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In a way to overcome challenges with global warming, the use of fossil fuels in producing environmentally friendly energy towards reducing the ozone layer depletion and greenhouse gas emissions by participating countries is of interest. The adsorption refrigeration system has the advantages of a long lifespan and its environmental friendliness; however, its major disadvantage is the low coefficient of performance which is a function of adsorbent-adsorbate, with Zeolite-water as the most common adsorbent–adsorbate working pair. Zeolite 4A and 13X are the most used Zeolite classes due to their higher selectivity for separating mixtures of CO2/N2 and CO2/CH4/N2 and their high-water adsorption capability, respectively. In this study, for the first time, the synthesis of Zeolite 4A and 13X from natural sources (Kankara kaolin) and the mixture optimization for solar adsorption refrigeration application were considered. Raw Kankara kaolin, beneficiated Kankara kaolin, calcined Kankara kaolin, and synthesised Zeolite 4A and 13X were characterised using X-ray fluorescence (XRF), while the synthesised Zeolite 4A and 13X were characterized using X-ray diffraction (XRD). Using the mixture simplex lattice design of experiment, mixtures of Zeolite 4A and 13X were developed and characterized using Brunauer, Emmett and Teller (BET) analysis to obtain their pore size, specific surface area, and pore volume. The statistical analysis produced the mathematical models of the response which were significant for pore size and specific surface area. The analysis proposed an optimal solution of 75 wt% Zeolite 4A and 25 wt% Zeolite 13X which gave a desirability of 0.944.