The composite photocatalyst NixMo1-xS2/MOF-5@g-C3N4 was successfully synthesized by means of hydrothermal with two step methods and the effective photocatalytic activity improvement was obtained. With the introduction of NixMo1-xS2, the H-2 production reached the maximum about 319 mu mol under continuous visible light irradiation for 5 h, which was 30 times higher than that of pure g-C3N4 photocatalyst. A series of characterization results shown that the MOF-5@g-C3N4 on the surface of NixMo1-xS2 provided the more active sites and improved the efficiency of photo-generated charge separation with SEM, XRD, TEM, EDX, XPS, UV-vis DRS, BET, FTIR, transient fluorescence and electrochemistry etc. and the results of which were in good mutual corresponding with each other. Furthermore, the reaction mechanism over the compound catalyst NixMo1-xS2/MOF-5@g-C3N4 was proposed. (C) 2018 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.