The invention relates to a method for deeply separating
molybdenum and
vanadium in a solution containing the
molybdenum and the
vanadium. The method includes: regulating the acidity [H<+>] of the solution containing the
molybdenum and the
vanadium to be 0.0003-10mol / L, and then using the compound of Mo(IV) or / and Mo(V) as the
reducing agent to selectively reduce the vanadium in the solution to obtain liquid after reduction; regulating the pH of the liquid after reduction to be 4-7,
settling the vanadium, and using an
ion exchanging method or extraction method to enrich the molybdenum; or regulating the pH of the liquid after reduction to be 2-4, using an
ion exchanging method or extraction method to enrich the molybdenum, then regulating the pH to 4-7, and
settling the vanadium. The method has the advantages that the E<0>Mo(VI) / Mo(V) and E<0>V(V) / V(IV) potential differences under an acidic condition are utilized, the compound of Mo(IV) or / and Mo(V) as the
reducing agent to selectively reduce the V(V) in the solution into V(IV), and the maximum differentiation of the properties of the molybdenum and the vanadium in the solution is achieved; the property that anion exchange resin or basic extractant can only selectively enrich the Mo(VI) in the solution and cannot absorb the V(IV) is utilized to deeply separate the molybdenum and the vanadium; the method is simple in process, short in process flow, convenient to operate, good in molybdenum-vanadium separation effect, low in treatment cost, environmental friendly, suitable for industrial application, and the like.