A process for preparing of the delaminated kaolinite was developed with intercalation of hydrazine, urea or potassium acetate followed by removing the chemical assistants. Delaminated kaolinite was characterized by XRD, solid-state NMR, thermal analyses, particle-size distribution analyses, etc. The particle size was reduced to ca. 440 nm in diameter and ca.15 nm in thickness in contrast to about 7 μm and 800 nm for untreated precursor respectively. The dehydroxylation temperature of kaolinite was shifted from 514°C to 490°C by the delamination. Additionally, a greater mass lost was also observed for the delaminated particles by dehydroxylation.