Flexible and Hydrophobic Zn-Based Metal鈥揙rganic Framework
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- 作者：Ines Maria Hauptvogel ; Ralf Biedermann ; Nicole Klein ; Irena Senkovska ; Amandine Cadiau ; Dirk Wallacher ; Ralf Feyerherm ; Stefan Kaskel
- 刊名：Inorganic Chemistry
- 出版年：2011
- 出版时间：September 5, 2011
- 年：2011
- 卷：50
- 期：17
- 页码：8367-8374
- 全文大小：1059K
- 年卷期：v.50,no.17(September 5, 2011)
- ISSN：1520-510X
文摘
A zinc-based metal鈥搊rganic framework Zn2(adb)2(dabco)路4.5 DMF (K) (DUT-30(Zn), DUT = Dresden University of Technology, adb = 9,10-anthracene dibenzoate, dabco =1,4-diazabicyclo[2.2.2]octane, DMF = N,N-dimethylformamide) was synthesized using a solvothermal route. This MOF exhibits six crystallographic guest dependent phases. Two of them were characterized via single crystal X-ray analysis. The as-synthesized phase K crystallizes in the orthorhombic space group Fmmm, with a = 9.6349(9), b = 26.235(3), and c = 28.821(4) 脜 and consists of two interpenetrated pillar-layer networks with pcu topology. When the substance loses 0.5 DMF molecules per formula unit, a phase transition from the kinetic phase K to a thermodynamic phase T occurs. Zn2(adb)2(dabco)路4 DMF (T) crystallizes in the tetragonal space group I4/mmm, with a = 19.5316(8) and c = 9.6779(3) 脜. During the evacuation the DUT-30(Zn) undergoes again the structural transformation to A. The activated compound A shows the gate pressure effect in the low pressure region of nitrogen physisorption isotherm and has a BET surface area of 960 m2 g鈥? and a specific pore volume of 0.43 cm3 g鈥?. Furthermore, DUT-30(Zn) exhibits a hydrogen storage capacity of 1.12 wt % at 1 bar, a CO2 uptake of 200 cm3 g鈥? at 鈭?8 掳C and 0.9 bar, and a n-butane uptake of 3.0 mmol路g鈥? at 20 掳C. The N2 adsorption process was monitored in situ via X-ray powder diffraction using synchrotron radiation. A low temperature induced transformation of phase A to phase V could be observed if the compound was cooled under vacuum to 鈭?96 掳C. A further crystalline phase N could be identified if the framework was filled with nitrogen at 鈭?96 掳C. Additionally, the treatment of activated phase A with water leads to the new phase W.