• Resources Recycling
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• v.28 no.6
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• pp.18-25
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• 2019

In order to recover the cerium contained in the spent nickel metal hydride batteries (NiMH battery), the recovered rare earth complex precipitates from NIMH were converted into rare earth hydroxides through ion exchange reaction to react with NaOH aqueous solution at a reaction temperature of 70 ℃, for 4 hours. Rare earth hydroxides were oxidized by injecting air at 80 ℃ for 4 hours to oxidize Ce³⁺ to Ce⁴⁺. The oxidation rate of cerium was confirmed to be about 25 % through XPS, and the oxidized powder was separated from the rest of the rare earth using the difference in solubility in dilute sulfuric acid. The finally recovered powder has a crystal phase of cerium hydroxide (Ce(OH)₄). The cerium purity of the final product was about 94.6 %, and the recovery rate was 97.3 %.

• Proceedings of the IEEK Conference
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• 2001.10a
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• pp.240-244
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• 2001

Recycling process involving mechanical, thermal, hydrometallurgical, and sol-gel step has been applied to recover cobalt and lithium from spent lithium ion batteries and to synthesize LiCoO$_2$from leach liquor as cathodic active materials. Electrode materials containing lithium and cobalt could be concentrated with 2-step thermal and mechanical treatment. Leaching behaviors of the lithium and cobalt in nitric acid media was investigated in terms of reaction variables. Hydrogen peroxide in 1 M HNO$_3$solution turned out to be an effective reducing agent by enhancing the leaching efficiency. O f many possible processes to produce LiCoO$_2$, the amorphous citrate precursor process (ACP) has been applied to synthesize powders with a large specific surface area and an exact stoichiometry. After leaching used LiCoO$_2$with nitric acid, the molar ratio of Li/Co in the leach liquor was adjusted at 1.1 by adding a fresh LiNO$_3$solution. Then, 1 M citric acid solution at a 100% stoichiometry was also added to prepare a gelatinous precursor. When the precursor was calcined at 95$0^{\circ}C$ for 24 hr, purely crystalline LiCoO$_2$was successfully obtained. The particle size and specific surface area of the resulting crystalline powders were 20 пm and 30 $\textrm{cm}^2$/g, respectively The LiCoO$_2$powder was proved to have good characteristics as cathode active materials in charge/discharge capacity and cyclic performance.

• Resources Recycling
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• v.9 no.2
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• pp.11-17
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• 2000

Consumption of nickel is continuously increasing and the wastes of secondary battery, ferrite and catalyst containing Ni are also generated periodically. Among those wastes, the aim of this research is the recovery of nickel from used Ni-Cd recharge battery. Battery consisted of Ni 24 wt%, Fe 30 wt% and Cd 18.5 wt%. Metal was recovered by solvent extraction after leaching. Cadmium was leached completely in 1N-HCl and Ni was recovered above 70%. 30 vol% MSP-8 separated Cd and Ni completely from acidic leaching solution. In addition $NH_4NO_3$ as one of ammonium salt type leachants showed an excellent leaching selectivity to Ni and Cd. Ni in leached solution was recovered completely by LIX-extractant and more than 70% of Cd in raffinate was by D2EHPA.

• Resources Recycling
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• v.17 no.1
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• pp.59-65
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• 2008

The adsorption features of nickel ion in wastewater on manganese dioxide from spent batteries were investigated for its usage as an adsorbent. The aquatic behavior of nickel ion was characterized by MINTEQ program and the considered influential variables on the adsorption of nickel ion were its initial concentration, reaction temperature, the amount of adsorbent, and pH. The adsorption ratio of nickel ion decreased with increasing its initial concentration and thermodynamic estimation has been carried out based on the adsorption characteristics of nickel ion depending on temperature. In addition, the adsorption of nickel ion was shown to be promoted according to the amount of manganese dioxide and a lot of nickel ions were adsorbed as the solution pH was raised.

• Resources Recycling
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• v.20 no.4
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• pp.65-70
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• 2011

Environmental friendly leaching process for the recovery of cobalt and lithium from the $LiCoO_2$ was investigated by organic acids as a leaching reagent. The experimental parameters, such as organic acid type, concentrations of leachant and hydrogen peroxide, reaction time and temperature as well as the pulp density were tested to obtain the most effective conditions for the leaching of cobalt and lithium. The results showed that the latic acid was the most effective leaching reagent for cobalt and lithium among the organic acids and was reached about 99.9% of leaching percentage respectively. With the increase of the concentration of citric acid, hydrogen peroxide and temperature, the leaching rate of cobalt and lithium increased. But the increase of pulp density decreased the leaching rate of cobalt and lithium.

• Resources Recycling
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• v.30 no.2
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• pp.53-60
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• 2021

Leaching experiments from single metal and metallic mixtures were conducted to develop a process for the recovery of cobalt, copper, and nickel in spent lithium ion batteries. Inorganic and organic acid solutions without oxidizing agents were employed. No copper was dissolved in the absence of an oxidizing agent in the leaching solutions. The leaching condition to completely dissolve single metal of cobalt and nickel was determined based on acid concentration, reaction temperature and time, and pulp density. The leaching condition to dissolve all of cobalt and nickel from the metallic mixtures was also obtained. Leaching of the metallic mixture with methanesulfonic acid led to selective dissolution of cobalt at low temperatures.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.28 no.5
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• pp.211-216
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• 2018

The recovery of rare earth elements (REE) including La, Nd and Ce from spent batteries is important issues to reuse scarce resources. Herein, we present a simple recovery process to obtain lanthanum oxide ($La_2O_3$) from spent Ni-MH batteries, and demonstrate the conversion mechanism from $NaLa(SO_4)_2{\cdot}H_2O$ to $La_2O_3$. This strategy requires the initial preparation of $NaLa(SO_4)_2{\cdot}H_2O$ and subsequent metathesis reaction with $Na_2CO_3$ at $70^{\circ}C$. This metathesis reaction resulted in the crystalline lanthanum carbonate hydrate ($La_2(CO_3)_3{\cdot}xH_2O$) powder with plate-like morphology. On the basis of TGA result, the $La_2(CO_3)_3{\cdot}xH_2O$ powder was calcined in air at three different temperatures, that is, $300^{\circ}C$, $500^{\circ}C$, and $1000^{\circ}C$. As the calcination temperature increased, the morphology of powder was changed; prism-like ($NaLa(SO_4)_2{\cdot}H_2O$) ${\rightarrow}$ platelike ($La_2(CO_3)_3{\cdot}xH_2O$) ${\rightarrow}$ aggregated irregular shape ($La_2O_3$). Futhermore, XRD results indicated that the crystalline $La_2O_3$ could be synthesized after the metathesis reaction with $Na_2CO_3$, followed by heat-treatment at $1000^{\circ}C$, along with a change of crystallographic structures; $NaLa(SO_4)_2{\cdot}H_2O$ ${\rightarrow}$ $La_2(CO_3)_3{\cdot}xH_2O$ ${\rightarrow}$ $La_2O_3$.

• Resources Recycling
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• v.28 no.5
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• pp.60-67
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• 2019

A valuable metal recovery from waste resources such as spent rechargeable secondary batteries is of critical issues because of a sharp increase in the amount of waste resources. In this context, it is necessary to research not only recycling waste lithium-ion batteries (LIBs), but also reusing valuable metals (e.g., Li, Co, Ni, Mn etc.) recovered from waste LIBs. In particular, the lithium hydroxide ($LiOH{\cdot}xH_2O$), which is of precursors that can be prepared by the recovery of Li in waste LIBs, can be reused as a catalyst, a carbon dioxide absorbent, and again as a precursor for cathode materials of LIB. However, most studies of recycling the waste LIBs have been focused on the preparation of lithium carbonate with a recovery of Li. Herein, we show the preparation of high purity lithium hydroxide powder along with the precipitation process, and the systematic study to find an optimum condition is also carried out. The lithium carbonate, which is recovered from waste LIBs, was used as starting materials for synthesis of lithium hydroxide. The optimum precipitation conditions for the preparation of LiOH were found as follows: based on stirring, reaction temperature $90^{\circ}C$, reaction time 3 hr, precursor ratio 1:1. To synthesize uniform and high purity lithium hydroxide, 2-step precipitation process was additionally performed, and consequently, high purity $LiOH{\cdot}xH_2O$ powder was obtained.