Ammonia (NH) exposure has a serious impact on human health because of its toxic and corrosive nature. Therefore, efficient personal protective equipment (PPE) such as masks is necessary to eliminate and mitigate NH exposure risks. Because economically and environmentally viable conditions are of interest for large-scale manufacture of PPE, we herein report a benign procedure to synthesize a Zn-azolate metal-organic framework (MOF), MFU-4, for NH capture. The surface area and morphology of MFU-4 obtained in alcohol solvents at room temperature is consistent with that of traditionally synthesized MFU-4 in ,-dimethylformamide at 140 °C. In addition to its large NH uptake capacity at 1 bar (17.7 mmol/g), MFU-4 shows outstanding performance in capturing NH at low concentration (10.8 mmol/g at 0.05 bar). Furthermore, the mild synthetic conditions implemented make it facile to immobilize MFU-4 onto cotton textile fiber. Enhanced NH capture ability of the MFU-4/fiber composite was also attributed to the well-exposed MOF particles. The benign synthetic MFU-4 procedure, high NH uptake, and easy integration onto fiber pave the way toward implementation of similar materials in PPE.