• Resources Recycling
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• v.33 no.1
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• pp.58-68
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• 2024

Critical minerals such as nickel, cobalt and lithium, are known as materials for cathodic active materials of lithium ion batteries. The consumption of the minerals is expected to grow with increasing the demands of electric vehicles, resulting from carbon neutrality. Especially, the demand for LIB (lithium ion battery) recycling is expected to increase to meet the supply of nickel, cobalt and lithium for LIB. The recycling of EOL (end-of-life) LIB can be achieved by leaching EOL LIB using inorganic acid such as HCl, HNO₃ and H₂SO₄, which are regarded as hazardous materials. In the present study, the potential use of MSA (Methanesulfonic acid), as an alternative lixiviant replacing sulfuric acid was investigated. In addition, leaching behaviors of NCM black mass leaching with MSA was also investigated by studying various leaching factors such as chemical concentration, leaching time, pulp density (P/D) and temperatures. The leaching efficiency of nickel (Ni), cobalt (Co), lithium (Li), and manganese (Mn) from LIB was enhanced by increasing concentration of lixiviant and reductant, leaching time and temperature. The maximum leaching of the metals was above 99% at 80℃. In addition, MSA can replace sulfuric acid to recover Ni, Co, Li, Mn from NCM black mass.

• 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.

• Resources Recycling
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• v.30 no.3
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• pp.41-46
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• 2021

Methanesulfonic acid (MSA) can be considered effective in the leaching of metals because of its advantageous physical and chemical properties. The chemical reactivities of MSA and sulfuric acid were compared based on their structures and the dissolution data of Co and Ni metal. The inductive and resonance effects play a vital role in the chemical reactivities of these two acids. The dissolution percentages of Co and Ni in the sulfuric acid solution were higher than those in the MSA solution under the same experimental conditions. Considering the strong acidity of MSA and the high solubility of its metal salts, MSA can be employed as a leaching agent for the recovery of metals.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2003.09a
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• pp.532-535
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• 2003

새만금 방조제를 통하여 새만금호로 유입되는 해수 침출수량과 새만금 방조제 내부에서의 해수와 담수 사이의 상호작용 등에 대한 연구를 수행하였다. 본 연구에는, 밀도 차이에 의한 흐름을 고려한 지하수 흐름 지배 방정식과 염류의 분산 및 이송 지배 방정식을 결합시킨 수치해석 모델이 이용되었다. 밀도류를 고려한 경우에는 밀도류를 고려하지 않았을 경우보다 해수 침출량은 다르지 않았으나, 해수 침출면의 길이가 축소되고 유속이 증가하였다. 부정류상태의 해수-담수 경계면은 정류 상태의 결과와 매우 달랐으며, 해수 침출면이 방조제의 하부가 아닌 상부에 존재함을 보였다.

• Resources Recycling
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• v.10 no.6
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• pp.9-14
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• 2001

A sulfuric acid leaching of $LiCoO_2$as cathodic active materials of lithium ion secondary batteries was investigated in terms of reaction variables. In the absence of a reducing agent, the extraction of cobalt was less than 40% in 2 M sulfuric acid at $75^{\circ}C$ instead of that of lithium could be almost 100% in the same conditions. To improve the Co extraction, hydrogen peroxide was used as a reducing agent in the range 2~20 vol%. When over 10vo1% hydrogen peroxide was added, the extractions of both metals were improved to about 95%. It seems to be due to the reduction of Co(III) to Co(II) that can be readily dissolved. The extractions of Co and Li were increased with increasing $H_2$$SO_4$concentration and temperature, and amount of hydrogen peroxide and with decreasing of pulp density. The optimum leaching conditions were determined at $2 M H_2$$SO_4$concentration, $75^{\circ}C$ operating temperature, 100 g/L. initial pulp density, 20 vol% $H_2$$O_2$addition and 30 min.

• Resources Recycling
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• v.4 no.3
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• pp.2-9
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• 1995

The rccoverg and separation pracess of nikcl, vanadium and molybdenum from spent dcsulfilrizing catalyst ofpetrochemical rndustries was studied. Tnis process was canied out wet process which is consist of roasting, ammonialeaching and solve111 exDaction techniqcs. The metal ions of NI, V and Mo as vduable compollents were treated byroasting them a1 low lernperatuc, 400$^{\circ}$C in first dep, and then dlssah'ed nu1 at 80$^{\circ}$C wlth ammonium cabonate mlulion.Aftcr cooling them a1 room tempertaure, vanadium wa rccavered from mathcr iiquur in thc f n m of precipitate, sodiumvanadales The Secand slep, roasting the catalyst which is added sodium carbonate ul IOOO"C, was employed. Leachingwith distilled ~ a l e rga ve a iwo phase resultant, solutio~c~a ntaning Ni, V and Mo and solid residue containing sibca,alurmniu~n and iron. A solvcnt exlclction technique uslng vvriuus extractanls, MSP-8, TOIUC, LIX64Pi was eflecnve farthc extraclion and scparation ol thrcc mcfals from thc ammonical 11qou1 thc ammonical 11qou1.

• Resources Recycling
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• v.9 no.4
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• pp.37-43
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• 2000

Leaching of $LiCoO_2$ as a cathodic active materials for recovering Li and Co from spent lithium ion battery was investigated in terms of reaction variables. At the optimum condition determined in the previous work, Li and Co in a $H_2SO_4$ and $HNO_3$ solution were dissolved 70~80% and 40%, respectively. Li and Co were leached over 95% with the addition of a reductant such as $Na_2S_2O_3$ or $H_2O_2$. This behavior is probably due to the reduction of $Co^{3+}$ to $Co^{2+}$. Leaching of $LiCoCo_2$ powder obtained by calcination of an electrode materials from spent batteries was also carried out. Leaching efficiency of Li and Co were over 99% at the optimum condition with $H_2O_2$ addition of 1.7 vol.%. It seems to be due to the activation of $LiCoO_2$ by repeated charging and discharging or an imperfect crystal structure by deintercalation of Li.

• Resources Recycling
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• v.31 no.4
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• pp.40-48
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• 2022

In waste lithium iron phosphate (LFP) batteries, the cathode material contains approximately 4% lithium. Recycling the constituent elements of batteries is important for resource circulation and for mitigating the environmental pollution. Li contained in the waste LFP cathode powder was selectively leached using persulfate-based oxidizing agents, such as sodium persulfate, potassium persulfate, and ammonium persulfate. Leaching efficiency and waste LFP powder properties were compared and analyzed. Pulp density was used as a variable during leaching, which was performed for 3 h under each condition. The leaching efficiency was calculated using the inductively coupled plasma (ICP) analysis of the leachate. All types of persulfate-based oxidizing agents used in this study showed a Li leaching efficiency over 92%. In particular, when leaching was performed using (NH₄)₂S₂O₈, the highest Li leaching percentage of 93.3% was observed, under the conditions of 50 g/L pulp density and an oxidizing agent concentration of 1.1 molar ratio.

• Applied Chemistry for Engineering
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• v.19 no.6
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• pp.668-673
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• 2008

The objective of this study is to optimize the leaching conditions of sequential leaching and extracting processes for selective Ni recovery from spent Ni-Mo-based catalyst. The selective Ni recovery process consists of two processes of leaching and extracting process. In this 2-step process, Ni component is dissolved from solid spent Ni-Mo-based catalyst into leaching agent in leaching process and sequentially extracted to Ni complex with an extracting agent in the extracting process. The solutions of nitric acid ($HNO_3$), ammonium carbonate ($(NH_4)_2CO_3$) and sodium carbonate ($Na_2CO_3$) were used as a leaching agent in leaching process and oxalic acid was used as an extracting agent in extracting process. $HNO_3$ solution is the most efficient leaching agent among the various leaching agent. Also, the optimized leaching conditions for the efficient and selective Ni recovery were the leaching temperature of $90^{\circ}C,\;HNO_3$ concentration of 6.25 vol% and elapsed time of 3 h. As a result, Nickel oxalate having the highest yield of 88.7% and purity of 100% was obtained after sequentially leaching and extracting processes under the optimized leaching conditions.

• Resources Recycling
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• v.4 no.3
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• pp.26-31
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• 1995

The leaching characteristics of manganese nodules were investigated in dilute hydrochloric acid solution using copper malie as a reductant. Thc capper matte has been found to be an effective reductant for exhacting morc than 96% of Mn, 95% of Ni, 91% of Ca, 88% of Cu and 36% of Fe when leached in 2.5 M HCI at 70$^{\circ}$C for 2hr. The dissolutions of Mu, Co, and Ni depend on thc amaunt of added cappcr matte. 7he ratin of liquid and solid is an important [actor on the extraction of metals during leaching The dissolution af Mn, Co, Ni and Cu incrcascd w~th the increase in temperalure of leachant. The leaching rates of Mn, Co, NI and Cu from manganese nodule m the presznce of copper matte is limited by bath thc surface chemical reaction and pare diffusion processes. Thc activation energies far Mn. Co: Ni and Cu were 17. 61, 12.8, 17.2 and 57.88 KcaUmol, rcspcctively.