망간浸出液에서 弗化칼슘化에 의한 高純度 망간酸化物의 製造
Production of High purity Mn₃O₄ powder by Precipitation of Calcium fluoride in the Manganese Leaching Solution
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초록
고탄소페로망간을중저탄소페로망간으로제조하는 AOD공정에서발생되는분진은약 90%가 Mn3O4이므로, 이를이용하여soft ferrite 의원료인고순도 Mn3O4 분말을제조하기위해서는침출한액의 Mn을더욱정제하여야한다. 분진을활성탄으로배소하여 MnO 로환원시키고, 상온의 4N 염산수용액에 180 g/L 의환원된분진을첨가하면용액의 pH가 5이상이되고 Fe와 Si가침전으로제거된약 10%의망간침출액이얻어진다. Mn의농도가약 15000 ppm 이되도록희석한 70oC의침출액에 F의농도가3000 ppm 이되도록 NH4F를첨가하면 Ca가침전하여약 14 ppm 이하로제거된다. Ca 를침전시킨상징액에 1.5M(NH4)2CO3수용액을 2 L/min 으로 Mn의당량만큼첨가하면미립의고순도 MnCO3가침전한다. 침전을여과하고건조한후에 1000oC에서 2 시간소성하면 median size 가 8.2 µm인 Mn3O4를얻을수있다. 제조된산물은 99% 이상의순도로 soft ferrite 용 Mn3O4 분말의규격을만족한다.
Abstract
In order to make the high purity Mn3O4 powder for the raw material of soft ferrite, Mn is extracted from the dust and the extracted solution is refined. The dust is generated in producing a medium-low carbon ferromanganese and contains 90% Mn 3O4. Mn3O4 in the dust was reduced into MnO by roasting with charcoal. Injection of the 180 g/L of the reduced dust into 4N HCl solution increased pH of the leaching solution higher than 5 and then a ferric hydroxide was precipitated. Because the ferric hydroxide co-precipitates with Si ion etc, Fe and Si ion was removed from the solution and the about 10% Mn solution was obtained. The solution was diluted with water to Mn-15000 ppm and NH4F was injected into the diluted solution at 70oC to the F-3000 ppm. As a result, Ca ion is precipitated as CaF2 and the residual concentration of Ca was 14 ppm. Injection of the equivalent 1.5M (NH4)2CO3 solution as 2 L/min at 25oC into the above solution precipitated a fine and high purity MnCO3 powder. The deposition was filtrated and roasted at 1000oC for 2 hours. As a result, MnCO3 powder is converted into Mn3O4 powder and it had 8.2 µm of median size. The final production is above 99% Mn3O4 powder and it satisfied the requirement of high purity Mn3O4 powder for a raw material of soft ferrite.