Abstract
Solvothermal synthesis is the most preferable preparation technique of metal–organic frameworks (MOFs) that consists of reactants mixing, ultrasonication, solvothermal reaction, product washing, and solvent evacuation. Owing to fast reaction kinetics in solvothermal reaction, this technique allows for production of uniform MOF particles with high crystallinity, high phase purity, and small particle sizes. However, it exhibits some difficulties of washing processes that may involve the blockage of pores due to incomplete removal of reactive medium from MOF products. The present study proposes an improvement of washing processes by introducing centrifugal separations with optimized parameters at two different stages: after reaction and after product washing. Nickel-based MOF-74 was synthesized as the experimental material for this purpose. The quality of the produced sample was evaluated by gas adsorption performance using CO2 at 1 bar and 25 °C. The final sample of the optimized synthesis routes was able to adsorb 5.80 mmol/g of CO2 uptake, which was competitive with literature data and significantly higher than the sample of the basic synthesis. Fourier-transform infrared spectroscopy (FTIR) and powder X-ray diffraction (PXRD) analysis revealed that the sample displayed much higher crystallinity structure and was clean from impurities after centrifugations. The outcome indicated the success of separation between MOF products and reactive medium during washing processes, leading to the effective pore activation of MOFs.
Highlights
Metal-organic frameworks (MOFs) are the assembly of metal-containing nodes coordinated to organic bridging ligands giving rise to characteristic three-dimensionally ordered crystalline structures [1]
The present study proposes an optimization of washing techniques in solvothermal synthesis of MOFs
Ni-MOF-74 powder was successfully synthesized and confirmed by the powder X-ray diffraction (PXRD) result, which was in agreement with the diffractions calculated from the reference structure available in Cambridge
Summary
Metal-organic frameworks (MOFs) are the assembly of metal-containing nodes coordinated to organic bridging ligands giving rise to characteristic three-dimensionally ordered crystalline structures [1]. The research area of these materials has grown tremendously, leaving behind other porous solids due to its superior potential advantages. MOFs are recognized for their ability to provide large nanoporous volumes and immense specific surface areas for numerous applications [2]. MOF pore structures are able to act as catalytic sites allowing their application in nanocatalysis [3]. MOF magnetic properties and their different adsorption behavior towards various gases allow their application in gas sensing [4]. The excellent biocompatibility of MOFs and their ability
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