Molten　salt　electrolysis　is　used　to　separate　and　recycling　of　elemental　tungsten　and　cobalt　from　cemented　carbides.　WC-6　wt%　Co　scrap　and　NaCl-KCl　molten　salt　was　used　as　a　sacrificial　anode　and　electrolyte,　respectively.　The　range　of　preparation　parameters　and　the　electrochemical　behavior　of　tungsten　and　cobalt　ions　were　investigated　through　electrochemical　techniques,　such　as　cyclic　voltammetry　(CV)　and　square　wave　voltammetry　(SWV).　Results　showed　that　the　dissolution　potential　of　cobalt　and　WC　were　0　V　and　0.6　V　(vs.　Ag/AgC1),　and　the　reduction　potentials　of　Co　(II)　+　2e(-)　＜-＞　Co　(0)　and　W(II)　+　2e(-)　＜-＞　W　(0)　were　-0.2　and　0.2　V　(vs.　Ag/AgC1),　respectively.　The　reduction　processes　of　Co(II)　to　Co　and　W(II)　to　W　were　both　reversible　reactions　controlled　by　ion　diffusion.　The　average　diffusion　coefficients　of　Co(II)　and　W(II)　were　determined　by　CP　to　be　5.62　x　10(-5)　sand　3.94　x　10(-5)　cm(2)　s(-1),　respectively.　Furthermore,　the　products　at　cathodes　Nos.　1　and　2　were　characterized　by　scanning　electron　microscopy,　X-ray　fluorescence　and　X-ray　diffraction　analyses.　Results　showed　that　pure　cobalt　and　WC　powder　with　a　diameter　of　＜　100　nm　was　obtained　at　cathode　No.　1　and　cathode　No.　2.　And　the　result　of　XRF　shows　that　the　purity　of　the　products　both　Co　and　WC　were　higher　than　90%.　This　study　reveals　that　cobalt　and　tungsten　can　be　separated　from　WC-6　wt%　Co　scrap　by　controlling　process　parameters　during　electrolysis.