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Abstract: Novel Pd-carrying composite carbon nanofibers based on polyacrylonitrile were prepared by electrospinning and carbonization process. The catalytic activities of the composite nanofibers were tested with a Sonogashria coupling reaction of iodobenzene and phenylacetylene in liquid-phase. Transmission electron microscope and X-ray diffraction analyzer were used to characterize the nanofibers and the metal nanoparticles on the fibers; gas chromatograph and nuclear magnetic resonance spectroscopy were used to characterize the product of the testing reaction. The results first showed that the catalyst not only had a high catalytic activity, but also had good leaching-resistance, retrieval and reusability for the Sonogashira reaction. [Copyright &y& Elsevier]