The synthesis of dimethyl carbonate (DMC) from CO2 represents a crucial application in C1 chemical conversion, where the alcoholysis of ethylene carbonate (EC) serves as the key step in this route. Although industrial sodium methoxide catalysts exhibit high activity, their strong alkalinity imposes stringent equipment requirements and generates environmental burdens due to non-recyclability and product separation challenges. Bimetal oxide catalysts have emerged as ideal heterogeneous catalytic materials for alcoholysis reactions owing to their tunable Lewis acid-base dual active sites and structural designability. However, current research faces critical scientific issues such as difficulty in synergistic optimization of catalytic activity and stability, unclear structure-activity regulation mechanisms, cumbersome preparation routes, harsh reaction conditions, and insufficient investigation on intensified synthesis strategies for bimetal oxide catalysts, which collectively hinder the design of heterogeneous catalytic systems for DMC synthesis. This study innovatively proposed an ultrasonic hydrothermal-ionic liquid-mediated regulation strategy. By employing the ultrasonic hydrothermal method combined with the ionic liquid [Bmim]BF4 as a structure-directing agent, a Mg-Zr bimetallic oxide catalyst (UIL-MgZrO) with both excellent activity and stability was successfully constructed. The influence mechanisms of the coupling between ionic liquid-mediated processes and different intensified preparation methods on the crystal growth, phase evolution, and surface characteristics of catalysts were systematically investigated, where the gradual transformation of crystals into a stable monoclinic phase with prolonged ultrasonic duration was observed. The operational principles for synergistic regulation of active sites in metal oxides were revealed, thereby improving the catalytic efficiency of bimetallic oxides. In alcoholysis reactions, the UIL-MgZrO catalyst achieved 72.1% EC conversion with 99.9% DMC selectivity under mild conditions (90℃, 1 h), representing top-tier performance among reported heterogeneous catalytic systems. This work provides new strategies for precise regulation of metal oxide surface properties and technical support for CO2-based carbonate synthesis processes, and offers potential applications for energy-related chemical production.