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The solubilities in the quaternary system K+, NH4+//Cl−, SO42--H2O and its two ternary subsystems NH4Cl-KCl-H2O, (NH4)2SO4-K2SO4-H2O at 80.0 °C were measured using the isothermal dissolution equilibrium method under atmospheric pressure, and the corresponding phase diagrams were plotted. In the phase diagram of the NH4Cl-KCl-H2O system, there are three crystalline zones, which correspond to (K1−m,(NH4)m)Cl, ((NH4)n,K1−n)Cl and the co-existence zone of (K1−m,(NH4)m)Cl and ((NH4)n,K1−n)Cl, respectively. In the phase diagram of the (NH4)2SO4-K2SO4-H2O system, there is only one crystalline zone for (K1−t,(NH4)t)2SO4. In the phase diagram of the K+, NH4+//Cl−, SO42--H2O system, there are three crystal zones, which correspond to (K1−t,(NH4)t)2SO4, (K1−m,(NH4)m)Cl and ((NH4)n,K1−n)Cl, respectively. According to the analysis and the calculations for the phase diagrams of the K+, NH4+//Cl−, SO42--H2O system at 80.0 °C and 50.0 °C, this paper proposes a technological process. In the process, the (K1−t,(NH4)t)2SO4 can be prepared at 80.0 °C and the ((NH4)n,K1−n)Cl can crystallize out at 50.0 °C. The mass fraction of K2SO4 in product L1 (K1−t,(NH4)t)2SO4 (t = 0.1465) is 88.48%. The composition of solid solutions in the K+, NH4+//Cl−, SO42--H2O system was experimentally determined and then theoretical calculations about the process can be carried out. [ABSTRACT FROM AUTHOR]