This study explored the hydrothermal synthesis of zeolites in a homogeneous reactor using coal fly ash (CFA) as a raw material via a two-step method at normal pressure. Fourier transform infrared spectroscopy and X-ray powder diffraction analysis showed that the synthetic products has the basic structural unit of microporous zeolite molecular sieves, and consiste of zeolite 4A and zeolite X. The ability of zeolites synthesized from CFAto adsorb Cu(ll) was studied. The optimal conditions for adsorption were as follows: pH 5 and dosage of modified CFA 4g l(-1). The isothermal adsorption of zeolites of Cu(ll) showed that the maximum adsorption quantity ranged from 69.44 (at 20 degrees C) to 140.85 mg g(-1) (at 50 degrees C). Adsorption kinetics analysis showed that chemical adsorption was the rate-controlling step. Apparent activation energy data, however, showed that the process of adsorption of Cu(II) had the features of physical adsorption. Thus, the adsorption process included both chemical and physical adsorption.