In this study, α-ZrP-CPC layered compound was gained by inserting cetyl pyridinium chloride (CPC) into α-ZrP with amines as pillaring agent. The amount of CPC intercalated reached the highest with the molar ratio of the amine/α-ZrP being 2. The lower concentration of CPC resulted in more CPC molecules intercalated into the interlayer of α-ZrP. The intercalation products were characterized by XRD, IR, TG-DSC and SEM. The result of TG-DSC showed that the amount of xylene adsorbed reached the peak value of 5.56%, when the content of CPC in α-ZrP-CPC was 41%.