The invention discloses a preparation method of nano antimony thioantimonate, wherein the preparation method comprises the steps: adding a sodium thioantimonate solution into a complex solution of trivalent antimony, dispersing with ultrasonic waves, controlling the temperature of the reaction system at 20-35 DEG C, adjusting the pH value of the reaction system to 6.3-7.8 with hydrochloric acid, after completion of addition of the sodium thioantimonate solution, continuing to disperse for 10-15 min by ultrasonic waves, filtering to take a filter residue, washing the filter residue with a potassium sodium tartrate solution and purified water, and grinding for 3-5 h by a ball mill, and thus obtaining the product. The content of sulfur in antimony thioantimonate obtained by the preparation method provided by the invention is low, the product is stable and pure, the yield is high, the properties are good, the particles are in nanoscale, and the nano antimony thioantimonate has the advantages of good compatibility with lubricating grease, good extreme pressure wear resistance and good lubrication performance; as an additive, the nano antimony thioantimonate has various properties far beyond the requirements of the national standards on extreme pressure lubricating grease, can be industrially produced and has a good application prospect.