• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2015.11a
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• pp.224-225
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• 2015

폐솔더 박리액으로부터 주석 및 구리의 분리를 위하여 옥살레이트 침전을 통해 각각 금속염으로 회수하기 위한 기초 연구를 실시하였다. 먼저 옥살산의 첨가량에 따라 주석의 침전율이 증가하였으며 당량비(옥살산/주석)의 1.0-1.5배를 첨가할 경우 주석이 99.5%, 구리는 2.0% 정도 침전되었고 철, 납 등은 거의 침전되지 않아 주석만 선택적으로 침전되는 것을 확인 하였다. 반응온도 증가에 따라 주석의 침전율은 증가하여 $60^{\circ}C$ 부근에서 최대값을 보이다가 온도가 더 증가하면 오히려 감소 경향을 보였다. 침전물의 고액분리 용이를 위해 카티온성 고분자 응집제를 이용하여 침강시킨 후, 분리된 침전물을 건조, 분쇄하여 $SnO_2$의 산화물을 얻을 수 있었다. 주석이 제거된 폐솔더 박리액에 옥살산을 첨가하여 구리가 약 91% 이상 침전되어 납, 철 등의 금속과 분리하여 선택적으로 회수가 가능하였다.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.8 no.2
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• pp.115-122
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• 2010

In this study, the removal of Cs and Tc from a simulated fission products (FP) solution which were co-dissolved with U during the oxidative-dissolution of spent fuel in a mixed carbonate solution of $(Na_2CO_3-NaHCO_3)-H_2O_2$ was investigated by using a selective precipitation method. As Cs and Tc might cause an unstable behavior due to the high decay heat emission of Cs as well as the fast migration of Tc when disposed of underground, it is one of the important issues to removal them in views of the increase of disposal safety. The precipitation of Cs and Re (as a surrogate for Tc) was examined by introducing sodium tetraphenylborate (NaTPB) and tetraphenylphosponium chloride (TPPCl), respectively. Precipitation of Cs by NaTPB and that of Re by TPPCl were completed within 5 minutes. Their precipitation rates were not influenced so much by the temperature and stirring speed even if they were increased by up to $50^{\circ}C$ and 1,000 rpm. However, the pH of the solution was found to have a great influence on the precipitation with NaTPB and TPPCl. Since Mo tends to co-precipitate with Re at a lower pH, especially, it was effective that a selective precipitation of Re by TPPCl was carried out at pH of above 9 without co-precipitation of Mo and Re. Over 99% of Cs was precipitated when the ratio of [NaTPB]/[Cs]>1 and more than 99% of Re, likewise, was precipitated when the ratio of [TPPCl]/[Re]>1.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.9 no.3
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• pp.131-139
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• 2011

This study was carried out to examine the stability of $Na_2CO_3-H_2O_2$ carbonate solution with aging time in the dissolving solution after oxidative dissolution of U by a carbonate solution, the Cs/Re filtrate after selective precipitation of Cs and Re (as a surrogate for Tc), and the acidification filtrate after precipitation of U by acidification, respectively. The compositions of dissolving solution were not changed with ageing time, and the selective precipitation of Re and Cs was also not affected without regard to the aging time of dissolving solution. The successive removal of Cs and Re from a carbonate dissolving solution was possible. However, the recovery yield of U by acidification was decreased with increasing the aging time of the dissolving solution and the Cs/Re-filtrate, respectively, because U was converted from the uranyl peroxocarbonato complex to the uranyltricarbonate in the solution aged for a long time. Accordingly, it is effective that a dissolving solution and a Cs/Re filtrate are treated within the aging of 7 days, respectively, in order to recover U more than 99%. On the other hand, the recovery of U was carried out in order of the oxidative dissolution of U selective precipitation of Re and Cs precipitation of U by acidification. Almost all of U and a part of FP were co-dissolved in oxidative dissolution step. Over 99% of Re and Cs from the FP co-dissolved with U could be removed by a TPPCl (tetraphenylphosphonium chloride) and a NaTPB (sodium tetraphenylborate), respectively. U was precipitated nearly 100% by acidification to pH 4. Therefore, it was confirmed that the validity of recovery of U by precipitation methods from a SF (spent fuel) in the $Na_2CO_3-H_2O_2$ solution.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2014.11a
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• pp.94-94
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• 2014

본 연구는 탈질용 폐 SCR 촉매로부터 유가금속인 바나듐과 텅스텐을 회수하기 위하여 고온 소다배소, 수침출, 침전 및 용매추출 실험 순으로 진행하였다. 소다배소는 $Na_2CO_3$ 첨가량 5당량, 폐촉매 평균 입자크기 $54{\mu}m$, 배소온도 $850^{\circ}C$, 배소시간 120분의 조건이 적절하였고, 소다배소 산물의 수침출 실험은 배소산물 입자크기 $-45{\mu}m$, 침출온도 $40^{\circ}C$, 침출시간 30분 및 광액밀도 10%의 조건이 적절하였다. 이와 같은 조건하에서 소다배소 및 수침출 실험을 수행한 결과, 바나듐 성분 약 46%와 텅스텐 성분 약 92%가 침출 되었다. 수침출 공정에서 얻어진 바나듐과 텅스텐이 함께 침출된 침출용액으로부터 바나듐 성분을 선택적으로 침전시키기 위하여 MgCl2를 사용하여 침전실험을 수행하였으나, 바나듐 성분이 침전될 때 텅스텐 성분이 함께 침전되어 큰 손실율을 나타내었다. 또한, 침출용액 내의 바나듐과 텅스텐 성분을 분리하기 위하여 용매추출 실험을 수행하였다. 아민계열의 추출제인 Alamine 336 및 Aliquat 336을 사용한 용매추출 실험에서 바나듐과 텅스텐 성분 모두 90% 이상 추출되었다. 이후 수행된 탈거실험에서 대부분의 역추출제에 의해 바나듐과 텅스텐은 동시에 탈거되었다. 그러나 Alamine 336을 추출제로 사용한 유기상의 탈거실험에서 NaCl 및 NH4Cl 용액을 탈거용액으로 사용하였을 경우에 바나듐과 텅스텐이 선택적으로 탈거될 수 있는 가능성을 나타내었다. 반면에 Aliquat 336을 추출제로 사용한 유기상의 탈거실험의 경우, NaOH 용액이 가장 선택적인 탈거용액임을 확인하였다.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1997.10a
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• pp.47-50
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• 1997

희토류원소의 광 환원 침전 특성이 연구되었다. 환원제로 isopropyl alcohol, 침전제로 (NH$_4$)$_2$SO$_4$가 사용되었다. 그리고 250nm의 파장을 방출하는 수은 램프가 사용되었다. Eu원소만을 함유하는 용액으로부터 Eu+3의 Eu+2로의 광 환원 결과는 97%이상이었으며 과산화수소가 소량 첨가되었을 경우 침전 속도는 증가하였다. 이 결과를 토대로 하여 희토류원소들(Sm,Eu,Gd)을 함유하는 수용액과 유기용액(HDEPH-Dodecan)에 UV광을 조사하였을 시 선택적으로 Eu을 분리해 낼 수 있었다. Eu의 침전 회수율은 두 상의 경우 모두 97%이상이었다.

• Resources Recycling
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• v.23 no.3
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• pp.37-43
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• 2014

A study has been made on the recovery of tin and copper from waste solder stripper by oxalate precipitation. With the increasing of the oxalic acid addition, tin was precipitated effectively and removed above 99.5% of tin when the oxalic acid, in an amount 1.0-1.5 times the stoichometric requirement, was added. But, in this case, only 2.0% of copper was precipitated and lead, iron were not precipitated. So, tin was selectively removed from the waste solution. With the increasing of the reaction temperature, the removal percentage of tin was increased and maximum value at arounf $60^{\circ}C$ and decreased with increase in the temperature any more. After filtering the precipitate and drying in oven, $SnO_2$ was obtained from the precipitate. After removal of tin in stripping solution, above 91% of copper was selectively removed by Cu-oxalate by addition of oxalic acid.

• Resources Recycling
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• v.30 no.2
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• pp.31-38
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• 2021

To investigate the separation of La(III) from sulfuric acid solutions containing Fe(III), rare earth double salt precipitation experiments were performed by adding sodium sulfate. In this work, the effect of sodium sulfate, Fe(III), and La(III) concentrations; reaction temperature; and time was investigated. The extent of precipitation of La(III) was proportional to the concentrations of Na+ and SO42- in the solution. As the reaction temperature increased to 100 ℃, the extent of precipitation of La(III) increased. The extent of precipitation of Fe(III) decreased with increasing reaction time. The concentration ratio of Fe(III) to La(III) did not have a significant effect on the precipitation of La(III). Our results indicate that it is possible to separate La(III) from a ferric sulfate solution through selective precipitation by adding sodium sulfate.

• Resources Recycling
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• v.30 no.6
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• pp.36-42
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• 2021

Spent lithium-ion batteries are treated by reduction-smelting at high temperatures to recover valuable metals. Solvent extraction and precipitation of the HCl leaching solution of reduction-smelted metallic alloys resulted in a filtrate containing Ni(II) and a small amount of Si(IV). Adsorption and precipitation experiments were conducted to recover pure Ni(II) compounds from the filtrate. Si(IV) was selectively loaded onto polyacrylamide, but this method did not efficiently filter the solution due to an increase in viscosity. The addition of Na₂CO₃ as a precipitant to the filtrate led to the simultaneous precipitation of Ni(II) and Si(IV). However, it was possible to recover nickel oxalate with a purity higher than 99.99% by selectively precipitating Ni(II) with the addition of Na₂C₂O₄ as a precipitant.

• Journal of the Korean Magnetics Society
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• v.16 no.3
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• pp.163-167
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• 2006

Ultrasonic irradiation in a solution during the chemical reaction may accelerate the rate of the reaction and the crystallization at low temperature. We have synthesized nanometer sized magnetite particles using coprecipitation method, sonochemical method without surfactant, and sonochemical method with surfactant, in order to investigate the effect of ultrasonic irradiation and surfactant on the coprecipitates of metal ions. The size of the magnetite nanoparticles prepared by coprecipitation method, and sonochemical method without surfactant showed broad distributions. But we got uniform nanoparticles using a sonochemical method with oleic acid. The average size of the particles can be controlled by the ratio $R=[H_2O]/[surfactant]$. The size of the magnetite nanoparticles prepared by this method showed narrow distributions. We have characterized the nanoparticles using an X-ray diffraction (XRD), a superconducting quantum interference device (SQUID), and atomic force microscope (AFM). The size and distribution of the magnetite nanoparticles were measured by dynamic light scattering (DLS) method.

• Journal of the Mineralogical Society of Korea
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• v.13 no.2
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• pp.73-83
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• 2000

다덕 광산 폐석내 섬아연석과 함망간탄산염 광물의 풍화현상과 그에 따른 중금속의 거동을 조사 하였다. 섬아연석은 풍화초기에 극미립 산화철의 망상구조 집합체로 교대되었으며, 후기에는 자연황이 용해중인 섬아연석과 산화철 집합체 사이에 침전되었다. 산화철 집합체에는 As가 다량 함유되어 있다. 능망간석와 함망간 방해석은 함아연산화망간의 망상구조 집합체로 교대되었으며, 함망간방해서과 함아연산화망간 사이에는 스미소나이트가 침전되었다. 선택적 용해외 X선회절분석을 이용하여 감정한 결과, 함아연산화망간은 헤테롤라이트/하이드로헤테롤라이트인 것으로 판명되었다. Zn의 일부는 규산과 결합하여 입간 공극에 월레마이트로 침전되었다. 풍화 초기에 형성되는 극미립 산화철 및 함아연산화망간의 치밀한 망상 집합체는 풍화용액의 순환을 차단하여, 모광물의 풍화 반응을 지체시키는 지화학적 장벽 역할을 하였다. 이에 따라 망상구조 내에 조성된 국지적 미환경하에서 풍화중간산물들이 침전되었다. 이상의 연구 결과로 다음과 같은 사항을 추론할 수 있다. 섬아연석의 Fe와 함망간탄산염의 Mn은 각각 산화철과 산화망간으로 침전되어 산성화에 기여하였다. 폐광석 더미내 As의 활동도는 저결정질 산화철에의 흡착에 의해 조절되며, Zn의 활동도는 미소환경조건에 따라 하이드로헤테롤라이트/헤테롤라이트, 스미소나이트, 월레마이트 등의 다양한 이차광물의 용해도에 의하여 조절된다.