The present work describes the novel application of Fe–Zn double metal cyanide complexes as solid acid catalysts for the synthesis of nopol from β-pinene. The series of Fe–Zn double metal cyanide complexes were prepared from aqueous solutions of ZnCl 2 and K 4 Fe(CN) 6 ·3H 2 O in the presence of tert-butanol, iso-butanol and n-butanol (complexing agent) and tri-block copolymer EO 20 PO 70 EO 20 (average molecular weight, 5800; co-complexing agent). The catalysts prepared were characterized by X-ray diffraction, thermal analysis, diffuse reflectance UV–vis and FT-IR spectroscopy. All the catalysts were found to be active solid acid catalyst for Prins condensation reaction between paraformaldehyde and β-pinene in the synthesis of nopol. Coordinatively unsaturated Zn 2+ ions in the framework of Fe–Zn double metal cyanide complexes are found to be possible active sites.