The method for separating and recovering cobalt and manganese in low-cobalt high-manganese waste materials with ammonia-sodium carbonate
A technology for separation and recovery, sodium carbonate, applied in the direction of improving process efficiency, etc., can solve the problems of small liquid-solid ratio, low cobalt leaching rate, cobalt is easily wrapped by manganese, etc., to improve recovery rate, low recovery cost, and ensure purity. Effect
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Embodiment 1）
[0033] The cobalt-manganese waste treated in this example is the waste cobalt-manganese catalyst produced in the production of PTA, wherein the content of cobalt is 9.872wt%, and the content of manganese is 17.12wt%.
[0034] The method for separating and recovering cobalt and manganese in low-cobalt high-manganese waste materials with ammonia-sodium carbonate of the present embodiment comprises the following steps:
[0035] ① Pretreatment. Take 13 grams of cobalt-manganese waste and add 220 mL of 5% nitric acid solution to the reaction vessel containing the cobalt-manganese waste. After the cobalt-manganese waste is completely digested, measure the pH value of the acid-dissolved liquid to -0.7. The ratio of the amount of acid to the amount of cobalt-manganese in the spent catalyst is n (H + ) : [ n ( Mn ) + n ( Co ) ] = 2 : 1~4 : 1.
[0036] Heat the acid-dissolved material with a pH value of less than 3.5 in a water bath at 80 °C for 30 min, and filter with suction to remo...
Embodiment 2）
[0051] The method of cobalt and manganese in the low-cobalt high-manganese waste material of the separation and recovery of ammonia-sodium carbonate of the present embodiment is the same as embodiment 1, and difference is:
[0052] After the trivalent cobalt ammonium complex in step ④ is reduced to the divalent cobalt ammonium complex, add sodium oxalate solution dropwise under stirring, after adding n(C 2 o 4 2- ): n(Co)=8:1 ~ 20:1.
[0053] In this embodiment, 150 mL of sodium oxalate solution with a concentration of 50 g / L was added dropwise, the dropping speed was 20 mL / min, and the stirring speed was 500 r / min.
[0054] In addition to the sodium oxalate solution described in this example, ammonium oxalate can also be used instead of sodium oxalate.
[0055] After drying, 3.0421 g of cobalt oxalate was obtained, the recovery rate of cobalt was 95.20%, and the purity of cobalt oxalate was 99.1%. Cobalt in cobalt-manganese waste is recovered in the form of cobalt oxalate...
Embodiment 3）
[0057] The method of cobalt and manganese in the low-cobalt high-manganese waste material of the separation and recovery of ammonia-sodium carbonate of the present embodiment is the same as embodiment 1, and difference is:
[0058] Step 1. during pretreatment, add 10% hydrochloric acid solution 44mL in the reaction vessel that fills cobalt-manganese waste material, after cobalt-manganese waste material is digested completely, the pH value of liquid after measuring acid-dissolving is 4.2. Add 10% hydrochloric acid to the acid-dissolved liquid until the pH drops below 3.5, then transfer to a water bath at 80 °C, heat in a water bath for 30 min, and filter with suction to remove organic matter in the acid-dissolved material.
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