In order to enhance the surface area, hole density and adsorption quantity of kaolinite, the authors carried out dispersion treatment of the sheet-like kaolinite after delamination and shattering based on the preparation of urea-kaolinite complex by microwave chemical reaction under further radiation. As a result, nano-kaolinite was obtained. The structures of the samples under processing were studied by Fourier transformation infrared spectrometry (FT-IR) and X-ray diffraction (XRD). The morphologies and sizes of the samples were examined by scanning electronic microscopy (SEM) and transmission electronic microscopy (TEM). The results show that, under the same condition, the time spent on delamination under microwave assistance is only 1/20 of the time spent on the single mechanical method, and that the average size of the nano kaolinite is 150 nm.