From Bench to Bulk: Investigating Kinetics, Recyclability, and Scale‐Up of ZIF‐67

ABSTRACT Zeolitic imidazolate framework‐67 (ZIF‐67), a subclass of metal–organic frameworks (MOFs), has garnered considerable attention due to its high surface area, open crystal structure, tunable porosity, and potential applications in gas separation, catalysis, and carbon capture. However, large‐scale synthesis remains limited due to challenges in reproducibility, high solvent usage, and poorly understood reaction kinetics. This study investigates the coprecipitation method for synthesizing ZIF‐67, aiming to develop a simple, cost‐effective, and sustainable approach, emphasizing scalability and ease of production. This study systematically explores the effect of key reaction parameters such as impeller speed, molar ratio of precursors, reaction temperature, aging time, and solvent type on the morphology, particle size, and surface area of the synthesized ZIF‐67 particles. To improve the process sustainability, the reuse of the mother liquor is also explored. A detailed kinetic analysis confirms that ZIF‐67 synthesis is mass transfer–controlled, with a low activation energy (0.643 kJ/mol), highlighting the importance of effective mixing and reactor design. The optimized scale‐up yielded ZIF‐67 with a surface area of 1368.7 m 2 /g and consistent rhombic dodecahedral morphology, validating the scalability of the laboratory‐developed process. Advanced characterization techniques, such as X‐ray diffraction, scanning electron microscopy, particle size analysis, and Brunauer–Emmett–Teller surface area analysis, are employed to assess crystallinity, morphology, particle size distribution, and surface area, respectively. This study aims to bridge the gap between academic research and industrial‐scale production by integrating chemical engineering principles into the synthesis of ZIF‐67. The objective is to develop an optimized, reproducible synthesis protocol that can serve as a blueprint for scaling up other MOFs for real‐world applications.