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Application of support materials in nanoparticle technology can effectively preserve the reactivity of nanoparticles through preventing nanoparticle aggregation. In this study, the composite of activated carbon fiber-supported bimetallic Fe/Ni nanoparticles (ACF-Fe/Ni) was synthesized and several characterizations for ACF-Fe/Ni were carried out, including scanning electron microscopy, Brunauer-Emmett-Teller surface area, X-ray diffraction, and X-ray photoelectron spectroscopy. Subsequently, dechlorination performance of ACF-Fe/Ni toward chloroform (CF) was evaluated via a series of batch experiments. Results showed that 92.1% of CF was removal by ACF-Fe/Ni within 45 min, higher than that of raw Fe/Ni (63.3%) and ACFs (13.7%) under the identical condition. Analysis of dechlorination products and chloride ion formed during the dechlorination process indicated that the possible pathway of CF removal by ACF-Fe/Ni included hydrogenolysis and complete dechlorination. Moreover, influence of key parameters manifested that rising ACF-Fe/Ni dosage and ambient temperature and lowering initial pH value were conducive to the removal of CF. Common ions and sulfur compounds both showed a detrimental effect on the removal of CF by ACF-Fe/Ni, specifically sulfides almost completely inhibiting the reactivity of ACF-Fe/Ni.