基于刚性配体和模板效应构筑的MOF孔道材料
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摘要
多孔性金属-有机框架化合物(Metal-organic frameworks MOF)在气体吸附和存储、离子交换、分子识别、催化、化合物选择性分离和手性分离以及光、电、磁等领域有巨大的潜在应用，已经发展成为一种新型的多功能材料，引起了人们的极大兴趣。MOF与传统分子筛材料相比不仅由于具有不同于分子筛的孔道特征、迷人的拓扑结构，而且还具有更加优良吸附和存储特性。MOF可以按照晶体工程的原理，通过选择特定几何构型的刚性有机配体和有机溶剂模板，在一定程度上实现多孔性MOF的定向设计和合成。
本论文选用不同构型的刚性的有机羧酸和含氮配体和金属离子并结合不同尺度的有机溶剂和离子(作为溶剂和离子模板)来合成金属-有机框架孔道材料。我们考察其对所构筑的化合物网络结构的影响的同时，也考察这类化合物作为多功能材料在离子交换、气体吸附及荧光等方面的潜在应用。
通过水热和溶剂热技术，我们合成了二十三个化合物，通过元素分析、IR、XRPD、TG、1H NMR和单晶X-射线衍射对晶体结构进行了表征，对部分化合物的氮气吸附性质、主客体性质、液相离子交换性质和荧光性质进行了初步研究讨论。这些研究结果主要包括以下四个方面：
1、合成了一系列不同尺度的酰胺类溶剂DMF、DMA、DEE、DEP、DPE、DPP作为模板，利用BTC羧酸为配体，与过渡金属在水热条件下反应，成功得到了十二个孔径不同的三维MOF孔道材料。Zn_2(BTC)(NO_3)(DMA)_3(1)[Zn_(11)(BTC)6(NO_3)_4·9DEE](2)[Zn_11(BTC)_6(NO_3)_4·8DEP](3)[Zn(BTC)][(CH_3)_2NH_2]·DMA (4)[Zn_3(BTC)_3][(CH_3)_2NH_2]_3·3DMA (5)[Zn_9(BTC)_6(OH)_2][(CH_3)2NH_2]_2·3DMA (6)[Zn_9(BTC)_5(OH)_3(C_2O_4)][(CH_3)_2NH_2]_2·6DEE (7)[Cd(BTC)][(CH_3)_2NH_2]·DMA (8)Cd_2(BTC)(NO_3)(DMA)_3(9)Cd_2(BTC)(NO_3)(DEE)_3(10)Co_2(BTC)(NO_3)(DMA)_3(11)Co_2(BTC)(NO_3)(DEE)_3(12)
我们发现溶剂模板的尺度越大，得到的孔的尺度也越大，孔道的拓扑结构也会更新颖。从而探索了一种合成新颖的MOF孔材料和调控MOF孔道尺寸的方法。首次实现了系统利用溶剂模板的尺度来调控孔道的尺度和结构。首次利用situ-1HNMR对MOF孔材料的溶剂交换和离子交换行为进行了表征。
2、以有机胺阳离子为模板，利用不同的刚性羧酸配体成功得到三个孔径不同的三维阴离子型MOF。[(CH_3)_2NH_2][Cd(BPDC)_(1.5)]·2DMA (13)[(CH_3)_2NH_2][Cd(BPDC)_(1.5)]·2DMA (14)[Me_2NH_2]2[Cd_2(NH_2BDC)_3]·4DMA (15)
发现这些阴离子框架基本上都是低对称的。对这些阴离子型框架的离子交换行为我们利用1H NMR进行了跟踪。
3、合成和利用刚性桥联含N配体如3-BPH，4-BPH与刚性的羧酸配体一起和过渡金属作用，合成得到4个不同结构的混合配体柱支撑型的MOF。Co_2(BPDC)_2(4-BPH)·4DMF (16)Cd(BPDC)(4-BPH)·2DMF (17)Co_4(BTC)(C_2H_2N2O_2)0.5(4-BPH)0.5(DMF)_2·H_2O (18)Ni_2(BDC)_2(3-BPH)_2(H_2O)·4DMF (19)
研究结构表明这类MOF具有灵活多变的配位方式，通过其空间构型的可调整性以及氮原子的配位作用，可以合成得到柱支撑型结构新颖的MOF孔材料。
4、合成和利用刚性多齿含N配体TPB、IP与刚性的羧酸配体一起和过渡金属作用，合成得到4个不同结构的混合配体的MOF。[Cu (TPB)][SO_4] H_2O (20)Zn(TPB)(BDC)·2H_2O (21)Co_2(BPTC)(IP)_4·12H_2O (22)Ni(BPTC)(IP)_2·6H_2O (23)
研究结构表明这类含N配体TPB、IP并不容易形成三维多孔的框架。意外地，我们得到了一个稳定的超分子框架，孔道尺度为1.2nm。
Porous Metal-organic frameworks (MOF) as novel multifunctional materials, haveattracted more and more attention because of their flexible structures, various topologies,potential applications in gas storage, ion-exchange, adsorption, molecular recognization,catalysts, selective separation and chiral separation along with optics, electrics, magnetismand enantiomeric separation. These open frameworks possess not only crystalline porousstructure, but also better performance in gas sorption and storage comparing with traditionalzeolites. In addition, according to the principle of crystal engineering, it is possible thatrational design and synthesis of porous MOFs by selecting special organic ligands, metalsand templates.
In this dissertation, we synthesize N-donor and carboxylate ligands, and use solventwith different size as templates to construct porous MOFs. We also investigate fluorescentproperty of the compound as multi-functional material with potential applications.Under hydrothermal and solvothermal conditions, we have synthesized23porousMOF. These compounds have been structurally characterized by the elemental analysis, IR,XRPD, TG,1H NMR and single-crystal X-ray diffraction. Moreover, the ions-exchange, N2absorption and fluorescence properties of some MOFs have been studied and discussed.These results include the following four issues:
1. We synthesize a series of solvents with different size and then choose1,3,5-benzenetricarboxylate (BTC) coupled with metal ions to evaluating influence ofsolvents with different size. We successfully obtain twelve different3D porous MOFs:Zn_2(BTC)(NO_3)(DMA)_3(1)[Zn_(11)(BTC)_6(NO_3)_4·9DEE](2)[Zn_(11)(BTC)_6(NO_3)_4·8DEP](3)[Zn(BTC)][(CH_3)_2NH_2]·DMA (4)[Zn_3(BTC)_3][(CH_3)_2NH2]3·3DMA (5)[Zn_9(BTC)_6(OH)_2][(CH_3)_2NH_2]_2·3DMA (6)[Zn_9(BTC)_5(OH)_3(C_2O_4)][(CH_3)_2NH_2]_2·6DEE (7)[Cd(BTC)][(CH_3)_2NH_2]·DMA (8)Cd_2(BTC)(NO_3)·(DMA)_3(9)Cd_2(BTC)(NO_3)·(DEE)_3(10)Co_2(BTC)(NO_3)·(DMA)_3(11)Co_2(BTC)(NO_3)·(DEE)_3(12)
Using solvents with different size as space-templating method, a cheap and easysynthesis approach have been successfully applied to synthesize MOFs. Not only does thisapproach can systematically control the pore size, but it also allows access to new structuresand topologies previously unrealized in MOFs. In general, that is ‘the larger the solventssize, the larger the pores’. The ion exchange behavior, gas absorbtion and the fluorescentproperty were studied and discussed.
2. By choosing organic amine cations as a template and different rigid carboxylateligands, we successfully obtain three different3D MOFs with anionic frameworks.[(CH_3)_2NH_2][Cd(BPDC)_(1.5)]·2DMA (13)[(CH_3)_2NH_2][Cd(BPDC))_(1.5)]·2DMA (14)[Me_2NH_2]_2[Cd_2(NH_2BDC)_3]·4DMA (15)
We found that these anionic frameworks are basically low-symmetric, which aredifferent with the neutral framework and easier to form chiral structures. The ion exchangebehavior, gas absorbtion and the fluorescent property are studied and discussed.
3. By using rigid N-donor ligands such as3-BPH,4-BPH and so on, together with rigidcarboxylic acid ligands and transition metal ions, we synthesized four mixed ligand basedMOFs with different structures.Co_2(BPDC)_2(4-BPH)·4DMF (16)Cd(BPDC)(4-BPH)·2DMF (17)Co4(BTC)(C_2H_2N_2O_2)0.5(4-BPH)0.5(DMF)2·H_2O (18)Ni_2(BDC)_2(3-BPH)_2(H_2O)·4DMF (19)
It shows that these MOFs possess flexible coordination modes. Through its adjustablespatial configuration and role of the coordination of nitrogen atoms, novel pillared MOFshave been synthesized. The gas absorbtion property are also studied and discussed
4. Using multi N-containing ligands such as TPB, IP and so on, together with rigidcarboxylic acid ligands and transition metal ions, we synthesized four mixed ligand basedMOFs with different structures.[Cu (TPB)][SO_4] H_2O (20)Zn(TPB)(BDC)·2H_2O (21)Co_2(BPTC)(IP)_4·12H_2O (22)Ni(BPTC)(IP)_2·6H_2O (23)
Study shows that the ligands TPB, IP are not easy to form three-dimensional porousframeworks. Unexpectedly, we get a stable supramolecular framework, where the pore size is1.2nm.
本论文选用不同构型的刚性的有机羧酸和含氮配体和金属离子并结合不同尺度的有机溶剂和离子(作为溶剂和离子模板)来合成金属-有机框架孔道材料。我们考察其对所构筑的化合物网络结构的影响的同时，也考察这类化合物作为多功能材料在离子交换、气体吸附及荧光等方面的潜在应用。
通过水热和溶剂热技术，我们合成了二十三个化合物，通过元素分析、IR、XRPD、TG、1H NMR和单晶X-射线衍射对晶体结构进行了表征，对部分化合物的氮气吸附性质、主客体性质、液相离子交换性质和荧光性质进行了初步研究讨论。这些研究结果主要包括以下四个方面：
1、合成了一系列不同尺度的酰胺类溶剂DMF、DMA、DEE、DEP、DPE、DPP作为模板，利用BTC羧酸为配体，与过渡金属在水热条件下反应，成功得到了十二个孔径不同的三维MOF孔道材料。Zn_2(BTC)(NO_3)(DMA)_3(1)[Zn_(11)(BTC)6(NO_3)_4·9DEE](2)[Zn_11(BTC)_6(NO_3)_4·8DEP](3)[Zn(BTC)][(CH_3)_2NH_2]·DMA (4)[Zn_3(BTC)_3][(CH_3)_2NH_2]_3·3DMA (5)[Zn_9(BTC)_6(OH)_2][(CH_3)2NH_2]_2·3DMA (6)[Zn_9(BTC)_5(OH)_3(C_2O_4)][(CH_3)_2NH_2]_2·6DEE (7)[Cd(BTC)][(CH_3)_2NH_2]·DMA (8)Cd_2(BTC)(NO_3)(DMA)_3(9)Cd_2(BTC)(NO_3)(DEE)_3(10)Co_2(BTC)(NO_3)(DMA)_3(11)Co_2(BTC)(NO_3)(DEE)_3(12)
我们发现溶剂模板的尺度越大，得到的孔的尺度也越大，孔道的拓扑结构也会更新颖。从而探索了一种合成新颖的MOF孔材料和调控MOF孔道尺寸的方法。首次实现了系统利用溶剂模板的尺度来调控孔道的尺度和结构。首次利用situ-1HNMR对MOF孔材料的溶剂交换和离子交换行为进行了表征。
2、以有机胺阳离子为模板，利用不同的刚性羧酸配体成功得到三个孔径不同的三维阴离子型MOF。[(CH_3)_2NH_2][Cd(BPDC)_(1.5)]·2DMA (13)[(CH_3)_2NH_2][Cd(BPDC)_(1.5)]·2DMA (14)[Me_2NH_2]2[Cd_2(NH_2BDC)_3]·4DMA (15)
发现这些阴离子框架基本上都是低对称的。对这些阴离子型框架的离子交换行为我们利用1H NMR进行了跟踪。
3、合成和利用刚性桥联含N配体如3-BPH，4-BPH与刚性的羧酸配体一起和过渡金属作用，合成得到4个不同结构的混合配体柱支撑型的MOF。Co_2(BPDC)_2(4-BPH)·4DMF (16)Cd(BPDC)(4-BPH)·2DMF (17)Co_4(BTC)(C_2H_2N2O_2)0.5(4-BPH)0.5(DMF)_2·H_2O (18)Ni_2(BDC)_2(3-BPH)_2(H_2O)·4DMF (19)
研究结构表明这类MOF具有灵活多变的配位方式，通过其空间构型的可调整性以及氮原子的配位作用，可以合成得到柱支撑型结构新颖的MOF孔材料。
4、合成和利用刚性多齿含N配体TPB、IP与刚性的羧酸配体一起和过渡金属作用，合成得到4个不同结构的混合配体的MOF。[Cu (TPB)][SO_4] H_2O (20)Zn(TPB)(BDC)·2H_2O (21)Co_2(BPTC)(IP)_4·12H_2O (22)Ni(BPTC)(IP)_2·6H_2O (23)
研究结构表明这类含N配体TPB、IP并不容易形成三维多孔的框架。意外地，我们得到了一个稳定的超分子框架，孔道尺度为1.2nm。
Porous Metal-organic frameworks (MOF) as novel multifunctional materials, haveattracted more and more attention because of their flexible structures, various topologies,potential applications in gas storage, ion-exchange, adsorption, molecular recognization,catalysts, selective separation and chiral separation along with optics, electrics, magnetismand enantiomeric separation. These open frameworks possess not only crystalline porousstructure, but also better performance in gas sorption and storage comparing with traditionalzeolites. In addition, according to the principle of crystal engineering, it is possible thatrational design and synthesis of porous MOFs by selecting special organic ligands, metalsand templates.
In this dissertation, we synthesize N-donor and carboxylate ligands, and use solventwith different size as templates to construct porous MOFs. We also investigate fluorescentproperty of the compound as multi-functional material with potential applications.Under hydrothermal and solvothermal conditions, we have synthesized23porousMOF. These compounds have been structurally characterized by the elemental analysis, IR,XRPD, TG,1H NMR and single-crystal X-ray diffraction. Moreover, the ions-exchange, N2absorption and fluorescence properties of some MOFs have been studied and discussed.These results include the following four issues:
1. We synthesize a series of solvents with different size and then choose1,3,5-benzenetricarboxylate (BTC) coupled with metal ions to evaluating influence ofsolvents with different size. We successfully obtain twelve different3D porous MOFs:Zn_2(BTC)(NO_3)(DMA)_3(1)[Zn_(11)(BTC)_6(NO_3)_4·9DEE](2)[Zn_(11)(BTC)_6(NO_3)_4·8DEP](3)[Zn(BTC)][(CH_3)_2NH_2]·DMA (4)[Zn_3(BTC)_3][(CH_3)_2NH2]3·3DMA (5)[Zn_9(BTC)_6(OH)_2][(CH_3)_2NH_2]_2·3DMA (6)[Zn_9(BTC)_5(OH)_3(C_2O_4)][(CH_3)_2NH_2]_2·6DEE (7)[Cd(BTC)][(CH_3)_2NH_2]·DMA (8)Cd_2(BTC)(NO_3)·(DMA)_3(9)Cd_2(BTC)(NO_3)·(DEE)_3(10)Co_2(BTC)(NO_3)·(DMA)_3(11)Co_2(BTC)(NO_3)·(DEE)_3(12)
Using solvents with different size as space-templating method, a cheap and easysynthesis approach have been successfully applied to synthesize MOFs. Not only does thisapproach can systematically control the pore size, but it also allows access to new structuresand topologies previously unrealized in MOFs. In general, that is ‘the larger the solventssize, the larger the pores’. The ion exchange behavior, gas absorbtion and the fluorescentproperty were studied and discussed.
2. By choosing organic amine cations as a template and different rigid carboxylateligands, we successfully obtain three different3D MOFs with anionic frameworks.[(CH_3)_2NH_2][Cd(BPDC)_(1.5)]·2DMA (13)[(CH_3)_2NH_2][Cd(BPDC))_(1.5)]·2DMA (14)[Me_2NH_2]_2[Cd_2(NH_2BDC)_3]·4DMA (15)
We found that these anionic frameworks are basically low-symmetric, which aredifferent with the neutral framework and easier to form chiral structures. The ion exchangebehavior, gas absorbtion and the fluorescent property are studied and discussed.
3. By using rigid N-donor ligands such as3-BPH,4-BPH and so on, together with rigidcarboxylic acid ligands and transition metal ions, we synthesized four mixed ligand basedMOFs with different structures.Co_2(BPDC)_2(4-BPH)·4DMF (16)Cd(BPDC)(4-BPH)·2DMF (17)Co4(BTC)(C_2H_2N_2O_2)0.5(4-BPH)0.5(DMF)2·H_2O (18)Ni_2(BDC)_2(3-BPH)_2(H_2O)·4DMF (19)
It shows that these MOFs possess flexible coordination modes. Through its adjustablespatial configuration and role of the coordination of nitrogen atoms, novel pillared MOFshave been synthesized. The gas absorbtion property are also studied and discussed
4. Using multi N-containing ligands such as TPB, IP and so on, together with rigidcarboxylic acid ligands and transition metal ions, we synthesized four mixed ligand basedMOFs with different structures.[Cu (TPB)][SO_4] H_2O (20)Zn(TPB)(BDC)·2H_2O (21)Co_2(BPTC)(IP)_4·12H_2O (22)Ni(BPTC)(IP)_2·6H_2O (23)
Study shows that the ligands TPB, IP are not easy to form three-dimensional porousframeworks. Unexpectedly, we get a stable supramolecular framework, where the pore size is1.2nm.
引文
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