Aging oil is a common pollutant in petrochemical enterprises due to its severe emulsification and flocculation, poor settling performance, low oil recovery rate, and high difficulty in treatment. This article adopts the method of mechanical, ultrasonic, and chemical coupling demulsification to treat aging oil, with the water content and oil recovery rate of the treated aging oil as the inspection indicators. The experiment shows that when the oil-water ratio is 1:4, the heating temperature is 50℃, the stirring speed is 180rpm, the ultrasonic frequency is 25kHz, the power is 40W, the ultrasonic time is 25min, and the pH is adjusted to 3-4. The additional amount of FeSO4 is 160mg/L, the additional amount of H2O2 is 0.11%, and the heating stirring reaction is 40min. When the dosage of cationic PAM with an ion degree of 50 is 35mg/L, the centrifugation speed is 3200rpm. The centrifugation time is 20 min, the crude oil recovery rate after aging oil treatment can reach over 94.6%, and the water content of the treated crude oil is less than 0.5%, meeting the standards for crude oil gathering and transportation in China. The oil content in the water generated after aging oil treatment is about 150 mg.L-1, the suspended solids content is 200 mg.L-1, the oil content in the residue is 6%, and the water content is 53%. By analyzing the appearance of aging oil before and after treatment, it was found that when using this process to treat aging oil, the original spatial cross-linking network structure of the aging oil was broken, allowing the water droplets wrapped in the oil to be released, thereby significantly reducing the water content in the recovered oil and improving the oil recovery rate.