With potassium acetate as an intercalation agent, kaolinite-potassium acetate(KAc) intercalation complexes was prepared. Afterwards, nano-kaolinite was successfully made through exfoliated intercalation complexes using power ultrasonic. The intermediate and final products were characterized by X-ray diffraction(XRD), infrared spectroscopy(IR), laser particle size analyzer, and scanning electron microscope (SEM). The results show that intercalation of KAc into kaolinite resulted in a crystal space expansion, from a basal spacing of 7.14Ǻ to 14.20 Ǻ, and the intercalation rate was about 80%. KAc intercalation causes the weakening of interlayer stability. It was shown that the particles of nano-kaolinite is very thin lamellar in shape, whose average thickness, average particle size, are 50 nm and 450 nm respectively.