以金属配合物为模板的无机开放骨架化合物的合成与表征
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摘要
以分子筛为代表的无机开放骨架化合物由于具有规则的孔道结构和独特的性能，在催化、吸附、分离和离子交换等领域具有重要应用。除此之外，在电学、磁学、化学传感以及医学方面也有着潜在的应用前景。因此，开发新型的无机开放骨架化合物一直是多孔材料领域的研究热点之一。在合成新型无机开放骨架化合物的过程中引入结构导向剂是必要的。传统的结构导向剂包括碱金属离子、碱土金属离子、有机胺类、季铵盐(碱)、金属配合物、氟离子等。其中金属配合物作为结构导向剂，由于具有刚性、特殊的空间构象(如手性)、大量的氢键位点等特点，成为合成化学中研究的热点。
本论文以钴(镍)胺配合物为结构导向剂，利用水热/溶剂热的合成方法开展了锗酸镓分子筛、金属氟化物复合物及磷酸盐等开放骨架化合物的合成研究，取得的主要成果如下：
1.利用外消旋的乙二胺合镍配合物为模板剂，在溶剂热条件下成功地合成出具有新型分子筛结构的锗酸镓[Ni(en)_3][[Ga_2Ge_4O_(12)](GaGeO-CJ63)。GaGeO-CJ63是由TO_4(T=Ge,Ga)四面体之间通过共享顶点形成三维四连接的骨架。其结构完全由三元环构成，沿三个方向上存在交叉的10-元环孔道。在目前已知分子筛结构中，GaGeO-CJ63的骨架密度是第三低的。在该化合物中存在着两种笼：一种为非手性笼、一种为手性笼。手性笼是由外消旋的Ni(en)_32+导向生成的。GaGeO-CJ63锗酸镓被国际分子筛协会命名为JST。
2.在溶剂热条件下成功地原位合成出以1,2-丙二胺合镍配合物为模板剂，具有新型分子筛结构的锗酸镓GaGeO-CJ64。其结构是由单六元环和双六元环通过spiro-5结构单元连接构成三维四连接骨架。GaGeO-CJ64是第一例具有11-元环交叉孔道的分子筛结构。该化合物具有较低的骨架密度，其无机骨架结构中含有一个新颖的空旷的笼[3~(12)·4~3·6~2·11~6]。
3.成功地合成出两种金属配合物与氟化锆的复合物[Co(en)_3]_2(Zr_2F_(12))(ZrF_6H_2O)·H_2O和[Co(en)_3](Zr_2F_(11)H_2O)，并对其结构及光电性质进行了表征。实验结果表明，这两种复合物均在紫外区显现出光电效应，响应信号位置与其紫外-可见吸收光谱中的钴胺配合物阳离子的一个吸收峰位置相一致。这种特殊的光电现象归因于钴胺配合物阳离子与氟化锆阴离子簇之间发生的协同作用。
4.在水热条件下，以六氨合钴配合物阳离子为模板剂，合成出一个新颖的双层状磷酸锌[Co(NH_3)_6]3[Zn8(HPO_4)8(PO_4)2](PO_4)(ZnPO-CJ68)。该化合物沿三个方向上具有交叉的八元环孔穴，客体Co(NH_3)_63+阳离子不仅存在于层间而且也存在于层内，且Co(NH_3)_6~(3+)阳离子的构型与层内的8~6孔穴的构型完美匹配，起到了真正模板的作用。
5.在溶剂热条件下，采用[d,l-Co(en)_3]~(3+)配合物阳离子作为模板剂，合成出一维链状磷酸锌[Co(en)_3][Zn_2(H_2PO_4)(HPO_4)_2Cl_2]，它是由无限的阴离子链[Zn_2(H_2PO_4)(HPO_4)_2Cl_2]_n~(3-)构成。该化合物含有由HPO_4和ZnO_3Cl构成的四元环，据我们所知，以磷氧四面体连接两个相邻四元环构成的链的连接方式在磷酸锌中是少见的。同时，以二乙烯三胺合钴配合物阳离子为模板剂，成功地合成出二维层状磷酸铝Co(dien)_2Al_3(PO_4)_4(AlPO-CJ54)。该化合物的铝氧四面体和磷氧四面体严格排列交替连接形成Z字形链，链与链之间连接起来构成阴离子Al_3(PO_4)_4~(3-)的二维层，该层含有四元环和八元环，无序的模板剂存在于层间。
6.在溶剂热条件下，以二乙烯三胺合镍配合物为模板剂，成功地合成出具有CHA分子筛结构类型的过渡金属掺杂磷酸铝微孔化合物MAPO-CHA(M=Zn,Mg)。其无机骨架结构是由铝(锌、镁)氧四面体和磷氧四面体严格交替排列连接成三维结构，其沿三个方向具有三维8-元环交叉孔道。二乙烯三胺合镍配合物阳离子位于cha笼中，起到平衡骨架负电荷和填充的作用。
Inorganic open-framework materials such as molecular sieves have beenextensively used in many industrial processes such as catalysis, adsorption andseparation, as well as in new applications of electronic, magnetism, chemical sensors,medicine, etc. Therefore, the preparation of new inorganic open-framework materialsis one of the most important fields for the material science. To synthesize newinorganic open-framework materials, the introduction of a structure-directing agent(SDA) is necessary. Conventional SDAs include alkali metal cations, alkaline earthcations, protonated organic amines, quaternary ammonium cations, metal complexescations and fluorine ions. Compared with conventional SDAs, metal complexescations can offer a particular spatial configuration, the wide range of oxidation states,more H-bonds, chiral symmetry and have an unexpected properties with the hostframework through the cooperative behavior, it is a focus at all times in thepreparation of inorganic materials.
This thesis is focused on the synthesis of a series of open-framework compoundsunder the hydro/solvothermal conditions templated by metal complexes cations. Mainachievements are as follows:
1. A novel three-dimensional gallogermanate zeolite [Ni(en)_3][Ga_2Ge_4O_(12)](GaGeO-CJ63) has been successfully synthesized under solvothermal condition.GaGeO-CJ63is a strictly4-connected zeolitic structure constructed exclusively bythree-ring building units, and its FD(framework density) is the third lowest among allknown zeolite frameworks. It contains10-ring channels along the three directions.GaGeO-CJ63was synthesized by using racemic [Ni(en)_3]~(2+) cations asstructure-directing agent, and chirality transfer could be clearly observed from chiraltemplates to chiral cages in its framework. GaGeO-CJ63is denoted as JST by theInternational Zeolite Association.
2. A novel three-dimensional gallogermanate zeolite GaGeO-CJ64has beensuccessfully synthesized in the presence of chiral metal complexes in situ synthesismethod. Its inorganic structure is constructed by s6r(single6-ring), d6r(double6-ring), spiro-5building units. To the best of our knowledge, it is the first zeolite that contains11-ring intersecting channels along three directions. GaGeO-CJ64contains a novelvoid cage [3~(12)·4~3·6~2·11~6].
3.[Co(en)_3]_2(Zr_2F_(12))(ZrF_6H_2O)·H_2O and [Co(en)_3](Zr_2F_(11)H_2O), two compoundshave been successfully synthesized using different methods. Both compounds existextensive hydrogen bonds. Interestingly, they exhibit unusual photoelectronic effectsin the near-UV region. The fact that the signal of surface photovoltage of eachcompound is coincident with one of the UV/Vis absorption transitions of the cobaltamine complexes. This suggests that cooperative behavior between cobalt aminecomplexes and metal fluoride ions through interactions might be responsible for theseunexpected photoelectric phenomena.
4. A new zinc phosphate structure [Co(NH_3)6]_3[Zn_8(HPO_4)_8(PO_4)_2](PO_4)(ZnPO-CJ68) with unusual double-sheet layers, has been successfully synthesized,which used cobalt hexaammine as the SDA. The structure of ZnPO-CJ68containsunusual layered host frameworks with interconnecting8-ring apertures along thethickness of the layers as well as in the planes of the layers. As the structural template,the guest cobalt hexaammine complex perfectly fits the shape of the intralayermicropore.
5. A1D(one dimensional) infinite chain structure[Co(en)_3][Zn_2(H_2PO_4)(HPO_4)_2Cl_2] has been synthesized under hydrothermalcondition templated by [d,l-Co(en)_3]~(3+)cations. It is constructed by a macro anionic[Zn_2(H_2PO_4)(HPO_4)_2Cl_2]_n~(3-)chain involving Zn-centered tetrahedra and P-centeredtetrahedral(ZnO_3Cl, H_2PO_4, HPO_4). It is rare that [Co(en)_3][Zn_2(H_2PO_4)(HPO_4)_2Cl_2]contains4-ring which consists of ZnO3Cl and HPO_4. Each4-ring is connected to forman infinite chain through PO_4tetrahedra. In addition, using cobalt amines cations astemplate, a2D layered Co(dien)2Al_3(PO_4)_4(AlPO-CJ54) has been prepared. Itsinorganic layer is constructed from strict alternation of AlO_4and PO_4tetrahetra toform zigzag ladder-type chains. The connectivity between the chains leads to anionic[Al_3P_4O_(16)]~(3-)layers. These layers only have four-and eight-membered rings. Thedisordered cobalt ammine complexes are located between layers.
6. Two transition metal containing aluminophosphates MAPO-CHA(M=Zn,Mg)with CHA zeotype have been synthesized under the solvothermal conditions. Thelinkages of AlO_4(MO_4) tetrahedra and PO_4tetrahedra through vertex oxygen atoms form the inorganic framework [M_2Al_4(PO_4)_6]~(2-). It contains8-ring channels along thethree directions. Nickel amine complexes are located in the cha cage to neutralize thenegative charge of the host.
本论文以钴(镍)胺配合物为结构导向剂，利用水热/溶剂热的合成方法开展了锗酸镓分子筛、金属氟化物复合物及磷酸盐等开放骨架化合物的合成研究，取得的主要成果如下：
1.利用外消旋的乙二胺合镍配合物为模板剂，在溶剂热条件下成功地合成出具有新型分子筛结构的锗酸镓[Ni(en)_3][[Ga_2Ge_4O_(12)](GaGeO-CJ63)。GaGeO-CJ63是由TO_4(T=Ge,Ga)四面体之间通过共享顶点形成三维四连接的骨架。其结构完全由三元环构成，沿三个方向上存在交叉的10-元环孔道。在目前已知分子筛结构中，GaGeO-CJ63的骨架密度是第三低的。在该化合物中存在着两种笼：一种为非手性笼、一种为手性笼。手性笼是由外消旋的Ni(en)_32+导向生成的。GaGeO-CJ63锗酸镓被国际分子筛协会命名为JST。
2.在溶剂热条件下成功地原位合成出以1,2-丙二胺合镍配合物为模板剂，具有新型分子筛结构的锗酸镓GaGeO-CJ64。其结构是由单六元环和双六元环通过spiro-5结构单元连接构成三维四连接骨架。GaGeO-CJ64是第一例具有11-元环交叉孔道的分子筛结构。该化合物具有较低的骨架密度，其无机骨架结构中含有一个新颖的空旷的笼[3~(12)·4~3·6~2·11~6]。
3.成功地合成出两种金属配合物与氟化锆的复合物[Co(en)_3]_2(Zr_2F_(12))(ZrF_6H_2O)·H_2O和[Co(en)_3](Zr_2F_(11)H_2O)，并对其结构及光电性质进行了表征。实验结果表明，这两种复合物均在紫外区显现出光电效应，响应信号位置与其紫外-可见吸收光谱中的钴胺配合物阳离子的一个吸收峰位置相一致。这种特殊的光电现象归因于钴胺配合物阳离子与氟化锆阴离子簇之间发生的协同作用。
4.在水热条件下，以六氨合钴配合物阳离子为模板剂，合成出一个新颖的双层状磷酸锌[Co(NH_3)_6]3[Zn8(HPO_4)8(PO_4)2](PO_4)(ZnPO-CJ68)。该化合物沿三个方向上具有交叉的八元环孔穴，客体Co(NH_3)_63+阳离子不仅存在于层间而且也存在于层内，且Co(NH_3)_6~(3+)阳离子的构型与层内的8~6孔穴的构型完美匹配，起到了真正模板的作用。
5.在溶剂热条件下，采用[d,l-Co(en)_3]~(3+)配合物阳离子作为模板剂，合成出一维链状磷酸锌[Co(en)_3][Zn_2(H_2PO_4)(HPO_4)_2Cl_2]，它是由无限的阴离子链[Zn_2(H_2PO_4)(HPO_4)_2Cl_2]_n~(3-)构成。该化合物含有由HPO_4和ZnO_3Cl构成的四元环，据我们所知，以磷氧四面体连接两个相邻四元环构成的链的连接方式在磷酸锌中是少见的。同时，以二乙烯三胺合钴配合物阳离子为模板剂，成功地合成出二维层状磷酸铝Co(dien)_2Al_3(PO_4)_4(AlPO-CJ54)。该化合物的铝氧四面体和磷氧四面体严格排列交替连接形成Z字形链，链与链之间连接起来构成阴离子Al_3(PO_4)_4~(3-)的二维层，该层含有四元环和八元环，无序的模板剂存在于层间。
6.在溶剂热条件下，以二乙烯三胺合镍配合物为模板剂，成功地合成出具有CHA分子筛结构类型的过渡金属掺杂磷酸铝微孔化合物MAPO-CHA(M=Zn,Mg)。其无机骨架结构是由铝(锌、镁)氧四面体和磷氧四面体严格交替排列连接成三维结构，其沿三个方向具有三维8-元环交叉孔道。二乙烯三胺合镍配合物阳离子位于cha笼中，起到平衡骨架负电荷和填充的作用。
Inorganic open-framework materials such as molecular sieves have beenextensively used in many industrial processes such as catalysis, adsorption andseparation, as well as in new applications of electronic, magnetism, chemical sensors,medicine, etc. Therefore, the preparation of new inorganic open-framework materialsis one of the most important fields for the material science. To synthesize newinorganic open-framework materials, the introduction of a structure-directing agent(SDA) is necessary. Conventional SDAs include alkali metal cations, alkaline earthcations, protonated organic amines, quaternary ammonium cations, metal complexescations and fluorine ions. Compared with conventional SDAs, metal complexescations can offer a particular spatial configuration, the wide range of oxidation states,more H-bonds, chiral symmetry and have an unexpected properties with the hostframework through the cooperative behavior, it is a focus at all times in thepreparation of inorganic materials.
This thesis is focused on the synthesis of a series of open-framework compoundsunder the hydro/solvothermal conditions templated by metal complexes cations. Mainachievements are as follows:
1. A novel three-dimensional gallogermanate zeolite [Ni(en)_3][Ga_2Ge_4O_(12)](GaGeO-CJ63) has been successfully synthesized under solvothermal condition.GaGeO-CJ63is a strictly4-connected zeolitic structure constructed exclusively bythree-ring building units, and its FD(framework density) is the third lowest among allknown zeolite frameworks. It contains10-ring channels along the three directions.GaGeO-CJ63was synthesized by using racemic [Ni(en)_3]~(2+) cations asstructure-directing agent, and chirality transfer could be clearly observed from chiraltemplates to chiral cages in its framework. GaGeO-CJ63is denoted as JST by theInternational Zeolite Association.
2. A novel three-dimensional gallogermanate zeolite GaGeO-CJ64has beensuccessfully synthesized in the presence of chiral metal complexes in situ synthesismethod. Its inorganic structure is constructed by s6r(single6-ring), d6r(double6-ring), spiro-5building units. To the best of our knowledge, it is the first zeolite that contains11-ring intersecting channels along three directions. GaGeO-CJ64contains a novelvoid cage [3~(12)·4~3·6~2·11~6].
3.[Co(en)_3]_2(Zr_2F_(12))(ZrF_6H_2O)·H_2O and [Co(en)_3](Zr_2F_(11)H_2O), two compoundshave been successfully synthesized using different methods. Both compounds existextensive hydrogen bonds. Interestingly, they exhibit unusual photoelectronic effectsin the near-UV region. The fact that the signal of surface photovoltage of eachcompound is coincident with one of the UV/Vis absorption transitions of the cobaltamine complexes. This suggests that cooperative behavior between cobalt aminecomplexes and metal fluoride ions through interactions might be responsible for theseunexpected photoelectric phenomena.
4. A new zinc phosphate structure [Co(NH_3)6]_3[Zn_8(HPO_4)_8(PO_4)_2](PO_4)(ZnPO-CJ68) with unusual double-sheet layers, has been successfully synthesized,which used cobalt hexaammine as the SDA. The structure of ZnPO-CJ68containsunusual layered host frameworks with interconnecting8-ring apertures along thethickness of the layers as well as in the planes of the layers. As the structural template,the guest cobalt hexaammine complex perfectly fits the shape of the intralayermicropore.
5. A1D(one dimensional) infinite chain structure[Co(en)_3][Zn_2(H_2PO_4)(HPO_4)_2Cl_2] has been synthesized under hydrothermalcondition templated by [d,l-Co(en)_3]~(3+)cations. It is constructed by a macro anionic[Zn_2(H_2PO_4)(HPO_4)_2Cl_2]_n~(3-)chain involving Zn-centered tetrahedra and P-centeredtetrahedral(ZnO_3Cl, H_2PO_4, HPO_4). It is rare that [Co(en)_3][Zn_2(H_2PO_4)(HPO_4)_2Cl_2]contains4-ring which consists of ZnO3Cl and HPO_4. Each4-ring is connected to forman infinite chain through PO_4tetrahedra. In addition, using cobalt amines cations astemplate, a2D layered Co(dien)2Al_3(PO_4)_4(AlPO-CJ54) has been prepared. Itsinorganic layer is constructed from strict alternation of AlO_4and PO_4tetrahetra toform zigzag ladder-type chains. The connectivity between the chains leads to anionic[Al_3P_4O_(16)]~(3-)layers. These layers only have four-and eight-membered rings. Thedisordered cobalt ammine complexes are located between layers.
6. Two transition metal containing aluminophosphates MAPO-CHA(M=Zn,Mg)with CHA zeotype have been synthesized under the solvothermal conditions. Thelinkages of AlO_4(MO_4) tetrahedra and PO_4tetrahedra through vertex oxygen atoms form the inorganic framework [M_2Al_4(PO_4)_6]~(2-). It contains8-ring channels along thethree directions. Nickel amine complexes are located in the cha cage to neutralize thenegative charge of the host.
引文
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