In the current study, two series of catalysts were synthesized and characterized by various physicochemical techniques. In the first series of catalysts, a chemical precipitation method was used for loading 1–20 wt. % ZrO₂ on the surface of sugarcane bagasse fly ash (SCBFA) with the goal of finding out the optimal ZrO₂ loading. In the second series, the 20% ZrO₂/SCBFA composition was modified by (1–10 wt. %) SO₄²⁻ by wet impregnation method. The acidity of these catalysts was determined through the dehydration of isopropyl alcohol and the chemisorption of pyridine and 2,6‐dimethyl pyridine. The catalytic efficiency for the dehydration of methanol to dimethyl ether (DME) in a fixed‐bed reactor at atmospheric pressure was investigated. A ~ 95% yield toward DME is maximized over the 10% SO₄²⁻/20% ZrO₂/SCBFA catalyst at a reaction temperature of 400°C. Additionally, it maintained nearly the same …