• Resources Recycling
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• v.26 no.2
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• pp.18-24
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• 2017

The $FeCl_3$ solution has been used as an etchant for etching of metal. It is necessary to reuse the etching solution because waste $FeCl_3$ etchant generated after use has provided environmental and economic problems. In this study, HCl was mixed with the $FeCl_2$ solution and then $H_2O_2$ was added into the mixed solution to oxidize the $Fe^{2+}$. During the oxidation process, oxidation-reduction potential (ORP) was measured and the relationship between ORP and oxidation ratio was investigated. As a result, this study found that the ORP was increased with increasing the concentration of HCl and $H_2O_2$, while the ORP is decreased with oxidation progress. Such a behavior was in good agreement with Nernst's equation. Also, the oxidation efficiency reached about 99% when a sufficient amount of HCl and $H_2O_2$ were added.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.17 no.2
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• pp.127-137
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• 2019

Zr electrorefining is demonstrated herein using Zirlo tubes in a chloride-fluoride mixed molten salt in the presence of $AlF_3$. Cyclic voltammetry reveals a monotonic shift in the onset of metal reduction kinetics towards positive potential and an increase in intensity of the additional peaks associated with Zr-Al alloy formation with increasing $AlF_3$ concentration. Unlike the galvanostatic deposition mode, a radial plate-type Zr growth is evident at the top surface of the salt during Zr electrorefining at a constant potential of -1.2 V. The diameter of the plate-type Zr deposit gradually increases with increasing $AlF_3$ concentration. Scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDX) and X-ray photoelectron spectroscopy (XPS) analyses for the plate-type Zr deposit show that trace amount of Al is incorporated as Zr-Al alloys with different chemical compositions between the top and bottom surface of the deposit. Addition of $AlF_3$ is effective in lowering the residual salt content in the deposit and in improving the current efficiency for Zr recovery.

• Resources Recycling
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• v.32 no.1
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• pp.21-32
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• 2023

Because the application of lithium has gradually increased for the production of lithium ion batteries (LIBs), more research studies about recycling using solvent extraction (SX) should focus on Li⁺ recovery from the waste solution obtained after the removal of the valuable metals nickel, cobalt and manganese (NCM). The raffinate obtained after the removal of NCM metal contains lithium ions and other impurities such as Na ions. In this study, we optimized a selective SX system using di-(2-ethylhexyl) phosphoric acid (D2EHPA) as the extractant and tri-n-butyl phosphate (TBP) as a modifier in kerosene for the recovery of lithium from a waste solution containing lithium and a high concentration of sodium (Li⁺ = 0.5 ~ 1 wt%, Na⁺ = 3 ~6.5 wt%). The extraction of lithium was tested in different solvent compositions and the most effective extraction occurred in the solution composed of 20% D2EHPA + 20% TBP + and 60% kerosene. In this SX system with added NaOH for saponification, more than 95% lithium was selectively extracted in four extraction steps using an organic to aqueous ratio of 5:1 and an equilibrium pH of 4 ~ 4.5. Additionally, most of the Na⁺ (92% by weight) remained in the raffinate. The extracted lithium is stripped using 8 wt% HCl to yield pure lithium chloride with negligible Na content. The lithium chloride is subsequently treated with high purity ammonium bicarbonate to afford lithium carbonate powder. Finally the lithium carbonate is washed with an adequate amount of water to remove trace amounts of sodium resulting in highly pure lithium carbonate powder (purity > 99.2%).

• Clean Technology
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• v.26 no.2
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• pp.137-144
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• 2020

Metal-impregnated activated carbons were prepared via ultrasonic-assisted impregnation method for regeneration and low ammonia concentration. Magnesium and copper were selected as metals, while chloride (Cl^-) and nitrate (NO₃^-) precursors were used to impregnate the surface of activated carbon. The physical and chemical properties of the prepared adsorbents were characterized by TGA, BET, and NH₃-TPD. The ammonia breakthrough test was carried out using a fixed bed and flowing ammonia gas (1000 mg L^-1 NH₃, balanced N₂) at 100 mL min^-1, under conditions of temperature swing adsorption (TSA) and pressure swing adsorption (PSA, 0.3, 0.5, 0.7, 0.9 Mpa). The adsorption and desorption performance of ammonia were in the order of AC-Mg(Cl) > AC-Cu(Cl) > AC-Mg(N) > AC-Cu(N) > AC through NH₃-TPD and TSA and PSA processes. AC-Mg(Cl) using MgCl₂ showed the average adsorption amount of 2.138 mmol/g at TSA process. Also, AC-Mg(Cl) showed the highest initial adsorption amount of 3.848 mmol/g at PSA 0.9 Mpa. When metal impregnated the surface of the activated carbon, it was confirmed that not only physical adsorption, but also chemical adsorption increased, making enhancement in adsorption and desorption performances possible. Also, the prepared adsorbents showed stable adsorption and desorption performances despite repeated processes, confirming their applicability in the TSA and PSA processes.

• Resources Recycling
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• v.23 no.6
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• pp.22-29
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• 2014

Recycling process of iron should be developed for efficient recovery of neodymium (Nd), rare metal, from acid-leaching solution of Nd magnet. In this study, $FeCl_3$ solution as iron source was used for preparation of iron nano particles with the condition of various factors, such as, reductant, and surfactant. $Na_4P_2O_7$ and Polyvinylpyrrolidone (PVP) as surfactants, $NaBH_4$ as reductant, and palladium chloride ($PdCl_2$) as a nucleation seed were used. Iron powder was analyzed by using XRD, SEM for measuring shape and size. Iron nano particles were prepared at the ratio of 1:5 (Fe (III) : $NaBH_4$). Size and shape of iron particles were round-form and 50 ~ 100 nm size. Zeta-potential of iron at the 100 mg/L of $Na_4P_2O_7$ was negative value, which was good for dispersion of metal particle. When $Na_4P_2O_7$ (100 mg/L), PVP($FeCl_3:PVP$ = 1 : 4, w/w) and Pd($FeCl_3:PdCl_2$ = 1 : 0.001, w/w) were used, iron nano particles which were round-shape, well-dispersed and near 100 nm-sized range. In this condition, $FeCl_3$ solution changed with spent Nd leachate solution, and then it is possible to be made round-formed iron nano particles at pH 9 and at the reaction bath over 20 L which is not include any surfactant.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.13 no.12
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• pp.6187-6195
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• 2012

Recycling process of iron should be developed for efficient recovery of neodymium(Nd), rare metal, from acid-leaching solution of neodymium magnet. In this study, $FeCl_3$ solution as iron source was used for synthesis of iron nanoparticle with the condition of various factors, etc, reductant, surfactant. $Na_4O_7P_2$ and polyvinylpyrrolidone(PVP) as surfactants, $NaBH_4$ as reductant, and palladium chloride($PdCl_2$) as a nucleation seed were used. Iron powder was analyzed with instruments of XRD, SEM and PSA for measuring shape and size. Iron nanoparticles were made at the ratio of 1 : 5(Fe (III) : $NaBH_4$) after 30 min of reduction time. Size and shape of iron particles synthesized were round-form and 50 nm ~ 100 nm size. Zeta-potential of iron at the 100 mg/L of $Na_4O_7P_2$ was negative value, which is good for dispersion of metal particle. When $Na_4O_7P_2$(100 mg/L), PVP($FeCl_3$ : PVP = 1 : 4, w/w) and Pd($FeCl_3$ : $PdCl_2$ = 1 : 0.001, w/w) were used, iron nanoparticles which are round-shape, well-dispersed, near 100 nm-sized can be made.

• Journal of Korean Society of Water and Wastewater
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• v.34 no.5
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• pp.373-383
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• 2020

The purpose of this study was to evaluate the corrosion damage of large diameter metallic pipes buried in reclaimed land due to the corrosion effect by soil, and to propose a method of installing metal pipes in the reclaimed land. The results are as follow. First, the soil of the reclaimed land was gray clay, the soil specific resistance indicating soil corrosiveness was at least 120 Ω-cm, the pH was weakly acidic(5.04 to 5.60), the redox potential was at least 62 mV, the moisture content was at most 48.8%, and chlorine ions and sulfate ions were up to 4,706.1 mg/kg and 420 mg/kg. Therefore, the overall soil corrosivity score was up to 19, and the external corrosion effect seems to be very large. Second, the condition of straight part of pipes was in good condition, but most of KP joints were affected by corrosion at a severe level. The reason for this seems to be that KP joints accelerated corrosion due to stress and crevice corrosion in addition to galvanic corrosion in the same environment. Third, as a result of evaluating correlations of each item that affects the corrosion on the external part, the lower the soil resistivity and redox potential, the greater the effect on the KP joints corrosion, and the moisture content, chloride ion, and sulfate ion, the higher the value, the greater the effect on the corrosion of KP joints. In addition, among soil corrosion items, the coefficient of determination of soil resistivity with corrosion of KP joints was the highest with 0.6439~0.7672. Fourth, when installing metal pipes or other accessories because the soil of the reclaimed land is highly corrosive, it is necessary to apply a corrosion preventive method to extend the life of pipes and prevent leakage accidents caused by corrosion damage to the joint.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.4 no.4
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• pp.335-344
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• 2006

In this paper a computer program was developed, which simulates the Li reduction process of PWR spent fuel, and the amount of a produced metal or chloride compound was calculated at the various amount of Li with the program. It establishes a database, which is composed of some characteristics related to a chemical reaction equation and thermodynamic data, and it calculates the transformed rate of PWR spent fuel oxide at the certain amount of Li by using the database as input data. As the results of the performance test of the program, it was validated that the transformed values of oxides, except for $Eu_2O_3$ and $Sm_2O_3$, were almost the same to within about a 6 % error with those calculated by the previous code and that the calculated amount of Li was also exactly consistent with the theoretical one, which is used for a complete reaction of each oxide in a single chemical reaction. A relationship between Li and the transformed metal of each oxide was analyzed on the basis of the quantities calculated with the verified development program. Of the results, when the amount of Li was given to be 250 mole, the 83.73 percentage of $UO_2$ was transformed into U while the remainder was still to be $UO_2$. In addition, it was appeared that the 297 mole of Li was needed to completely convert $UO_2$ into U.

• Korean Chemical Engineering Research
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• v.50 no.2
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• pp.217-222
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• 2012

The synthesis of dimethyl carbonate(DMC) is a promising reaction for the use of naturally abundant carbon dioxide. DMC has gained considerable interest owing to its versatile chemical reactivity and unique properties such as high oxygen content, low toxicity, and excellent biodegradability. In this study, the synthesis of DMC through the transesterification of ethylene carbonate(EC) with methanol was investigated by using ionic liquid and metal oxide catalysts. The screening test of different catalysts revealed that choline hydroxide ([Choline][OH]) and 1-n-butyl-3-methyl imidazolium hydroxide([BMIm][OH]) had better catalytic performance than metal salts catalysts such as MgO, ZnO and CaO. The effects of reaction parameters such as reaction temperature, MeOH/EC mole ratio, and carbon dioxide pressure on the reactivity of [Choline][OH] catalyst were discussed. High temperature and high MeOH/EC mole ratio were favorable for high conversion of EC. However, the yield of DMC showed a maximum when carbon dioxide pressure was 1.34 MPa, and then it decreased for higher carbon dioxide pressure. Zinc chloride($ZnCl_2$) was used as co-catalyst with the ionic liquid catalyst. The mixed catalyst showed a synergy effect on the EC conversion and DMC yield probably due to the acid-base properties of the catalysts.

• Resources Recycling
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• v.15 no.6 s.74
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• pp.33-40
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• 2006

Leaching behavior of copper using electro-generated chlorine was investigated in hydrochloric acid solutions. When leached copper concentration was lower than 3.6g/L, the utilization efficiency of the electro-generated chlorine was close to 100% at $10mA/cm^2,\;25^{\circ}C$, 400 rpm in 1M HCl solutions. The concentration ot the leached copper over 3.6g/L caused the electrode potential to drop quietly, leading to a change or leaching mechanism. The leaching rate oi copper began to decrease at the concentration of copper 5.2g/L. This is probably due to the formation of a layer of CuCl on Cu metal in 1M HCl solutions. The leaching rate, however, was not retarded in a solution ot high chloride concentration. The high solubility of CuCl in the solution may prevent the formation of CuCl on Cu metal.