This paper is aimed at investigating activation behaviors for coal-series kaolin using fluidized bed calcination as a novel method. The properties of calcined products at different temperature by fluidized bed calcination were evaluated by determination of weight loss rate, whiteness, chemical oxygen demand (COD), aluminum dissolution degree. The thermal behaviors and reaction mechanism were characterized by thermo gravimetric-differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), particle size distribution (PSD) and scanning electron microscopy (SEM). The results showed that calcination temperature was essential factor determining the properties and crystallinity of calcined products using fluidized bed calcination. Coal-series kaolin transformed into irregular and amorphous metakaolin with excellent properties as calcined at 600-900 °C, which attributed to the dehydroxylation of kaolinite and combustion of carbon/organic matter. Calcined kaolin eliminated activity ascribed to the recrystallization into mullite when calcination temperature was over 1000 °C. It was believed that fluidized bed calcination was an efficient thermal activation technology for coal-series kaolin and the calcination temperature should be controlled accurately.