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含钼酸浸液为高温合金废料经氧化酸浸所得,其Mo浓度为0.67 g·L~(-1),采用离子交换法从含钼酸浸液中选择性提取钼;采用碳酸钠溶液调整含钼酸浸液p H后,先用D296树脂从含钼酸浸液中吸附钼,再用氨水和氯化铵混合溶液解吸钼,所得钼酸铵溶液经蒸发浓缩后冷却结晶制得钼酸铵白色晶体,使酸浸液中钼得到有效回收。实验结果表明:通过静态吸附法选择D296强碱性阴离子交换树脂作为Mo的吸附树脂;当树脂床体积为10 ml,反应温度为25℃、料液p H为2、吸附流速为45 ml·h~(-1)时,Mo吸附率达到98.45%;通过Mo吸附曲线测定D296树脂吸附Mo的饱和容量为50 mg·g-1;当氨水浓度为5%,氯化铵浓度为30 g·L~(-1),树脂床体积为10 ml,氨水和氯化铵混合溶液用量为80ml,解吸流速为10 ml·h~(-1),解吸后液中Mo浓度为3.282 g·L~(-1),Mo解吸率达到99.52%;当钼酸铵溶液含钼浓度达到60 g·L~(-1)以上,再冷却至常温结晶12 h以上,所得钼酸铵白色晶体纯度达到97.95%。
The molybdic acid-containing immersion liquid was obtained by oxidative acid leaching of the superalloy scrap. The Mo concentration was 0.67 g · L -1, and molybdenum was selectively extracted from the molybdic acid-containing immersion liquid by ion exchange method. The concentration of Mo was adjusted by sodium carbonate solution Molybdenum acid leaching solution p H, the first with D296 resin from molybdenum acid leaching solution adsorption molybdenum, ammonia and ammonium chloride solution and then desorption of molybdenum, the resulting ammonium molybdate solution was concentrated by evaporation after cooling crystallization of molybdenum acid Ammonium white crystals, the acid soak molybdenum was effectively recovered. The experimental results showed that D296 strongly basic anion exchange resin was selected as the adsorption resin of Mo by static adsorption method. When the volume of resin bed was 10 ml, the reaction temperature was 25 ℃, the feed liquid p H was 2 and the adsorption flow rate was 45 ml · h ~ (-1), the adsorption rate of Mo reaches 98.45%. The Mo adsorption capacity of MoO 2 is 50 mg · g-1. When the ammonia concentration is 5%, the concentration of ammonium chloride is 30 g · L ~ (-1), the volume of resin bed was 10 ml, the amount of mixture of ammonia and ammonium chloride was 80ml, the desorption flow rate was 10 ml · h -1, the concentration of Mo in the solution after desorption was 3.282 g · L ~ (-1) -1), and the desorption rate of Mo reached 99.52%. When the content of molybdenum in ammonium molybdate reached above 60 g · L -1, the purity of white crystals of ammonium molybdate was 97.95% .