DMSO was used to intercalate kaolin by means of ultrasonic oscillation which was different from traditional method, this could shorten the intercalation time greatly, and high intercalation effect was obtained. This paper considered four factors together in the experiment and made the experimental tabulations by means of orthogonal method, then made several groups of samples. The paper contrasted the effect of intercalation using orthogonal table of volume method and optimized the best factor combination. At the same time, the compound was investigated by micro-picture pick-up system. The microscope images indicated that the dispersity of kaolin intercalated was better and the particle size was smaller and more uniform.