Interfacial Synthesis of Free‐Standing Metal–Organic Framework Membranes

化学 金属有机骨架 过渡金属 无机化学 催化作用 硝酸锌 羧酸盐 己烷 对苯二甲酸 二甲基甲酰胺 溶剂 高分子化学 有机化学 吸附 聚酯纤维 生物化学
作者
Hongyu Lu,Shiping Zhu
出处
期刊:European Journal of Inorganic Chemistry [Wiley]
卷期号:2013 (8): 1294-1300 被引量:63
标识
DOI:10.1002/ejic.201201009
摘要

Abstract A method based on a liquid–liquid interfacial coordination mechanism has been developed for the synthesis of free‐standing metal–organic framework (MOF) membranes. MOF precursors, zinc nitrate [Zn(NO 3 ) 2 ] and terephthalic acid (TPA or H 2 BDC), as well as catalyst triethylamine (TEA), were dissolved in two immiscible solvents, dimethylformamide (DMF) and hexane. The reaction of Zn(NO 3 ) 2 and TPA (at a 2:1 molar ratio) in DMF was catalyzed by TEA in hexane at the solvent interface thus forming a free‐standing membrane. A region of reactant concentrations critical to membrane formation was identified; a free‐standing membrane could only be formed in the region of high Zn/TPA and low TEA concentrations. The combination of low Zn/TPA and high TEA concentrations yielded MOF particles that precipitated from DMF. The membranes were characterized by SEM and XRD and found to be asymmetric. SEM results showed that the top layer was particulate, whereas the bottom layer had a sheet‐like morphology, which was further revealed by XRD data as 3D Zn 4 O(BDC) 3 (also known as MOF‐5) and 2D ZnBDC · DMF (MOF‐2) for the top and bottom, respectively. Other transitional zinc–carboxylate structures between the two MOFs, namely Zn 3 (OH) 2 (BDC) 2 (MOF‐69c) and Zn 5 (OH) 4 (BDC) 3 , were also observed with small signal intensities revealing a transition of coordination modes between zinc ions and BDC groups from 3D to 2D at the membrane cross‐section. This was caused by a change of the TEA diffusion rate during the synthesis process, which might change the pH and alter the membrane growth. From both SEM and XRD characterizations, MOF‐2 is the dominant material in the overall composition. Nitrogen adsorption tests showed an average Langmuir surface area of 709 m 2 /g for the membrane, demonstrating its potential for gas separation applications.
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