Binary　Mn-Co　oxides　were　prepared　by　means　of　homogeneous　coprecipitation　with　various　Mn/Co　molar　ratios　to　investigate　the　effect　of　interaction　between　manganese　and　cobalt　on　the　catalytic　combustion　of　volatile　organic　compounds　(VOCs).　It　was　found　that　the　catalytic　activities　of　Mn-Co　oxides　for　VOC　combustion　were　higher　than　that　of　monometallic　oxides　(MnOxor　CoOx),　showing　a　synergistic　effect.　Kinetic　studies　showed　that　the　catalytic　activity　was　highly　dependent　on　the　property　of　oxygen　and　the　reaction　pathway　followed　the　Mars-van　Krevelen　(MvK)　mechanism　with　oxygen　in　dissociative　adsorption.　Temperature-programed　reduction　with　H2and　X-ray　photoelectron　spectroscopy　results　illustrated　that　the　interaction　between　manganese　and　cobalt　resulted　in　a　higher　concentration　of　Mn4+/Mn3+and　Co2+/Co3+redox　pairs,　which　favored　the　formation　of　active　oxygen　species　and　oxygen　mobility　and　thus　enhanced　the　catalytic　activity.　Moreover,　the　Mn1Co1Oxcatalyst　exhibited　high　stability　in　the　presence　of　water　vapor.　Furthermore,　diffuse　reflectance　infrared　Fourier　transform　spectroscopy　results　indicated　that　toluene　reacted　with　the　oxygen　of　the　catalyst　to　generate　benzyl,　benzyl　alcohol,　and　benzoate　species　in　consecutive　steps.　Finally,　the　benzoate　species　were　fully　oxidized　to　CO2and　H2O,　which　was　the　rate-determining　step　for　the　catalytic　combustion　of　VOCs.　These　results　provided　a　guideline　for　the　future　development　of　superior　catalysts　via　regulating　synergism　among　distinct　metals　for　the　catalytic　removal　of　VOCs.　©　2022　American　Chemical　Society.　All　rights　reserved.