During the process of in situ polymerization of Ani in the exfoliated ot-zirconium phosphate, ethylamine, butylamine and tetrabutyl oxyammonia (TBA+OH-) were used to exfoliate a-ZrP, and ammonium persulfate(APS)was oxidant. The composites of a·zirconium phosphate/polyaniline (α-ZrP/PANi) were synthesized in acidic aqueous solution. The structures and properties were studied by fourier transform infrared (F-IR)spectra, X-ray diffraction(XRD), the standard four probe technique. And scanning electron microscopy (SEM). AU of the results show that strong interactions exist between exfoliated α-ZrP and PANi molecule. Comparing with non-exfoliation α-ZrP/PANi. Their conductivity increased. With the different exfoliated agents loading, obvious variations on structures and conductivity of the composites were observed. Larger layer distance of exfoliated α-ZrP would result in improved conductivity of composites.