Bimetallic nanoparticles (NPs) exhibit advantageous electrical, optical, and catalytic properties. Among the various NP synthesis methods, pulsed laser ablation in liquid (PLAL) is currently attracting much attention because of its simplicity and versatility. In this study, a pulsed laser was used to produce nickel/palladium (Ni/Pd) bimetallic NPs in methanol and deionized water. The morphological and optical properties of the resulting Ni/Pd bimetallic NPs were characterized. The synthesized Ni/Pd bimetallic NPs were used for the dechlorination of 1,2-dichlorobenzene (1,2-DCB) under various conditions. The dechlorination rates of 1,2-DCB while using single (Ni and Pd) and bimetallic (Ni powder/Pd and Ni/Pd) NPs were investigated. The results showed that the Ni/Pd bimetallic NPs with 19.16 wt.% Pd exhibited much enhanced degradation efficiency for 1,2-DCB (100% degradation after 30 min). Accordingly, the results of enhanced the degradation of 1,2-DCB provide plausible mechanism insights into the catalytic reaction.