• Membrane Journal
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• v.23 no.1
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• pp.92-99
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• 2013

In this study the nanofiltration (NF) membrane treatment of a sulfuric acid waste solutions containing copper ion ($Cu^{+2}$) discharging from the etching processes of the printed circuit board (PCB) manufacturing industry has been studied for the recycling of acid etching solution. SelRO MPS-34 4040 NF membrane from Koch company was tested to obtain the basic NF data for recycling of etching solution and separation efficiency (total rejection) of copper ion. NF experiments were carried out with a dead-end membrane filtration laboratory system. The pure water flux was increased with the increasing storage time in sulfuric acid solution and lowering pH of acid solution because of the enhancement of NF membrane damage by sulfuric acid. The permeate flux of acid solution was decreased with the increasing copper ion concentration. Total rejection of copper ion was decreased with the increasing storage time in sulfuric acid solution and copper ion concentration, and lowering the pH of acid solution. The total rejection of copper ion was decreased from initial 37% to 15% minimum value.

• Proceedings of the Korean Institute of Resources Recycling Conference
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• 2004.05a
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• pp.218-226
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• 2004

Solvent extraction and stripping experiments were conducted to separate iron from a spent $FeCl_3$ etching solution containing nickel. In the extraction, PC88A, MIBK and Alamine336 were tested as an extractant in various diluents. Alamine336 salt in toluene led to the highest extraction percentage of iron. Stripping percentage of iron from the loaded organic by Alamine336 increased with decreasing HCl conentration of stripping solution and with increasing volume ratio of aqueous to organic. In the operation of bench scale mixer-settler, 7 extraction stage with 1.0M Alamine336 salt in toluene and 10 stripping stage with 0.01M HCl solution resulted in a stripped solution with 133g/L of iron and in a raffinate with most of nickel together with a small amount of iron when the flow rate ratio of organic to aqueous was 7.

• Resources Recycling
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• v.14 no.3
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• pp.48-54
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• 2005

Solvent extraction and chemical reduction experiments have been performed to separate iron and nickel from a spent FeCl$_3$ etching solution and to recover nickel metal. It was possible to separate iron and nickel by extracting the spent solution with Alamine336. At the O/A ratio of 7:1, iron extraction percentage of 99% was obtained. In the stripping of the loaded organic with 0.01 M HCl solution, iron stripping percentage of 99% was obtained when the A/O ratio was 7:1. When the pH of the raffinate was controlled to be 10.5, nickel metal powder with 99% purity was obtained by using hydrazine as a reducing agent at 100$^{\circ}C$. A process was suggested to recover nickel metal from the spent FeCl$_3$ solution and to regenerate etching solution.

• Korean Chemical Engineering Research
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• v.52 no.2
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• pp.272-277
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• 2014

In this study the nanofiltration (NF) membrane treatment of a sulfuric acid waste solutions containing copper ion ($Cu^{+2}$) discharging from the etching processes of the printed circuit board (PCB) manufacturing industry has been studied for the recycling of acid etching solution. SelRO MPS-34 4040 NF membrane from Koch company was tested to obtain the basic NF data for recycling of etching solution and separation efficiency (total rejection) of copper ion. NF experiments were carried out with a cross-flow membrane filtration laboratory system. The permeate flux was decreased with the increasing copper ion concentration in sulfuric acid solution and lowering pH of acid solution, and its value was the range of $4.5{\sim}23L/m^2{\cdot}h$. Total rejection of copper ion was decreased with the increasing copper ion concentration, lowering pH of acid solution and decreasing cross-flow rate. The total rejection of copper ion was more than 70% at the experimental condition. The SelRO MPS-34 4040 NF membrane was represented the stable flux and rejection for 1 year operation.

• Proceedings of the IEEK Conference
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• 2001.10a
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• pp.140-143
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• 2001

A study has been made on the recovery of nitric acid and valuable metals such as Cu, Sn, Pb from the spent nitric etching solutions. The nitric acid was extracted effectively by TBP but the heavy metals such as Fe, Cu, Sn, Pb were not extracted by TBP from the spent nitric etching solutions. From the experimental results, 95% of nitric acid in spent etching solution was extracted at O:A ratio of 3:1 with five stage by 60% TBP and 98% of nitric acid was stripped from the loaded organic phase at O:A ratio of 1:1 with four stages by distilled water. After extracting nitric acid, Cu was recovered as a metal by electrowinning effectively and Sn was successfully removed by precipitation method by adjusting the pH of raffinate solution. Finally, Pb was recovered by cementation with iron scrap at $65^{\circ}C$. Parameters controlling the cementation process, such as temperature, pH and the effect of the additives were investigated.

• Resources Recycling
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• v.32 no.3
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• pp.9-17
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• 2023

Efforts are currently underway to develop a method for efficiently recovering lithium from the cathode material of waste lithium iron phosphate batteries (LFP). The successful application of lithium battery recycling can address the regional ubiquity and price volatility of lithium resources, while also mitigating the environmental impact associated with both waste battery material and lithium production processes. The isomorphic substitution leaching process was used to recover lithium from spent lithium iron phosphate batteries. Lithium was leached by the isomorphic substitution of Fe²⁺ in LFP using a relatively inexpensive ferric chloride etching solution as a leaching agent. In the study, the leaching rate of lithium was compared using the ferric chloride etching solution at various multiples of the LFP molar ratio: 0.7, 1.0, 1.3, and 1.6 times. The highest lithium leaching rate was shown at about 98% when using 1.3 times the LFP molar ratio. Subsequently, to eliminate Fe, the leachate was treated with NaOH. The Fe-free solution was then used to synthesize lithium carbonate, and the harvested powder was characterized and validated. The surface shape and crystal phase were analyzed using SEM and XRD analysis, and impurities and purity were confirmed using ICP analysis.

• Clean Technology
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• v.13 no.3
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• pp.188-194
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• 2007

In the present study, we developed a methodology to minimize a waste solution produced in the etching process. The condition for the optimization of the GRS process was studied on the basis of laboratory experiment and field test as well as pilot test. Through the study, we analyse the relation of the main process variables and the yield of the GRS process. The application of the new operation condition and the reactor internal modification results in 10% yield improvement in the GRS process and accordingly decreases a wasted solution.

• Resources Recycling
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• v.7 no.5
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• pp.46-51
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• 1998

A study has been on the recovery of nitric acid and valuable metals such as Fe, Cu, Sn, Pb, from spent nitric etching solutions. The effects of extractant of extractant type, concentrations, phase raios and selectivity from Fe, Cu, Sn, Pb on nitric acid extraction were studied. The results showed that TBP as an extractant for recovering of nitric acid was more effective than Alamine336, and the optimal concentration of TBP was found to be 60~70% of organic phase. Also, the nitric acid were only extracted by TBP from the spent etching solutions and the heavy metals such as Fe, Cu, Sn, Pb were not extracted above 0.1N nitric acid in spent etching solutions, From the analysis of McCabe-Thiele diagram, the extraction of 95% nitric acid is attained at a ratio of O/A=3 with five stages by 60% TBP and the stripping of 98% nitric acid from 80 g/l nitric acid in organic phase is attained at a ratio of O/A=1 with four stages by distilled water.

• Membrane Journal
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• v.19 no.4
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• pp.317-323
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• 2009

In this study the nanofiltration (NF) membrane treatment of a nitric acid waste solutions containing $Pb^{+2}$ heavy metal ion discharging from the etching processes of an electronics and semiconductors industry has been studied for the purpose of recycling of nitric acid etching solutions. Three kinds of NF membranes (General Electric Co. Duraslick NF-4040 membrane, Dow Co. Filmtec LP-4040 membrane and Koch Co. SelRO MPS-34 4040 membrane) were tested for their separation efficiency (total rejection) of $Pb^{+2}$ ion and membrane stability in nitric acid solution. NF experiments were carried out with a dead-end membrane filtration laboratory system. The membrane permeate flux was increased with the increasing storage time in nitric acid solution and lowering pH of acid solution because of the enhancing of NF membrane damage by nitric acid. The membrane stability in nitric acid solution was more superior in the order of Filmtec LP-4040 < Duraslick NF-4040 < SelRO MPS-34 4040 membrane. The total rejection of Pb+2 ion was decreased with the increasing storage time in nitric acid solution and lowering the pH of acid solution. The total rejection of $Pb^{+2}$ ion after 4 months NF treatment was decreased from 95% initial value to 20% in the case of Duraslick NF-4040 membrane, from 85% initial value to 65% in the case of SelRO MPS-34 4040 membrane and from 90% initial value to 10% in the case of Filmtec LP-4040 membrane. These results showed that SelRO MPS-34 4040 NF membrane was more suitable for the treatment of an acidic etching waste solutions containing heavy metal ions.

• 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.