Combined with the characteristics of flotation feed originating from China’s Panyidong Coal Preparation Plant, the ash, zeta potential, X-ray fluorescence spectroscopy and contact angle test were used to study changes in the surface properties of flotation feed under ultrasonic pre-treatment, and its effect on flotation of coal slime. Results show that Preferred pre-treatment process is ultrasonic secondary treatment, ultrasonic secondary pre-treatment can remove most of the high-ash fine mud for instance kaolinite, montmorillonite and quartz in the coal slurry, reduce the surface electronegativity of coal particles, and increase the contact angle of coal particles. Thus, the concentrate ash content decreases to 13%, the recovery rate, yield of flotation concentrate and combustible matter recovery reach 92.6%, 90.9% and 97.6%, respectively.