• 한국분말재료학회지
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• 제28권6호
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• pp.497-501
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• 2021

Cobalt (Co) is mainly used to prepare cathode materials for lithium-ion batteries (LIBs) and binder metals for WC-Co hard metals. Developing an effective method for recovering Co from WC-Co waste sludge is of immense significance. In this study, Co is extracted from waste cemented carbide soft scrap via mechanochemical milling. The leaching ratio of Co reaches approximately 93%, and the leached solution, from which impurities except nickel are removed by pH titration, exhibits a purity of approximately 97%. The titrated aqueous Co salts are precipitated using oxalic acid and hydroxide precipitation, and the effects of the precipitating agent (oxalic acid and hydroxide) on the cobalt microstructure are investigated. It is confirmed that the type of Co compound and the crystal growth direction change according to the precipitation method, both of which affect the microstructure of the cobalt powders. This novel mechanochemical process is of significant importance for the recovery of Co from waste WC-Co hard metal. The recycled Co can be applied as a cemented carbide binder or a cathode material for lithium secondary batteries.

• 한국환경과학회지
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• 제9권1호
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• pp.43-47
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• 2000

A study on the remediation of heavily for ion contaminated soils from abandoned iron mine was carried out, using ex-situ extraction process. Also, oxalic acid as a complex agent was evaluated as a function of concentration, reaction time and mixing ratio of washing agent in order to evaluate Fe removability of the soil contaminated from the abandoned iron mine. Oxalic acid showed a better extraction performance than 0.1N-HCl, i.e., the concentrations of Fe ion extracted from the abandoned mine for the former at uncontrolled pH and the latter were 1,750 ppm and 1,079 ppm, respectively. The optimum washing condition of oxalic acid was in the ratio of 1:5 and 1:10 between soil and acid solution during l hr reaction. The total concentrations of Fe ion by oxalic acid and EDTA at three repeated extraction, were 4,554 ppm and 864 ppm, respectively. The recovery of Fe ions from washing solution was achieved, forming hydroxide precipitation and metal sulfide under excess of calcium hydroxide and sodium sulfide. In addition, the amounted of sodium sulfide and calcium hydroxide for the optimal revovery of Fe were 15g/$\ell$ and 5g/$\ell$ from the oxalic acid complexes, respectively.

• 한국환경과학회지
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• 제10권4호
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• pp.299-304
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• 2001

For the remediation of the contaminated soil with heavy metals, Cd, Cr, Cu, and Pb, the reaction parameters were optimized. Tartaric acid (TA) and oxalic acid(OA) as a washing agent and recovery of metals, The optimum washing conditions of TA and OA were in the ratio of 1 : 20 between soil and acid solution during 2hr reaction under unbuffered pH solutions. At the optimized reaction conditions, the removal efficiencies were compared with that of 0.1 M HCl and ethylenediamine tetraacetic acid(EDTA). TA showed higher efficiency on the removal of Pb than that of EDTA, which established for the remediation of contaminated soil with Pb and Cd metals. The recovery of metal ions from washing solution was achieved by adding calcium hydroxide and sodium sulfide by forming the precipitation of metal hydroxide and metal slfied. Optimum amounts of sodium sulgide and calcium hydroxide were Cd = 25g/$\ell$, Cu = 5~10g/$\ell$ and Pb = 5~10g/$\ell$ for the washing solution of OA and 2~5g/$\ell$ for the washing solution of TA, respectively. The amounts of $Na_2S$ and $CA(OH)_2$ for the tartaric acid was less than that of oxalic acid.

• 분석과학
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• 제12권4호
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• pp.290-298
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• 1999

임피던스 위상각 적정법을 산화환원적정, 산염기적정, 착화적정 그리고 침전적정에 적용하여 정확한 종말점 검출법을 연구하였다. 일정한 교류전류가 두 백금전극사이를 통과하도록 하였고 그중 하나는 $0.1cm^2$ 또는 $0.026cm^2$의 표면적을 가진 초소형 분극전극이었고 다른 하나는 $1cm^2$의 표면적을 비분극전극을 사용하였다. 과망간산칼륨에 의한 옥살산의 산화환원적정에서 임피던스 위상각 적정법을 적용하였을때 $50{\mu}A$, 0.0005 M 이상의 농도에서 뚜렷한 종말점을 얻었고, 50 Hz 근방의 주파수 영역에서 가장 확실한 종말점을 얻을 수 있었다. NaOH에 의한 인산의 산염기 적정에서 0.001 M 수산화나트륨에 의한 0.001 M 인산의 적정시 임피던스 위상각 적정법을 적용하여 $50{\mu}A$, 주파수 25-97 Hz의 넓은 주파수 영역에서 뚜렷한 제1당량점을 얻었다. 이는 전도도의 반대 개념으로서의 임피던스의 변화량이 종말점을 기점으로 변곡하고 이에따라 위상각이 변화하는데 원인됨을 알았다. 또한 제2당량점에서는 임피던스 위상각 적정법으로 뚜렷한 종말점을 얻지 못하였다. 이는 $Na_2HPO_4$의 가수분해를 막기 위하여 적정시 과량으로 첨가되는 NaCl에 의한 방해로 생각된다. 0.1 M EDTA에 의한 0.01 M 황산구리의 착화적정시에는 위상각 측정으로 적정종말점을 찾기 보다는 "다른위상" 임피던스 Z"을 측정하여 종말점을 알아내는 것이 유리함을 알았다. $AgNO_3$에 의한 $Cl^-$의 침전적정에 있어 $100{\mu}A$, 0.1 M 농도에서 임피던스 위상각 적정법을 적용하여 명확한 종말점을 얻었고, 15-30Hz 범위에서 가장 안정적인 뚜렷한 변화를 볼 수 있었다. 그러나 0.01 M 농도에서는 임피던스 위상각의 뚜렷한 변화를 볼 수 없었다. 본 연구에서 임피던스 위상각 적정법을 산화환원적정, 산염기적정, 착화적정 그리고 침전적정시의 종말점 검출을 위해 사용하였을 때 대부분 성공적이었으며 이는 적정시 종말점을 정확히 측정하는 목적에 활용 할수 있음을 보여주는 것이다.