Abstract: MoS₂/TiO₂ nanocomposites was prepared by mixing MoS₂ with hydrothermally synthesized TiO₂; the effects of MoS₂ loading on the photocatalytic performance of MoS₂/TiO₂ in phenol degradation were investigated. The XRD, SEM, EDS, FT-IR and UV-vis DRS characterization results show that for the MoS₂/TiO₂ nanocomposites, lamellar MoS₂ is uniformly dispersed around the TiO₂ nanoparticles. The increase of MoS₂ loading is beneficial to the photocatalytic degradation of phenol; with a MoS₂ loading of 27%, the MoS₂/TiO₂ nanoparticles exhibited the highest photocatalytic activity, over which phenol can be completely degraded in 80 min. The intermediates during reaction are further tracked to investigate the reaction kinetics of photodegradation of phenol over MoS₂/TiO₂ nanocomposties. The results reveal that an increase in MoS₂ loading is able to promote the formation of various intermediates such as benzoquinone, hydroquinone and catechol, which can further enhance the overall photodegradation efficiency.