由邻菲罗啉衍生物构筑的过渡金属配合物的合成、表征及其对染料的催化降解作用
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摘要
随着现代社会的快速发展,具有特殊功能的材料,如具有光电性能优点、磁性能及环境友好的光催化功能材料,成为科学研究的热点。配合物材料,不仅具有多样性的价键形成和新颖的空间结构,而且还具有特殊的光、电、磁性及催化性能,特别是在环境污染物催化降解处理方面应用的可行性,引起研究者广泛的兴趣。过渡金属配合物整合了金属和聚合物的诸多优点,在清洁能源、智能响应材料、高性能器件制备方面具有广泛的应用潜力。水热法合成的密闭条件有利于进行那些对人体健康有毒有害的反应体系,尽可能的减少环境污染,整个实验过程属于绿色环保的过程。本论文通过水热合成的方法制备了17个结构新颖的过渡金属配合物,采用X-单晶衍射仪对配合物的结构进行了测定,并对其光学、磁学和光催化性能进行了研究。
本课题开展了以下两个方面的研究工作：
首先,我们利用邻菲罗啉衍生物{2-(4-甲氧基)-1氢-咪唑[4,5-f][1,10]邻菲罗啉,MOPIP和2-(9-葸)-1氢-咪唑[4,5-f][1,10]邻菲罗啉,AIP}合成了10个过渡金属配合物：[Cd4(MOPIP),2]·(H2O)9 (1), [Mn2(MOPIP)6]·(H2O)6 (2), [Cu(MOPIP)2]·(OH)2 (3), [Ni(MOPIP)3]·H2O·C6H5O3 (4), [Ag2(MOPIP)(HMOPIP)]n·nNO3·1.5n H2O (5), [Cr(MOPIP)2]Cl (6), [Co(MOPIP)(HMOPIP)2]·(OH)2·3H2O (7), [Cu2(MOPIP)2]n (8), [Zr(MOPIP)3]·(OH)·3H2O (9),[Co(AIP)(HAIP)2](OH)2 (10)。在配合物(1)、(2)、(4)、(7)、(9)、(10)中,每个金属中心离子与来自三个不同HMOPIP或MOPIP(HAIP或AIP)上的六个氮原子进行配位,形成畸变的八面体构型。在配合物(3)、(6)中,每个中心离子与来自两个不同MOPIP分子上的氮原子形成四配位的四面体结构,配合物(5)、(8)为一维链状结构,其中心离子分别与来自于不同HMOPIP和MOPIP配体上的三个氮原子配位,分别形成三配位畸变的三角形构型。利用Guassian 03程序对配合物(3)和(6)进行了自然键轨道分析(NBO)。对配合物(2)、(3)和(4)分别进行了光催化降解染料试验,结果表明配合物(3)的催化降解效果比较好,在废水处理方面具有潜在的应用价值。
其次,我们利用邻菲罗啉衍生物(2-甲基吡嗪[3,2-f：2',3'-h]喹喔啉,Medpq)和芳香羧酸(1,2-H2BDC=1,2-苯二甲酸,1,4-H2BDC=1,4-苯二甲酸,H2PDC=2,3-吡啶二羧酸)作为共配体,与过渡金属配位,合成了7个过渡金属配合物：[Ni(1,2-BDC)(Medpq)(H2O)3] (11), [Cd(1,4-BDC)(Medpq)·H2O]n (12), [Co(1,4-BDC)(Medpq)·H2O]n (13), [Co(Medpq)(PDC)·H2O]2n·2.4nH2O(14), [Cd(Medpq)(PDC)·H2O]n·nH2O (15),{[Mn(1,2-BDC)(Medpq)(H2O)]·0.25nH2O}n (16), [Mn(Medpq)(PDC)·H2O]n·2nH2O (17)。在配合物(11)中,整个晶体由1,2-BDC-Ni-Medpq单元组成零维结构。配合物(12)-(17)均为一维无限链状结构。应用Guassian 03程序对配合物(11)进行了自然键轨道分析(NBO),结果表明Ni(Ⅱ)与配位原子间的价键类型都属于共价键范畴。在比较配合物(12)、(14)和(15)的发光性能中发现,配合物(12)和(15)具有较好的发光性能,发光峰位分别位于567.7nm(黄光)以及638.7 nm(橙色光)处。对配合物(12)和(13)进行了染料光催化降解实验,研究结果显示,(12)的催化效果要好于(13)。
With the rapid development of modern society, materials with special functions, such as optical and electrical properties, magnetic properties and photocatalytic properties, have become a hot topic of scientific research. Complex, a kind of meaterial with not only great variety of bond and novel spatial structure but the special optical, electric, magnetic and catalytic properties, especially the feasibility of application in the photocatalytic degradation of environmental pollution, has been received much attention. The transition metal complexes possess the merits of both metal and polymer and have wide potential in clean power source, smart response materials and high-performance devices. The airtight conditions of hydrothermal synthesis are in favor of processing those harmful and toxic reaction, which can reduce the environmental pollution as much as possible and the entire experimental process belongs to the one of green environmental protection. In this paper, seventeen novel transition metal complexes were prepared by hydrothermal synthesis method. Their structures were characterized by X-ray crystal diffraction. The optical, magnetic, and photocatalytic properties of these complexes were investigated.
Two aspects of research work in this paper is shown in the following:
Firstly, ten new compounds, namely [Cd4(MOPIP)12]·(H2O)9 (1), [Mn2(MOPIP)6]·(H2O)6 (2), [Cu(MOPIP)2]-(OH)2 (3), [Ni(MOPIP)3]·H2O·C6H5O3 (4), [Ag2(MOPIP)(HMOPIP)]n·nNO3·1.5n H2O (5), [Cr(MOPIP)2]Cl (6), [Co(MOPIP)(HMOPIP)2](OH)2·3H2O (7),[Cu2(MOPIP)2]n (8), [Zr(MOPIP)3]-(OH)·3H2O (9), [Co(AIP)(HAIP)2](OH)2 (10), based on 1,10-phenanthroline derivatives (2-(4-methoxyphenyl) -1H-imidazo[4,5-f][1,10] phenanthroline, MOPIP and 2-(9-anthryl) -1H-imidazo[4,5-f][1,10] phenanthroline, AIP) were synthesized under hydrothermal conditions. In (1), (2), (4), (7), (9) and (10), every metal ion is hexa-coordinated with six nitrogen atoms from three different MOPIP ligands in the crystal structure, showing a slightly distorted octahedral geometry. In the complexes (3) and (6), the each center ion is coordinated with four nitrogen atoms from two different MOPIP molecules, showing tetrahedronal structure. The complexes (5) and (8) are one-dimensional chains. In (5) and (8), the each center ion is three-coordinated with three nitrogen atoms from different HMOPIP and MOPIP ligands, assuming a slightly distorted triangle, respectively. The quantum chemical calculation and analysis of the natural bond orbital (NBO) of (3) and (6) was performed by using the Gaussia 03 Program. The photocatalytic activity of complexes (2), (3) and (4) was investigated by degradation of dye, respectively. The results show that the catalytic degradation rate of complex (3) is much higher than the others. Thus, complex (3) has the potential application in wastewater treatment.
Secondly, seven new compounds, viz. [Ni(1,2-BDC)(Medpq)(H2O)3] (11), [Cd(1,4-BDC)(Medpq)·H2O]n (12), [Co(1,4-BDC)(Medpq)·H2O]n (13), [Co(Medpq)(PDC)·H2O]2n·2.4nH2O (14), [Cd(Medpq)(PDC)·H2O] n·nH2O(15),{[Mn(1,2-BDC)(Medpq)(H2O)]·0.25nH2O}n (16), [Mn(Medpq)(PDC)·H2O]n·2nH2O (17), based on 1,10-phenanthroline derivatives (2-methyldipyrido[3,2-f:2',3'-h] quinoxaline, Medpq) and aromatic carboxylic acid (1,2-H2BDC= 1,2-benzenedicarboxylic acid, 1,4-H2BDC= 1,4-benzenedicarboxylic acid, H2PDC= 2,3-pyridinedicarboxylic acid) as the mixed ligands coordinated with transition metal, were synthesized under hydrothermal conditions. Compound (11) exhibits a zero-dimensional structure with 1,2-BDC-Ni-Medpq as building units. Compounds (12)-(17) all exhibit one-dimensional infinite chain structure. The quantum chemical calculation of (11) was performed by using the Gaussian 03 Program. The results show that the valence-bond of Ni(Ⅱ) and the coordinated atoms all belong to the covalent bond category. Comparing with complex (14), the fluorescent properties of complexes (12), (15) were relatively better. The emission bands of complexes (12) and (15) are located at 567.7 nm (yellow light) and 638.7 nm (orange light), respectively. The photocatalytic activity of complexes (12) and (13) was investigated by degradation of dye, respectively. The results show that the catalytic performance of (12) is much better than (13) due to their different central ion.
本课题开展了以下两个方面的研究工作：
首先,我们利用邻菲罗啉衍生物{2-(4-甲氧基)-1氢-咪唑[4,5-f][1,10]邻菲罗啉,MOPIP和2-(9-葸)-1氢-咪唑[4,5-f][1,10]邻菲罗啉,AIP}合成了10个过渡金属配合物：[Cd4(MOPIP),2]·(H2O)9 (1), [Mn2(MOPIP)6]·(H2O)6 (2), [Cu(MOPIP)2]·(OH)2 (3), [Ni(MOPIP)3]·H2O·C6H5O3 (4), [Ag2(MOPIP)(HMOPIP)]n·nNO3·1.5n H2O (5), [Cr(MOPIP)2]Cl (6), [Co(MOPIP)(HMOPIP)2]·(OH)2·3H2O (7), [Cu2(MOPIP)2]n (8), [Zr(MOPIP)3]·(OH)·3H2O (9),[Co(AIP)(HAIP)2](OH)2 (10)。在配合物(1)、(2)、(4)、(7)、(9)、(10)中,每个金属中心离子与来自三个不同HMOPIP或MOPIP(HAIP或AIP)上的六个氮原子进行配位,形成畸变的八面体构型。在配合物(3)、(6)中,每个中心离子与来自两个不同MOPIP分子上的氮原子形成四配位的四面体结构,配合物(5)、(8)为一维链状结构,其中心离子分别与来自于不同HMOPIP和MOPIP配体上的三个氮原子配位,分别形成三配位畸变的三角形构型。利用Guassian 03程序对配合物(3)和(6)进行了自然键轨道分析(NBO)。对配合物(2)、(3)和(4)分别进行了光催化降解染料试验,结果表明配合物(3)的催化降解效果比较好,在废水处理方面具有潜在的应用价值。
其次,我们利用邻菲罗啉衍生物(2-甲基吡嗪[3,2-f：2',3'-h]喹喔啉,Medpq)和芳香羧酸(1,2-H2BDC=1,2-苯二甲酸,1,4-H2BDC=1,4-苯二甲酸,H2PDC=2,3-吡啶二羧酸)作为共配体,与过渡金属配位,合成了7个过渡金属配合物：[Ni(1,2-BDC)(Medpq)(H2O)3] (11), [Cd(1,4-BDC)(Medpq)·H2O]n (12), [Co(1,4-BDC)(Medpq)·H2O]n (13), [Co(Medpq)(PDC)·H2O]2n·2.4nH2O(14), [Cd(Medpq)(PDC)·H2O]n·nH2O (15),{[Mn(1,2-BDC)(Medpq)(H2O)]·0.25nH2O}n (16), [Mn(Medpq)(PDC)·H2O]n·2nH2O (17)。在配合物(11)中,整个晶体由1,2-BDC-Ni-Medpq单元组成零维结构。配合物(12)-(17)均为一维无限链状结构。应用Guassian 03程序对配合物(11)进行了自然键轨道分析(NBO),结果表明Ni(Ⅱ)与配位原子间的价键类型都属于共价键范畴。在比较配合物(12)、(14)和(15)的发光性能中发现,配合物(12)和(15)具有较好的发光性能,发光峰位分别位于567.7nm(黄光)以及638.7 nm(橙色光)处。对配合物(12)和(13)进行了染料光催化降解实验,研究结果显示,(12)的催化效果要好于(13)。
With the rapid development of modern society, materials with special functions, such as optical and electrical properties, magnetic properties and photocatalytic properties, have become a hot topic of scientific research. Complex, a kind of meaterial with not only great variety of bond and novel spatial structure but the special optical, electric, magnetic and catalytic properties, especially the feasibility of application in the photocatalytic degradation of environmental pollution, has been received much attention. The transition metal complexes possess the merits of both metal and polymer and have wide potential in clean power source, smart response materials and high-performance devices. The airtight conditions of hydrothermal synthesis are in favor of processing those harmful and toxic reaction, which can reduce the environmental pollution as much as possible and the entire experimental process belongs to the one of green environmental protection. In this paper, seventeen novel transition metal complexes were prepared by hydrothermal synthesis method. Their structures were characterized by X-ray crystal diffraction. The optical, magnetic, and photocatalytic properties of these complexes were investigated.
Two aspects of research work in this paper is shown in the following:
Firstly, ten new compounds, namely [Cd4(MOPIP)12]·(H2O)9 (1), [Mn2(MOPIP)6]·(H2O)6 (2), [Cu(MOPIP)2]-(OH)2 (3), [Ni(MOPIP)3]·H2O·C6H5O3 (4), [Ag2(MOPIP)(HMOPIP)]n·nNO3·1.5n H2O (5), [Cr(MOPIP)2]Cl (6), [Co(MOPIP)(HMOPIP)2](OH)2·3H2O (7),[Cu2(MOPIP)2]n (8), [Zr(MOPIP)3]-(OH)·3H2O (9), [Co(AIP)(HAIP)2](OH)2 (10), based on 1,10-phenanthroline derivatives (2-(4-methoxyphenyl) -1H-imidazo[4,5-f][1,10] phenanthroline, MOPIP and 2-(9-anthryl) -1H-imidazo[4,5-f][1,10] phenanthroline, AIP) were synthesized under hydrothermal conditions. In (1), (2), (4), (7), (9) and (10), every metal ion is hexa-coordinated with six nitrogen atoms from three different MOPIP ligands in the crystal structure, showing a slightly distorted octahedral geometry. In the complexes (3) and (6), the each center ion is coordinated with four nitrogen atoms from two different MOPIP molecules, showing tetrahedronal structure. The complexes (5) and (8) are one-dimensional chains. In (5) and (8), the each center ion is three-coordinated with three nitrogen atoms from different HMOPIP and MOPIP ligands, assuming a slightly distorted triangle, respectively. The quantum chemical calculation and analysis of the natural bond orbital (NBO) of (3) and (6) was performed by using the Gaussia 03 Program. The photocatalytic activity of complexes (2), (3) and (4) was investigated by degradation of dye, respectively. The results show that the catalytic degradation rate of complex (3) is much higher than the others. Thus, complex (3) has the potential application in wastewater treatment.
Secondly, seven new compounds, viz. [Ni(1,2-BDC)(Medpq)(H2O)3] (11), [Cd(1,4-BDC)(Medpq)·H2O]n (12), [Co(1,4-BDC)(Medpq)·H2O]n (13), [Co(Medpq)(PDC)·H2O]2n·2.4nH2O (14), [Cd(Medpq)(PDC)·H2O] n·nH2O(15),{[Mn(1,2-BDC)(Medpq)(H2O)]·0.25nH2O}n (16), [Mn(Medpq)(PDC)·H2O]n·2nH2O (17), based on 1,10-phenanthroline derivatives (2-methyldipyrido[3,2-f:2',3'-h] quinoxaline, Medpq) and aromatic carboxylic acid (1,2-H2BDC= 1,2-benzenedicarboxylic acid, 1,4-H2BDC= 1,4-benzenedicarboxylic acid, H2PDC= 2,3-pyridinedicarboxylic acid) as the mixed ligands coordinated with transition metal, were synthesized under hydrothermal conditions. Compound (11) exhibits a zero-dimensional structure with 1,2-BDC-Ni-Medpq as building units. Compounds (12)-(17) all exhibit one-dimensional infinite chain structure. The quantum chemical calculation of (11) was performed by using the Gaussian 03 Program. The results show that the valence-bond of Ni(Ⅱ) and the coordinated atoms all belong to the covalent bond category. Comparing with complex (14), the fluorescent properties of complexes (12), (15) were relatively better. The emission bands of complexes (12) and (15) are located at 567.7 nm (yellow light) and 638.7 nm (orange light), respectively. The photocatalytic activity of complexes (12) and (13) was investigated by degradation of dye, respectively. The results show that the catalytic performance of (12) is much better than (13) due to their different central ion.
引文
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