Poly(N-(2-hydroxyethyl)aniline) microsphere was prepared in aqueous hydrochloric acid (HCl) in one step, using ammonium persulphate as an oxidant. The effect of monomer, oxidant, HCl concentrations and temperature on polymerization rates was investigated. The data show that polymerization rate increases with increasing reactant concentrations. In addition, the initial rate increases with raising the temperature. The apparent activation energy found was 57.4319 kJ/mole. Also, ÁH* and ÁS* found were 55.0691 kJ/mole and 78.3662 J/mole K respectively. Infrared and proton nuclear magnetic resonance spectroscopies, thermogravimetric analysis, X-ray diffraction, scanning electron microscopy and elemental analysis characterize the obtained polymer sample to confirm the suggested structure. The mechanism of the polymerization reaction are discussed.