含N/O配体配合物的合成、表征及草酸铁配合物光催化降解次甲基蓝研究
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摘要
配合物作为一种新型分子功能材料不仅具有丰富的拓扑结构和多样的堆积方式，而且在有机废水的处理、光催化性能、气体存储、分离、热稳定性、光学性能、机械性能、磁学性能等领域具有巨大的应用潜力。晶体工程涉及分子或化学基团在晶体中的行为、晶体的设计、结构与性能的控制以及晶体结构预测，它是实现从分子到功能材料的一条重要途径。而设计与合成结构新颖且在环境领域内具有潜在应用价值的配合物和无机一有机杂化材料是晶体工程学研究的两个重要的方面。
本文以芳香羧酸及其取代物为配体，与过渡金属盐反应合成了6个配合物Cu(phth)_2(H_2O)_2(1)、Ni(H_2O)_6·(μ-H_2O)_2·K_2(phth)_4(H_2O)(2)、[Cu(H_2O)_6][Na_2(SO_4)_2]，(3)、Cu(H_2O)(C_6H_6NSO_3)2·2H_2O(4)、Cd(C_7H_5O_4)2·3H_2O]·2H_2O(5)、[Ni_2(C_7H_5O_4)_4·2H_2O](6)。以咪唑或六次甲基四胺为配体合成了四个配合物，[Cu(im)_6]Cl_2·4H_2O(7)、[Cu(im)_6]Cl_2·2H_2O(8)、[Cu(H_2O)_6]Cl_2·2{(CH_2)_6N_4)·4H_2O(9)、[Ag_2(C_6H_(12)N_4)_2Cr_2O_7·H_2O(10)。
配合物1晶体属单斜晶系，空间群为P2(1)／c,Z=2，a=8．3895(17)(?)，b=14．441(3)(?)，c=7．0992(14)(?)，α=90°，p=112．14(3)°，γ=90°。配合物2晶体属单斜晶系，空间群为P2(1)／c，Z=2，a=10．455(2)(?)，b=6．8670(14)(?)，c=29．704(6)(?)，α=90°，β=98．14(3)°，γ=90°。配合物3品体属单斜品系，空间群为P2(1)／c，Z=2，a=6．2345(12)(?)，b=12．333(3)(?)，c=9．1822(18)(?)，a=90°，β=105．56(3)°，γ=90°。配合物4晶体属单斜品系，空间群为P2(1)／n，Z=2，a=7．4485(8)(?)，b=17．4102(19)(?)，c=7．6509(9)(?)，α=90°，β=116．6880(10)°，γ=90°。配合物5晶体属单斜品系，空间群为P2(1)／c，Z=4，a=7．8338(8)(?)，b=19．8658(19)(?)，c=12．2359(12)(?)，α=90°，β=105．8920(10)°，γ=90°。配合物6晶体属单斜晶系，空间群为P21／n，Z=2，a=8．2698(2)(?)，b=19．4936(8)(?)，c=9．9987(4)(?)，α=90°，β=102．641(3)°，γ=90°。配合物7晶体属三斜晶系，空间群为P-1，Z=1，a=8．8097(18)(?)，b=9．0812(18)(?)，c=10．586(2)(?)，α=75．08(3)°，β=83．14(3)°，γ=61．84(3)°。配合物8晶体属单斜晶系，空问群为P21／n，Z=2，a=8．073(2)(?)，b=13．239(2)(?)，c=15．0810(10)(?)，α=90°，β=97．940(10)°，γ=90°。配合物9晶体属三斜晶系，空间群为P-1，Z=1，a=9．321(3)(?)，b=9．3923(16)(?)，c=9．4261(16)(?)，α=119．523(2)°，β=94．153(3)°，γ=101．065(3)°。配合物10晶体属单斜晶系，空间群为P21／n，Z=4，a=11．1095(16)(?)，b=10．9848(14)(?)，c=14．101(2)(?)，α=90°，β=100．131(2)°，γ=90°。用X射线衍射法对配合物品体结构进行了测定，解析了单晶结构，用元素分析、红外光谱、差热一热重分析等方法对上述配合物进行了结构表征。单晶结构分析发现，合成的方法、pH值、溶剂、温度、反应时间、氢键能显著影响配合物配位环境和晶体堆积。
近年来，随着环境污染的同益严重，环境问题越来越受到人们的重视，寻求一种广谱、高效、低廉的方法对难降解有机废水的处理是近年环境科学研究的热点之一。本文以合成的二元羧酸的配合物草酸铁为例，讨论了它对次甲基蓝的光降解，研究了不同双氧水浓度、溶液pH值等对次甲基蓝降解速率的影响，脱色降解反应均符合一级动力学反应，表明过渡金属的配合物草酸铁可有效处理难降解有机废水，与传统高级氧化方法相比，具有反应快速、操作简单等优点。
As new type of molecular functional materials, coordination compounds are not only a wealth of topology and the accumulation variety of ways, but also have tremendous potential such as in gas in storage, separation, catalytic properties, thermal stability, optical properties, mechanical properties, magnetic properties and so on. Crystal engineering involved in molecule or chemical group in the crystal structure and properties of the design and control as well as the crystal structure prediction. It is an important way to realize from molecular to functional materials. The design and synthesis of novel structure and the potential value of coordination polymers and inorganic - organic hybrid materials are two important aspects of crystal engineering research.
In this paper, we have been prepared nine kinds of single crystals using aromatic carboxylic acid and it's substitute as ligands, Cu(phth)_2(H_2O)_2(l)、Ni (H_2O)_6·(μ-H_2O)_2·K_2(phth)_4(H_2O)(2)、[Cu(H_2O)_6][Na_2(SO_4)_2] (3)、Cu(H_2O )(C_6H_6NSO3)2·2H_2O (4)、Cd(C_7H_5O_4)_2·3H_2O]·2H_2O (5)、[Ni_2(C_7H_5O_4)_4·2H_2O] (6). We also synthesis four kinds of single crystals using imidazole or hexamethylenetetramine as ligands, [Cu(im)_6]Cl_2·4H_2O (7)、[Cu(im)_6]Cl_2·2H_2O (8)、[Cu(H_2O)_6]Cl_2·2{(CH_2)_6N_4}·4H_2O (9)、[Ag2(C_6H_(12)N_4)_2Cr_2O_7·H_2O(10).
Complex 1 crystallized in Monoclinic, space group P2(l)/c, Z =2, a = 8.3895(17)(A), b=14.441(3) (A), c = 7.0992(14) (A),α= 90°,β= 112.14(3)°,γ= 90°; 2 crystallized in Monoclinic, space group P2(l)/c, Z=2, a =10.455(2) ((?)), b = 6.8670(14) ((?)), c =29.704(6) ((?)),α= 90°,β=98.14(3)°,γ=90°. 3 crystallized in Monoclinic, space group P2(l)/c, Z=2, a = 6.2345(12) ((?)), b = 12.333(3) ((?)), c = 9.1822(18) ((?)),α= 90°,β= 105.56(3)°,γ= 90°; 4 crystallized in Monoclinic, space group P2(l)/n,Z=2, a = 7.4485(8) ((?)),b= 17.4102(19)((?)), c = 7.6509(9) ((?)),α= 90°,β= 116.6880(10)°,γ= 90°; 5 crystallized in Monoclinic, space group P2(l)/c, Z=4, a= 7.8338(8) ((?)),b=19.8658(19) ((?)), c= 12.2359(12)((?)),α= 90°,β= 105.8920(10)°,γ= 90°; 6 crystallized in Monoclinic, space group P21/n, Z=2, a = 8.2698(2) ((?)),b=19.4936(8) ((?)), c = 9.9987(4)((?)),α= 90°,β= 102.641(3)°,γ= 90°; 7 crystallized in Triclinic, space group P-1, Z=l, a = 8.8097(18) ((?)), b = 9.0812(18) ((?)), c=10.586(2) ((?)),α= 75.08(3)°,β=83.14(3)°, y =61.84(3)°;8 crystallized in Monoclinic, space group P 21/n, Z=2, a =8.073(2) ((?)), b =13.239(2) ((?)), c =15.0810(10) (A),α= 90°,β= 97.940(10)°，γ= 90°; 9 crystallized in Triclinic, space group P-1,Z=1, a =9.321(3) ((?)),b = 9.3923(16) ((?)), c =9.4261(16) ((?)),α= 119.523(2)°,β= 94.153(3)°,γ= 101.065(3)°; 10 crystallized in Monoclinic, space group P 21/n, Z=4, a =11.1095(16) ((?)),b = 10.9848(14) ((?)), c = 14.101(2) ((?)),α=90°,β= 100.131(2)°,γ=90°. All crystals were characterized by X-ray diffraction, elemental analysis, IR, TG X-ray diffraction analysis revealed that synthesis methods, pH value, solvent, temperature, reaction time, hydrogen bonding can significantly affect the environment and accumulation way of coordination compounds.
In recent years, seeking a highly efficient, low-cost method of refractory organic wastewater treatment are one of the hot environment for scientific research. This article also studied the iron (Ⅲ) - oxalic acid complexes degradation of methylthionine, discussed the different concentrations of hydrogen peroxide, the pH value of the solution degradation rate of methylthionine, the degradation of decolorization reaction dynamics is one order reaction. The result showing that transition metal complexes can be more effectively ferrioxalate refractory organic wastewater treatment comparing with advanced oxidation and traditional methods, with a rapid response, simple operation and so on.
本文以芳香羧酸及其取代物为配体，与过渡金属盐反应合成了6个配合物Cu(phth)_2(H_2O)_2(1)、Ni(H_2O)_6·(μ-H_2O)_2·K_2(phth)_4(H_2O)(2)、[Cu(H_2O)_6][Na_2(SO_4)_2]，(3)、Cu(H_2O)(C_6H_6NSO_3)2·2H_2O(4)、Cd(C_7H_5O_4)2·3H_2O]·2H_2O(5)、[Ni_2(C_7H_5O_4)_4·2H_2O](6)。以咪唑或六次甲基四胺为配体合成了四个配合物，[Cu(im)_6]Cl_2·4H_2O(7)、[Cu(im)_6]Cl_2·2H_2O(8)、[Cu(H_2O)_6]Cl_2·2{(CH_2)_6N_4)·4H_2O(9)、[Ag_2(C_6H_(12)N_4)_2Cr_2O_7·H_2O(10)。
配合物1晶体属单斜晶系，空间群为P2(1)／c,Z=2，a=8．3895(17)(?)，b=14．441(3)(?)，c=7．0992(14)(?)，α=90°，p=112．14(3)°，γ=90°。配合物2晶体属单斜晶系，空间群为P2(1)／c，Z=2，a=10．455(2)(?)，b=6．8670(14)(?)，c=29．704(6)(?)，α=90°，β=98．14(3)°，γ=90°。配合物3品体属单斜品系，空间群为P2(1)／c，Z=2，a=6．2345(12)(?)，b=12．333(3)(?)，c=9．1822(18)(?)，a=90°，β=105．56(3)°，γ=90°。配合物4晶体属单斜品系，空间群为P2(1)／n，Z=2，a=7．4485(8)(?)，b=17．4102(19)(?)，c=7．6509(9)(?)，α=90°，β=116．6880(10)°，γ=90°。配合物5晶体属单斜品系，空间群为P2(1)／c，Z=4，a=7．8338(8)(?)，b=19．8658(19)(?)，c=12．2359(12)(?)，α=90°，β=105．8920(10)°，γ=90°。配合物6晶体属单斜晶系，空间群为P21／n，Z=2，a=8．2698(2)(?)，b=19．4936(8)(?)，c=9．9987(4)(?)，α=90°，β=102．641(3)°，γ=90°。配合物7晶体属三斜晶系，空间群为P-1，Z=1，a=8．8097(18)(?)，b=9．0812(18)(?)，c=10．586(2)(?)，α=75．08(3)°，β=83．14(3)°，γ=61．84(3)°。配合物8晶体属单斜晶系，空问群为P21／n，Z=2，a=8．073(2)(?)，b=13．239(2)(?)，c=15．0810(10)(?)，α=90°，β=97．940(10)°，γ=90°。配合物9晶体属三斜晶系，空间群为P-1，Z=1，a=9．321(3)(?)，b=9．3923(16)(?)，c=9．4261(16)(?)，α=119．523(2)°，β=94．153(3)°，γ=101．065(3)°。配合物10晶体属单斜晶系，空间群为P21／n，Z=4，a=11．1095(16)(?)，b=10．9848(14)(?)，c=14．101(2)(?)，α=90°，β=100．131(2)°，γ=90°。用X射线衍射法对配合物品体结构进行了测定，解析了单晶结构，用元素分析、红外光谱、差热一热重分析等方法对上述配合物进行了结构表征。单晶结构分析发现，合成的方法、pH值、溶剂、温度、反应时间、氢键能显著影响配合物配位环境和晶体堆积。
近年来，随着环境污染的同益严重，环境问题越来越受到人们的重视，寻求一种广谱、高效、低廉的方法对难降解有机废水的处理是近年环境科学研究的热点之一。本文以合成的二元羧酸的配合物草酸铁为例，讨论了它对次甲基蓝的光降解，研究了不同双氧水浓度、溶液pH值等对次甲基蓝降解速率的影响，脱色降解反应均符合一级动力学反应，表明过渡金属的配合物草酸铁可有效处理难降解有机废水，与传统高级氧化方法相比，具有反应快速、操作简单等优点。
As new type of molecular functional materials, coordination compounds are not only a wealth of topology and the accumulation variety of ways, but also have tremendous potential such as in gas in storage, separation, catalytic properties, thermal stability, optical properties, mechanical properties, magnetic properties and so on. Crystal engineering involved in molecule or chemical group in the crystal structure and properties of the design and control as well as the crystal structure prediction. It is an important way to realize from molecular to functional materials. The design and synthesis of novel structure and the potential value of coordination polymers and inorganic - organic hybrid materials are two important aspects of crystal engineering research.
In this paper, we have been prepared nine kinds of single crystals using aromatic carboxylic acid and it's substitute as ligands, Cu(phth)_2(H_2O)_2(l)、Ni (H_2O)_6·(μ-H_2O)_2·K_2(phth)_4(H_2O)(2)、[Cu(H_2O)_6][Na_2(SO_4)_2] (3)、Cu(H_2O )(C_6H_6NSO3)2·2H_2O (4)、Cd(C_7H_5O_4)_2·3H_2O]·2H_2O (5)、[Ni_2(C_7H_5O_4)_4·2H_2O] (6). We also synthesis four kinds of single crystals using imidazole or hexamethylenetetramine as ligands, [Cu(im)_6]Cl_2·4H_2O (7)、[Cu(im)_6]Cl_2·2H_2O (8)、[Cu(H_2O)_6]Cl_2·2{(CH_2)_6N_4}·4H_2O (9)、[Ag2(C_6H_(12)N_4)_2Cr_2O_7·H_2O(10).
Complex 1 crystallized in Monoclinic, space group P2(l)/c, Z =2, a = 8.3895(17)(A), b=14.441(3) (A), c = 7.0992(14) (A),α= 90°,β= 112.14(3)°,γ= 90°; 2 crystallized in Monoclinic, space group P2(l)/c, Z=2, a =10.455(2) ((?)), b = 6.8670(14) ((?)), c =29.704(6) ((?)),α= 90°,β=98.14(3)°,γ=90°. 3 crystallized in Monoclinic, space group P2(l)/c, Z=2, a = 6.2345(12) ((?)), b = 12.333(3) ((?)), c = 9.1822(18) ((?)),α= 90°,β= 105.56(3)°,γ= 90°; 4 crystallized in Monoclinic, space group P2(l)/n,Z=2, a = 7.4485(8) ((?)),b= 17.4102(19)((?)), c = 7.6509(9) ((?)),α= 90°,β= 116.6880(10)°,γ= 90°; 5 crystallized in Monoclinic, space group P2(l)/c, Z=4, a= 7.8338(8) ((?)),b=19.8658(19) ((?)), c= 12.2359(12)((?)),α= 90°,β= 105.8920(10)°,γ= 90°; 6 crystallized in Monoclinic, space group P21/n, Z=2, a = 8.2698(2) ((?)),b=19.4936(8) ((?)), c = 9.9987(4)((?)),α= 90°,β= 102.641(3)°,γ= 90°; 7 crystallized in Triclinic, space group P-1, Z=l, a = 8.8097(18) ((?)), b = 9.0812(18) ((?)), c=10.586(2) ((?)),α= 75.08(3)°,β=83.14(3)°, y =61.84(3)°;8 crystallized in Monoclinic, space group P 21/n, Z=2, a =8.073(2) ((?)), b =13.239(2) ((?)), c =15.0810(10) (A),α= 90°,β= 97.940(10)°，γ= 90°; 9 crystallized in Triclinic, space group P-1,Z=1, a =9.321(3) ((?)),b = 9.3923(16) ((?)), c =9.4261(16) ((?)),α= 119.523(2)°,β= 94.153(3)°,γ= 101.065(3)°; 10 crystallized in Monoclinic, space group P 21/n, Z=4, a =11.1095(16) ((?)),b = 10.9848(14) ((?)), c = 14.101(2) ((?)),α=90°,β= 100.131(2)°,γ=90°. All crystals were characterized by X-ray diffraction, elemental analysis, IR, TG X-ray diffraction analysis revealed that synthesis methods, pH value, solvent, temperature, reaction time, hydrogen bonding can significantly affect the environment and accumulation way of coordination compounds.
In recent years, seeking a highly efficient, low-cost method of refractory organic wastewater treatment are one of the hot environment for scientific research. This article also studied the iron (Ⅲ) - oxalic acid complexes degradation of methylthionine, discussed the different concentrations of hydrogen peroxide, the pH value of the solution degradation rate of methylthionine, the degradation of decolorization reaction dynamics is one order reaction. The result showing that transition metal complexes can be more effectively ferrioxalate refractory organic wastewater treatment comparing with advanced oxidation and traditional methods, with a rapid response, simple operation and so on.
引文
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