In this paper, the authors applied microwave techniques to the preparation of kaolinite/organics intercalated compound. The effects of microwave during intercalation, displacement and in situ polymerization were investigated through DMSO and aerylamide. The result shows that the microwave energy can accelerate intercalation and displacement reactions. After 30 minutes of reaction, the intercalation rate reached 75%. The displacement rate of acrylamide reached above 77% after 50 minutes of irradiation. It is also found that the microwave energy has the exfoliation effect on kaolinite. The intercalated compound and the reaction principle of microwave irradiation were studied by such means as FT-IR, XRD, TG and TEM.