Carbon modified-titanium dioxide (@C-TiO2) was prepared by one-pot procedure from TiCl4 and glucose under hydrothermal conditions at 150 ºC for 24 hours. The obtained @C-TiO2 was employed as support for Ni-Ag(3.0)@C-TiO2 nanocomposite (3.0 is the Ni/Ag molar ratio). The synthesized catalysts were characterized by means of XRD and UV-Vis DRS Spectroscopy. The XRD patterns of @TiO2 show the brookite as the main phase, meanwhile the main phase in the @C-TiO2, Ni-Ag(3.0)@TiO2 and NiAg(3.0)@C-TiO2 nanocomposites were anatase. The band gap of the TiO2 sample slightly shifted to the visible range after the addition of C dopant or Ni-Ag(3.0) co-catalyst as indicated by UV-Vis DRS spectra. Ni-Ag(3.0)@C-TiO2 catalyst showed high photocatalytic activity for photodegradation of MB under both UV and visible irradiations at 60 ºC within 2 hours with maximum MB conversion of 67.5% and 54.1%, respectively. The synergistic action of C dopant or Ni-Ag(3.0) co-catalyst is believed to be important in the improvement of photocatalytic activity of @TiO2. Copyright ©2019 BCREC Group. All rights reserved Keywords: C-doped TiO2; bimetallic Ni-Ag co-catalyst; methylene blue; photodegradation How to Cite: Putri, K., Annisa, A., Husain, S., Rodiansono, R. (2020). One-pot Synthesis of Carbondoped TiO2 with Bimetallic Ni-Ag co-catalysts in Photodegradation of Methylene Blue under UV and Visible Irradiation. Bulletin of Chemical Reaction Engineering & Catalysis, 15(1): 35-42 (doi:10.9767/bcrec.15.1.4811.35-42)