结构的金属-有机配位聚合物,并通过红外光谱、元素分析、X-射线单晶衍射和热重分析等分析方法,对其的结构和热稳定性进行了表征。
利用单一配体邻苯二甲酸、均苯三甲酸和异烟酸合成了四种简单的金属-有机配位聚合物:(1) [Cd(1,2-BDC)2·H2O]n,(2) [Cd2Na2(BTC)2(H2O)4]n,(3) [Cd(C6H 4O2N)2·4H2O]n,(4)[Co(C6H4O2N)2·4H2O]n。其中,配合物(2)具有双核中心,并且多齿配体均苯三甲酸中羧基具有两种配位形式。研究了影响水热合成的条件:pH值、反应温度、反应时间、降温速率、反应物的摩尔比和反应容器等的影响,确定了合成适合X射线衍射尺寸的单晶的反应条件:反应前电磁搅1h,160~180℃下恒温水热反应4天,降温速率为6℃/h。
利用线性双齿配体4,4'-联吡啶、咪唑等合成了四种混配的金属-有机配合物:(5)[Mn(4,4'-bipy)(1,3-BDC)]n,(6) [Cd(4,4'-bipy)(C3H4N2)2]n,(7) {[Cd(4,4'-bipy)(CH3COO)2]·H2O}n,(8) [Zn(1,2-BDC)(C3H4N2)2]n。配合物(5)、(6)和(7)通过分子间氢键连接以及π-π堆积作用形成三维结构,配合物(8)是通过咪唑配体和邻苯二甲酸形成一维链状结构。
利用2,2'-联吡啶合成了三种混配的金属-有机配位聚合物:(9) [Zn2(OH) (BTC) (2, 2'-bipy)]n,(10) [Cd(C2H2O4) (2,2'-bipy)]n,(11) [Cd Br2 (2, 2'- bipy)]n,分别具有三维、二维和一维结构。配合物(9)中的Zn(II)具有两种不同的配位环境,多齿配体均苯三甲酸中羧基的氧原子具有多种配位形式。
Metal-organic coordination polymers are a type of self-assembly formed by organic ligands and metal ions. Diversified structures of the coordination polymers result in unusual properties of the novel materials.
In this thesis, eleven metal-organic coordination polymers with novel structures were hydrothermally synthesized. Structure and thermal stabilization of the eleven kinds of coordination polymers were characterized by many kinds of analysis methods, such as infrared spectra, element analysis, X-ray single crystal diffraction and thermal gravity analysis.
Four simple metal-organic coordination polymers were synthesized using 1,2- H2BDC(1,2-benzendicarboxylic acid)、H3BTC (1, 3, 5-benzentricarboxylic acid ) and isonicotinic acid. There are two mental centers in coordination polymer(2) and the carboxyl of the H3BTC ligand have two coordinated styles. Moreover, several factors in the hydrothermal synthesis have been studied: pH value、action temperature、action time、cooling rate、mole proportion of the reactant and reaction vessel. The condition of hydrothermal reaction of which products are suited for single-crystal X-ray study was conformed. The pH of the solution was adjusted to 6.5 and the resulting suspension was stirred for 1h, then reacted at 160～180℃for 4 days and cooled at the rate of 6℃/h.
Four metal-organic coordination polymers were synthesized using linear ligand 4,4'-bipyridine. Coordination (5)、(6) and (7) was formed three dimensional structure by hydrogen bonds andπ-πinteractions. Coordination (8) was formed one dimensional structure by the imidazole and 1,2-H2BDC ligand.
Three metal-organic coordination polymers which have three、two and one dimensional structure, respectively, were synthesized using 2,2'- bipyridine. Zn(II) in coordination (9) have two different coordinated environments.
本文通过水热法合成了一系列具有新型结构的金属-有机配位聚合物,并通过红外光谱、元素分析、X-射线单晶衍射和热重分析等分析方法,对其的结构和热稳定性进行了表征。
利用单一配体邻苯二甲酸、均苯三甲酸和异烟酸合成了四种简单的金属-有机配位聚合物:(1) [Cd(1,2-BDC)2·H2O]n,(2) [Cd2Na2(BTC)2(H2O)4]n,(3) [Cd(C6H 4O2N)2·4H2O]n,(4)[Co(C6H4O2N)2·4H2O]n。其中,配合物(2)具有双核中心,并且多齿配体均苯三甲酸中羧基具有两种配位形式。研究了影响水热合成的条件:pH值、反应温度、反应时间、降温速率、反应物的摩尔比和反应容器等的影响,确定了合成适合X射线衍射尺寸的单晶的反应条件:反应前电磁搅1h,160~180℃下恒温水热反应4天,降温速率为6℃/h。
利用线性双齿配体4,4'-联吡啶、咪唑等合成了四种混配的金属-有机配合物:(5)[Mn(4,4'-bipy)(1,3-BDC)]n,(6) [Cd(4,4'-bipy)(C3H4N2)2]n,(7) {[Cd(4,4'-bipy)(CH3COO)2]·H2O}n,(8) [Zn(1,2-BDC)(C3H4N2)2]n。配合物(5)、(6)和(7)通过分子间氢键连接以及π-π堆积作用形成三维结构,配合物(8)是通过咪唑配体和邻苯二甲酸形成一维链状结构。
利用2,2'-联吡啶合成了三种混配的金属-有机配位聚合物:(9) [Zn2(OH) (BTC) (2, 2'-bipy)]n,(10) [Cd(C2H2O4) (2,2'-bipy)]n,(11) [Cd Br2 (2, 2'- bipy)]n,分别具有三维、二维和一维结构。配合物(9)中的Zn(II)具有两种不同的配位环境,多齿配体均苯三甲酸中羧基的氧原子具有多种配位形式。
Metal-organic coordination polymers are a type of self-assembly formed by organic ligands and metal ions. Diversified structures of the coordination polymers result in unusual properties of the novel materials.
In this thesis, eleven metal-organic coordination polymers with novel structures were hydrothermally synthesized. Structure and thermal stabilization of the eleven kinds of coordination polymers were characterized by many kinds of analysis methods, such as infrared spectra, element analysis, X-ray single crystal diffraction and thermal gravity analysis.
Four simple metal-organic coordination polymers were synthesized using 1,2- H2BDC(1,2-benzendicarboxylic acid)、H3BTC (1, 3, 5-benzentricarboxylic acid ) and isonicotinic acid. There are two mental centers in coordination polymer(2) and the carboxyl of the H3BTC ligand have two coordinated styles. Moreover, several factors in the hydrothermal synthesis have been studied: pH value、action temperature、action time、cooling rate、mole proportion of the reactant and reaction vessel. The condition of hydrothermal reaction of which products are suited for single-crystal X-ray study was conformed. The pH of the solution was adjusted to 6.5 and the resulting suspension was stirred for 1h, then reacted at 160～180℃for 4 days and cooled at the rate of 6℃/h.
Four metal-organic coordination polymers were synthesized using linear ligand 4,4'-bipyridine. Coordination (5)、(6) and (7) was formed three dimensional structure by hydrogen bonds andπ-πinteractions. Coordination (8) was formed one dimensional structure by the imidazole and 1,2-H2BDC ligand.
Three metal-organic coordination polymers which have three、two and one dimensional structure, respectively, were synthesized using 2,2'- bipyridine. Zn(II) in coordination (9) have two different coordinated environments.
引文
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