Production of High purity $Mn_3O_4$Powder by Precipitation of Calcium fluoride in the Manganese Leaching Solution

망간침출액에서 불화칼슘화에 의한 高純度 망간酸化物의 製造

  • 한기천 (인하대학교 자원공학과) ;
  • 이계승 (인하대학교 자원공학과) ;
  • 최재석 (한국건자재실험연구원) ;
  • 신강호 (삼척대학교 자원공학과) ;
  • 조동성 (인하대학교 자원공학과)
  • Published : 2002.02.01

Abstract

In order to make the high purity Mn$_3$O$_4$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$_3$O$_4$. Mn$_3$O$_4$in the dust was reduced into MnO by roasting with charcoal. Injection of the 180g/L of the reduced dust into 4N HCI 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 $NH_4$F was injected into the diluted solution at $70^{\circ}C$ to the F-3000 ppm. As a result, Ca ion is precipitated as $CaF_2$and the residual concentration of Ca was 14 ppm. Injection of the equivalent (NH$1.5M_4$)$_2$$CO_3$solution as 2 L/min at $25^{\circ}C$ into the above solution precipitated a fine and high purity $MnCO_3$powder. The deposition was filtrated and roasted at $1000^{\circ}C$ for 2 hours. As a result, $MnCO_3$powder is converted into $Mn_3$$O_4$powder and it had $8.2\mu$m of median size. The final production is above 99% $Mn_3$$O_4$powder and it satisfied the requirement of high purity $Mn_3$$O_4$powder for a raw material of soft ferrite.

고탄소페로망간을 중저탄소페로망간으로 제조하는 AOD공정에서 발생되는 분진은 약 90%가 $Mn_3$$O_4$이므로, 이를 이용하여 soft ferrite의 원료인 고순도 $Mn_3$$O_4$분말을 제조하기 위해서는 침출한 액의 Mn을 더욱 정제하여야 한다. 분진을 활성탄으로 배소하여 MnO로 환원시키고, 상온의 4N 염산수용액에 180g/L의 환원된 분진을 첨가하면 용액의 pH가 5이상이 되고 Fe와 Si가 침전으로 제거된 약 10%의 망간침출액이 얻어진다. Mn의 농도가 약 15000 ppm이 되도록 희석한 $70^{\circ}C$의 침출액에 F의 농도가 3000ppm이 되도록 $NH_4$F를 첨가하면 Ca가 침전하여 약14 ppm이하로 제거된다. Ca를 침전시킨 상징액에(NH$ 1.5M_4$)$_2$$CO_3$수용액을 2L/min으로 Mn의 당량만큼 첨가하면 미립의 고순도 $MnCO_3$가 침전한다. 침전을 여과하고 건조한 후에 $1000^{\circ}C$에서 2 시간 소성하면 median size가 $8.2mu$m인$ Mn_3$O$_4$를 얻을 수 있다. 제조된 산물은 99%이상의 순도로 soft ferrite용 Mn$O_3$$_4$분말의 규격을 만족한다.

Keywords

References

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