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Atmospheric water capture (AWC) has tremendous potential to address the global shortage of clean drinking water. The Ni₂Cl₂(BTDD) metal–organic framework (MOF) has shown optimal water sorption performance under low relative humidity conditions, but its potentially high production costs, stemming in part from its lengthy multiday synthesis, has hindered widespread implementation. As with most traditional MOF syntheses, the original synthesis of Ni₂Cl₂(BTDD) involves batch reactors that have intrinsic inefficiencies impacting productivity during scale-up. We report a continuous manufacturing process for Ni₂Cl₂(BTDD) that can achieve higher yields, reduced solvent use, and drastically faster crystallization times in comparison to the batch process. Optimization of the synthesis space in the flow reactor as a function of residence time, temperature, and solvent volume yields 50% and 40% reductions in …