Fe-Ni 合金 스크랩의 黃酸 浸出液으로부터 Ni와 Fe의 分離
Separation of Ni and Fe from H2SO4 leaching solution of scrapped Fe-Ni alloy
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주요 성분으로서 철(Fe²+/Fe³+=1.03); 47g/L, 니켈; 23.5g/L, 0.90M H₂SO₄의 조성을 갖는 철-니켈 합금 스크랩의 황산 침출액으로부터 시멘테이션법과 용매추출법으로 니켈과 철 이온을 분리하는 연구를 수행하였다. 침출액으로부터 니켈 이온의 시멘테이션을 위하여 철 분말이 환원제로 사용되었다. 60~80˚C에서 4.0 당량의 철 분말을 투입하였을 때 니켈 이온의 환원율은 17~20%에 불과하였으며, 이것은 니켈 이온의 환원석출이 Fe³+의 환원반응과 황산의 중화반응이 완료된 후에 시작되었기 때문이다. 이로부터 주성분으로 Fe³+를 함유하고 있는 침출액으로부터 니켈 이온의 분리회수에 있어서 시멘테이션은 비효율적임이 확인되었다. D2EHPA를 추출제로 사용하는 철 이온의 용매추출을 위하여 Fe²+는 Fe³+로 전환시켰다. 1.2 당량의 35% H₂O₂를 첨가함으로서 침출액에 존재하는 모든 Fe²+는 Fe³+로 산화되었다. 20 vol.% D2EHPA를 사용하여 cross-current 방식으로 침출액(23.5 g/L Fe³+)으로부터 Fe³+의 용매추출을 행하였을 때, 4단 추출에서 99.6%의 Fe³+를 추출하여 제거할 수 있었으며 순도가 98.5%인 황산니켈 용액이 얻어졌다.
Abstract
Cementation and solvent extraction processes were studied to separate nickel and iron ions from the H2SO4 leaching solution with 47g/L Fe(Fe²+/Fe³+=1.03), 23.5g/L Ni and 0.90 M H₂SO₄ which leached from Fe-Ni alloy. Iron powder was used as a reducing agent for the cementation of Ni ion from the leaching solution. The reduction percentage of Ni ion was 17~20% by adding 4 times stoichiometric amount of iron powder at 60~80 . This may result from the fact that the cementation of Ni ion occurred after the reduction of Fe²+ to Fe²+ and the neutralization of H₂SO₄ with iron powder. The cementation process was proved to be unfeasible for the separation/recovery of Ni ion from the leaching solution including Fe³+ as a major component. Fe²+ present in the leaching solution was converted to Fe³+ for solvent extraction of Fe ion using D2EHPA in kerosene as a extractant. The oxidation of Fe2+ to Fe³+ was completed by the addition of 1.2 times stoichiometric amount of 35% H2O2. 99.6% Fe³+ was extracted from the leaching solution (23.5g/L Fe³+) by 4 stages cross-current extraction using 20 vol.% D2EHPA in kerosene. NiSO4 solution with 98.5% purity was recovered from the H₂SO₄ leaching solution of scrapped Fe-Ni alloy.
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