This　study　proposes　a　technical　route　toward　the　comprehensive　recovery　of　valuable　metals　from　spent　Ni-Mo/　gamma-Al2O3　hydrofining　catalysts,　which　were　employed　to　remove　S,　N,　and　O　elements　and　metal-organic　compounds　from　crude　oil　and　petroleum　products.　Additionally,　the　process　conditions　are　optimized,　thereby　providing　good　economic　and　environmental　benefits.　Sodium　carbonate-assisted　roasting　of　the　spent　catalyst　effectively　improves　the　secondary　pollution　and　leaching　effect.　After　Al,　Mo,　and　Ni　elements　in　the　spent　catalyst　were　converted　into　NaAlO2,　Na2MoO4,　and　NiO,　more　than　99.8%　of　the　metal　ions　entered　the　leaching　solution,　minimizing　the　loss.　A　synergistic　extraction　system　using　the　di-(2-ethylhexyl)phosphoric　acid　(P204)　and　tri-n-octylamine　(TOA)　extractants　were　employed　to　extract　molybdenum　from　the　clarified　acid　leaching　solution,　and　more　than　97.5%　of　Mo　was　separated　from　Al　and　Ni.　The　MoO3　product　was　obtained　by　stripping　with　ammonia,　followed　by　evaporating,　and　roasting.　Furthermore,　by　adding　ammonia　to　adjust　the　pH　value　of　the　molybdenum　extraction　solution　to　4,　98.0%　of　the　Al　was　extracted　by　P204.　Subsequently,　a　Na2S　precipitation　agent　was　employed　to　convert　Ni2+　into　Ni(OH)S　with　a　precipitation　efficiency　of　97.9%.　Ultimately,　the　comprehensive　recovery　efficiencies　of　Al,　Mo　and　Ni　were　97.5%,　95.5%,　and　90.9%,　respectively,　thereby　realizing　the　comprehensive　recovery　of　metals　in　the　spent　catalyst.