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In this present work, the transformation of the Moroccan phosphogypsum (PG) waste, considered a potential source of sulfate, into potassium sulfate compound could help reduce environmental impact and create a new value chain for the phosphate industry. Generally, solid-liquid equilibria are frequently applied in chemical industries. They are a valuable aid in visualizing the precipitation, separation, and purification of a solid phase and the pathways by which crystallization can occur. This process aims to produce potassium sulfate (K 2 SO 4 ), a high-value fertilizer, from sulfate solutions obtained after dissolving PG in a NaOH medium. The quaternary phase diagram Na + , K + //Cl - , SO 4 2- -H 2 O at 25 °C was especially used to determine the operating conditions and the design of a crystallization process during the PG conversion into K 2 SO 4 . The Jänecke representation of this system enables the determination of the optimal trajectory in the phase diagram for the double decomposition reaction. X-ray fluorescent (XRF) and X-ray diffraction (XRD) techniques were conducted to identify the crystalline phases formed during our process. In summary, the results of this study could contribute to the development of a sustainable valorization PG. Furthermore, K 2 SO 4 represents a good alternative to potassium chloride for chloride-sensitive crops., (© 2022. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)