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Updated: Jan 22, 2026
Synthesis and Characterization of Functionalized Metal-organic Frameworks
Published on: September 5, 2014
Dehydration-Assisted Rapid Modulated Synthesis of Monodisperse Covalent Organic Framework Single Crystals With
Yixiao Ren1, Jingtian Cheng1, Jiao Xie1
1State Key Laboratory of Bioinspired Interfacial Materials Science, Institute of Functional Nano & Soft Materials (FUNSOM), Soochow University, Suzhou, China.
Abstract:
The effective control over mesoscale features of covalent organic framework (COF) single crystals is important for definitive structural analysis, systematic structure-performance study, and elucidating crystallization mechanisms. However, the rapid synthesis of COF single crystals with uniform but flexibly tunable size remains a challenge on account of the complicated process of crystallization. Here, we report a dehydration-assisted modulated strategy enabling the rapid synthesis of single-crystalline imine-linked three-dimensional (3D) COFs (COF-300, COF-303, and COF-320). The strategy stems from a systematic study on the role of water in solvothermal and aniline-modulated syntheses of COF-300 using 1,4-dioxane as solvent. Kinetic analyses reveal that the hydrolysis reaction reduces the efficiency of the imine-exchange reaction in regulating the reversible imine bond formation, thereby retarding crystallization in modulated synthesis. Based on this finding, a dehydrated modulated strategy employing hydratable benzonitrile as solvent was developed and flexibly combined with simple adjustments to reaction temperature, solvent, and static/stirring conditions to achieve rapid synthesis of COF-300 single crystals with uniform size tunable from 213 nm to 44.3 µm within 1∼3 h. Crystal size-dependent iodine sorption measurements demonstrate that shortening microporous diffusion paths can accelerate adsorption/desorption kinetics and enhance sorption capacity.
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