Improving the environmental safety and energy efficiency of water disinfection technologies is a key challenge in ecological engineering. This study proposes and experimentally validates a hybrid intelligent control system for a high – frequency ozonator based on a plasma – liquid process, aimed at maintaining operation within an environmentally safe regime by preventing both excessive and insufficient ozone dosing. Experimental results show that under hybrid control the dissolved ozone concentration is maintained within 0.18 – 0.22 mg/L, whereas under classical control it varies within 0.14 – 0.26 mg/L. The specific energy consumption is reduced from about 0.70 kWh/m³ to 0.52 – 0.58 kWh/m³, providing an energy saving of 22 – 25%. Under severe nonstationary disturbances (step change of water conductivity), the ozone concentration drop is limited to −13% with hybrid control compared to −35% with classical control. These results demonstrate that the proposed control system ensures a stable, energy-efficient, and environmentally safe operation of high – frequency ozonation-based water disinfection systems.