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Extraction Process of Lead and Variations of Physicochemical Properties using the Smelting Experiment of Galena (방연석 제련실험을 통한 납 추출과정 및 물리화학적 거동변화 연구)

  • Han, Woo-Rim;Kim, So-Jin;Lee, Eun-Woo;Hwang, Jin-Ju;Kim, Su-Ki;Han, Min-Su
    • Journal of Conservation Science
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    • v.29 no.1
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    • pp.69-79
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    • 2013
  • This study aims at identifying the variation of physicochemical properties for galena ore in order to use it in understanding of manufacturing techniques in terms of metallurgical method and smelting or refining process for obtaining lead. The ores in the study obtained from the operating mine have been washed and pre-treated for a test. Metallic lead has been extracted by roasting process. The result displays that galena is still in present in the matt despite of exposure to high temperature, over $1000^{\circ}C$. Nearly $11.1g/cm^3$ specific gravity metallic lead has been collected from the refining test of which aim was to remove the remnant galena and a trace of concentrated silver has been identified at the grain boundary. The result suggests that at least one refining process was essential to acquire high purity metallic lead and cupellation had been executed to remove remnant silver.

Recovery of the Vanadium and Tungsten from Spent SCR Catalyst Leach Solutions by Hydrometallurgical Methods (SCR 폐촉매 침출액으로부터 습식제련법에 의한 바나듐, 텅스텐의 회수)

  • Choi, In-Hyeok;Moon, Gyeonghye;Jeon, Jong-Hyuk;Lee, Jin-Young;Jyothi, Rajesh Kumar
    • Resources Recycling
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    • v.29 no.2
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    • pp.62-68
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    • 2020
  • In new millennium, wide-reaching demands for selective catalytic reduction (SCR) catalyst have been increased gradually in new millennium. SCR catalyst can prevent the NOx emission to protect the environment. In SCR catalyst the main composition of the catalyst is typically TiO2 (70~80%), WO3 (7~10%), V2O5 (~1%) and others. When the SCR catalysts are used up and disposed to landfills, it is problematic that those should exist in the landfill site permanently due to their extremely low degradability. A new advanced technology needs to be developed primarily to protect environment and then recover the valuable metals. Hydrometallurgical techniques such as leaching and liquid-liquid extraction was designed and developed for the spent SCR catalyst processing. In a first stage, V and W selectively leached from spent SCR catalyst, then both the metals were processed by liquid-liquid extraction process. Various commercial extractants such as D2EHPA, PC 88A, TBP, Cyanex 272, Aliquat 336 were tested for selective extraction of title metals. Scrubbing and stripping studies were tested and optimized for vanadium and tungsten extraction and possible separation. 3rd phase studies were optimized by using iso-decanol reagent.

A Study on Iron-manufacture Method through Analysis of Ironware excavated from Byeokje, Goyang (고양 벽제 제철 유구 출토 철기의 분석을 통한 제철방법 연구)

  • Lim, Ju-Yeon;Kim, Soo-Ki
    • Journal of Conservation Science
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    • v.28 no.4
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    • pp.367-376
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    • 2012
  • The ironware production technology is a measure to fathom the society's level of development in time. To understand iron-manufacure methods in the past, various investigations on the fine structures and additions of ironware remains and Iron ingot have been conducted in a way of natural science. This study metallurgically reclassifies remains excavated in iron-manufacture remains located in Beokje, Goyang, which are thought to be in time of Goryeo Dynasty, and draws an inference from the element analysis on the iron-manufacture and smelting technology. Iron ingot samples with a cast iron structure are divided into those with a white cast iron structure and those with a grey cast iron rich in P. The P content of grey cast iron appeared to be the result of adding a flux agent like lime, iron ingot and carbon steel iron ingot with a cast iron structure excavated in the area is regarded as pig iron which was made without a refining process. In this study it seems that two methods of making ironware were used in the area; one is the method of making ironware by pouring cast iron to the casting, and the other is the method of making carbon steel through the refinement of pig iron. It appears that highly even steel structure of carbon steel and a small amount of MnS inclusion are very similar with that of the modern steel to which Mn is artificially added. Nevertheless, these data alone cannot be used to determine the source of Mn in the carbon steel of the excavated from the iron-manufacture remains, which raises the need for further studies on the source and the possibility of carbon steel via the iron-manufacture process of cast iron.

Material Characteristic of Slags and Iron Bloom Produced by Smelting Process Using Sand Iron (사철 제련을 통해 생산된 슬래그와 괴련철의 재료과학적 특성 비교)

  • Cho, Sung Mo;Cho, Hyun Kyung;Kwon, In Cheol;Cho, Nam Chul
    • Journal of Conservation Science
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    • v.34 no.1
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    • pp.39-50
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    • 2018
  • This study replicated traditional smelting methods to produce iron blooms from sand iron. The metallurgical properties of the slag and the iron blooms were analyzed. The sand iron materials used in the smelting experiments, which were based on ancient documents, were collected from Gyeong-Ju and Pohang. Analysis by WD-XRF and XRD showed that Gyeong-Ju's sand iron contains a high-titanium, with magnetite, and Pohang's sand iron contains a low-titanium, which magnetite and ilmenite were mixed. Analysis of the slag with XRD, and the micro-structure with metal microscopes and SEM-EDS, confirmed that the major compounds in the slag of the Gyeong-Ju's sand iron were fayalite and $w\ddot{u}stite$, and those in the slag of the Pohang's sand iron were titanomagnetite and fayalite. The differences in the main constituents were confirmed according to the Ti quantity. Finally, we observed the microstructures of the iron blooms. In the case of the iron bloom produced from Gyeong-Ju's sand iron, the outside was found to be dominantly a pearlite of eutectoid steel, while the inside was a hypo-eutectoid steel where ferrite and pearlite were mixed together. While, the major component of the iron bloom produced from Pohang's sand iron was ferrite, which is almost like pure iron. However, there were many impurities inside the iron blooms. Therefore, this experiment confirmed that making ironware required a process that involved removing internal impurities, refining, and welding. It will be an important data to identify the characteristics of iron by-products and the site through traditional iron-making experiments under various conditions.

Recovery of Cobalt from Waste Cathodic Active Material Generated in Manufacturing Lithium Ion Batteries by Hydrometallugical Process (리튬이온전지 제조공정의 폐양극활물질로부터 습식제련공정에 의한 코발트의 회수)

  • Swain Basudev;Jeong Jinki;Kim Min Seuk;Lee Jae-chun;Sohn Jeong-Soo
    • Resources Recycling
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    • v.14 no.6 s.68
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    • pp.28-36
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    • 2005
  • A hydrometallurgical process to leach cobalt from the waste cathodic active material, $LiCoO_{2}$, and subsequently to separate it by solvent extraction was developed. The optimum leaching conditions for high recovery of colbalt and lithium were obtained: 2.0 M sulfuric acid, 5 $vol.\%$ hydrogen peroxide, $75^{\circ}C$ leaching temperature, 30 minutes leaching time and an initial pulp density of 100 g/L. The respective leaching efficiencies for Co and Li were $93\%$ and $94.5\%$. About $85\%$ Co was extracted from the sulfuric acid leach liquor containing 44.72 g/L Co and 5.43 g/L Li, using 1.5 M Cyanex272 as an extractant at the initial pH 5.0 and in organic to aqueous phase ratio of 1.6:1 under the single stage extraction conditions. The Co in the raraffinate was completely extracted by 0.5 M Na-Cyanex272 at the inital pH 5.0, and an organic to aqueous phase ratio of 1;1. The cobalt sulfate solution of higher than $99.99\%$ purity could be recovered from waste $LiCoO_{2}$, using a series of hydrometallurgical processes: sulfuric acid leaching of waste $LiCoO_{2}$- solvent extraction of Co by Na-Cyanex 271 - scrubbing of Li by sodium carbonate solution - stripping of Co by sulfuric acid solution.

A Basic Study on Non-aqueous Electrolysis of Neodymium for Room-temperature Metallurgy (상온제련을 위한 네오디뮴의 비수계 전해 기초연구)

  • Park, Jesik;Lee, Churl Kyoung
    • Resources Recycling
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    • v.27 no.4
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    • pp.29-35
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    • 2018
  • In this study, the electrochemical redox behavior of neodymium in non-aqueous electrolytes was investigated to confirm the possibility of neodymium metallurgy at room temperature. The non-aqueous electrolytes include ionic liquids such as $[C_4mim]PF_6$, $[C_4mim]Cl$, and $[P_{66614}]PF_6$, ethanol which are highly soluble in neodymium salts, and mixed electrolytes based on carbonate with highly electrochemical stability. The electrochemical redox properties of neodymium were better than those of other electrolytes in the case of the mixed electrolyte based on ethylene carbonate (EC)/di-ethylene carbonate (DEC). Ethanol was added to improve the physical properties of the mixed electrolyte. Thorough the analysis about ionic conductivity of EC/DEC ratio, ethanol content and $NdCl_3$ concentration, the best electrolyte composition was 50 vol% content of ethanol and 0.5 M of $NdCl_3$. Using cyclic voltametry and linear sweep voltametry, a current peak estimated at -3.8 V (vs. Pt-QRE) was observed as a limiting current of neodymium reduction. Potentiostatic electrolysis for 18 hours at room temperature at -6 V (vs. Pt-QRE) confirmed that metallic neodymium was electrodeposited.

Scientific Analysis for Furnace Walls of the Joseon Dynasty Excavated in Southern Region of the Korean Peninsula (한반도 남부지역 출토 조선시대 노벽의 과학적 분석)

  • Jang, Won Jin;Han, Min Su
    • Journal of Conservation Science
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    • v.37 no.6
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    • pp.807-820
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    • 2021
  • A study on the Joseon Dynasty's furnace walls, excavated from south Korea, was conducted to identify the correlations and differences of the furnace walls found in Jeolla and Gyeongsang regions. Three ruins in the Jeolla region and two in the Gyeongsang region were selected for the analysis. The results showed a layer change depending on the degree of plasticity and difference in the number of layers and particle phase. Furthermore, although the temperature to be subjected to heat was divided into 1300℃ and 1100℃, it was not a phenomenon that appeared according to the region. Additionally, analysis result of major components revealed that the TiO2 content of most samples does not exceed 1wt%, This means that the furnace did not smelt iron sand or smelted it into low-titanium sand. This study indicated a slight similarity between the furnace walls found in the two regions, and the correlation was determined based on the nature of the ruins, raw materials of the metals ores, and composition of the raw materials constituting the furnace walls.

A Provenance Study of Iron Archaeological Sites in the Gyeongsang Province: Petrographic and Geochemical Approaches (경상지역 제철유적의 산지추정 연구: 암석기재학 및 지화학적 접근)

  • Jaeguk Jo;Seojin Kim;Jiseon Han;Su Kyoung Kim;Dongbok Shin;Byeongmoon Kwak;Juhyun Hong;Byeongyong Yu;Jinah Lim
    • Economic and Environmental Geology
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    • v.56 no.4
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    • pp.475-499
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    • 2023
  • To infer the provenance of raw iron materials utilized in iron production at the archaeological sites in Gyeongsang province, petrographic and geochemical analyses were conducted for smelting samples and major iron ores sourced from ore deposits. The smelting samples excavated from various iron archaeological sites were classified into different types according to their refining processes, such as iron bloom, iron bloom slag, pig iron, pig iron slag, forging iron flake, smithery iron, iron flake, and arrowhead. These samples exhibited discernable differences in their mineralogical components and texture. The enrichments of major elements such as aluminum and calcium in silicate minerals of the residual slags and the high contents of trace elements such as nickel and copper in some iron-making relics reflect the characteristics of raw iron ores, and thus can be regarded as potential indicators for inferring the provenance of source materials. In particular, the compositional ranges of Pb-Sr isotope ratios for the iron smelting samples were classified into three categories: 1) those exhibiting similar ratios to those of the raw iron ores, 2) those enriched in strontium isotope ratio, and 3) those enriched in both lead and strontium isotope ratios. The observed distinct Pb-Sr isotope characteristics in the iron smelting samples suggest the potential contribution of specific additives being introduced during the high-temperature refining process. These results provide a new perspective on the interpretation of the provenance study of the iron archaeological samples in Gyeongsang province, particularly in terms of the potential contribution of additives on the refining process.

Analysis of Heavy Metal Extracted from Road Dust under Acid Rain Condition in Ulsan (울산지역 Road Dust의 중금속 성분 용출분석)

  • 이병규;김정기
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2003.05b
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    • pp.241-242
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    • 2003
  • 울산지역은 1962년 공업 특구로 지정된 후 지난 30년 동안 우리나라의 기간 산업인 석유화학, 제련, 자동차, 조선공업 등 대단히 크고 많은 생산시설이 입주하여 운영 중에 있다. 특히 1974년부터 가동된 온산 국가공업단지에 많은 비철금속관련 업체들이 들어서면서 해양, 토양 뿐 아니라 대기중의 중금속 오염도를 가속 시켜 왔다. 최근 환경부 대기중의 중금속 측정망 분석 결과에 따르면 울산은 국내 여러 공단 도시에 비해 중금속의 오염정도가 매우 심각한 것으로 나타나고 있다. 특히, 온산공단의 대기나 토양의 카드뮴의 오염은 국내 최고치를 나타내고 있다. (중략)

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Reductive reaction of U and Lanthanides using Cd-Li metal in LiCl-KCl Molten Salt (LiCl-KCl 용융염에서 Cd-Li 금속을 이용한 U 및 란탄족의 환원반응)

  • 우문식;이병직;김응호;유재형
    • Proceedings of the Korean Radioactive Waste Society Conference
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    • 2004.06a
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    • pp.339-339
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    • 2004
  • 원자로를 이용하여 장수명핵종(long lived nucleus)을 소멸처리하는 과정에서 초우라늄(TRU, transuranium)과 희토류(RE, rare earth) 금속에 포함되어 있는 소량의 핵분열성(fissile) 물질인 우라늄을 제거할 필요가 있다. 본 실험은 LiCl-KCl 용융염계에서 전해제련법(Electrowinning)을 이용하여 용융염욕에 존재하는 우라늄을 제거하기 위하여 필요한 Cd-Li 양전극 물질을 제조하였고, 제조된 금속을 이용하여 우라늄 및 란탄족(Dy, Ce, Y, Nd, Gd) 금속의 환원 특성을 파악하였다.(중략)

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