Optimization of Washing Processes in Solvothermal Synthesis of Nickel-Based MOF-74

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 CO(2) at 1 bar and 25 °C. The final sample of the optimized synthesis routes was able to adsorb 5.80 mmol/g of CO(2) 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.