Herein, perylene-3,4,9,10-tetracarboxylic acid-doped polyaniline (PTP) nanofibers with/without photoreactive anatase TiO 2 (TiO 2 –PTP and PTP, respectively) have been successively synthesized and subsequently decorated by Pt nanoparticles (Pt NPs) to prepare Pt–PTP and Pt–TiO 2 –PTP composites. High-resolution transmission electron microscopy confirms the presence of ∼3 nm spherical-shaped Pt NPs on both the composites along with TiO 2 on Pt–TiO 2 –PTP. Pt loading on the composites is deliberately kept similar to compare the methanol electro-oxidation in the two composites. The Pt nanocomposites along with the precursor polyanilines are characterized by optical characterization, X-ray diffraction study, X-ray fluorescence spectroscopy, and Raman spectroscopy. The ternary composite-modified (Pt–TiO 2 –PTP) electrode demonstrates high electrocatalytic performance for methanol oxidation reaction in acid medium than Pt–PTP and Pt–TiO 2 . The higher electrochemical surface area (1.7 times), high forward/backward current ratio, and the higher CO tolerance ability for Pt–TiO 2 –PTP make it a superior catalyst for methanol oxidation reaction in the electrochemical process than Pt–PTP. Moreover, the catalytic activity of Pt–TiO 2 –PTP is further enhanced significantly with light irradiation. The cooperative effects of photo- and electrocatalysis on methanol oxidation reaction in Pt–TiO 2 –PTP enhance the methanol oxidation catalytic activity approximately 1.3 times higher in light illumination than in dark. Therefore, the present work will be proficient to get a light-assisted sustainable approach for developing the methanol oxidation reaction activity of Pt NP-containing catalysts in direct methanol fuel cells.

Density functional theory calculations suggest the formation of an oxocarbenium ion intermediate in acid catalyzed ring-opening reactions of biomass derived lactones, which may play an important role in determining it's reactivity.

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