• 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.

• Applied Chemistry for Engineering
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• v.24 no.1
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• pp.67-71
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• 2013

$FeCl_3$ has been used as an etchant for metal etching such as Fe, Cu, and Al. In the process of metal etching, $Fe^{3+}$ is reducted to $Fe^{2+}$ and the etching rate becomes slow and etching efficiency decreased. Waste $FeCl_3$ etchant needs to be regenerated because of its toxicity and treatment cost. In this work, HCl was initially mixed with the waste $FeCl_3$ and then, strong oxidants, such as $O_2$ and $H_2O_2$, were added into the mixed solution to regenerate the waste etchant. During successive etching and regeneration processes, oxygen-reduction potential (ORP) was continuously measured and the relationship between ORP and etching capability was investigated. Regenerated etchant using a two vol% HCl of the total etchant volume and a very small amount of $H_2O_2$ was very effective in recovering etching capability. During the etching-regeneration process, the same oxygen-reduction potential variation cannot be repeated every cycle since concentrations of $Fe^{2+}$ and $Fe^{3+}$ ions were continuously changed. It suggested that the control of etching-regeneration process based on the etching time becomes more efficient than that of the process based on oxygen reduction potential changes.

• 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.

• 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.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.

• Plant Journal
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• v.5 no.2
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• pp.6-13
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• 2009

• Resources Recycling
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• v.31 no.4
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• pp.34-39
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• 2022

In this study, effects of ultrasonic energy on the cementation reaction and copper recovery rate were investigated for different types of iron samples, such as plate, chip, and powder, for recovering copper from waste etchant, which contained ~3.5% copper. The cementation reaction using the ultrasonic energy was more effective than the simple stirring reaction, with the former exhibiting a high copper recovery rate than the latter for the same time interval. When cementation was performed for 25 min with ultrasonic treatment, rather than simple stirring, the copper recovery rate of the plate, chip, and powder improved from 7.0% to 12.0%, 14.0% to 46.1%, and 41.9% to 77.2%, respectively. Therefore, the use of ultrasonic energy could detach the copper recovered by the cementation reaction from the surface of the iron samples, thereby increasing the copper recovery rate. Owing to the use of ultrasonic energy, the copper recovery rate increased by 2-6 times, and the recovered copper exhibited a decreased particle size compared to that obtained via simple stirring.

• Resources Recycling
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• v.16 no.1 s.75
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• pp.59-67
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• 2007

Recovery of acids from the waste etching solution of containing acetic, nitric and hydrofluoric acid discharged from silicon wafer manufacturing process has been attempted by using solvent extraction method. EHA(2-Ethylhexlalcohol) for acetic acid and TBP(Tri-butly Phosphate) for nitric and hydrofluoric acid as a extraction agent was used to the experiment to obtain the process design data in separation procedure. From the experimental data and McCabe-Thiele diagram analysis, we obtained the optimum conditions of phase ratio(O/A) and stages to separate each acid sequently from the mixed acids. The recovery yield was obtained above 90% for acetic acid from the acid mixtures, 90% for nitric acid from acetic acid extraction raffinate and then above 67% for hydrofluoric acid from final extraction raffinate.

• Clean Technology
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• v.27 no.3
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• pp.240-246
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• 2021

The waste etching solution for chip on film (COF) contained about 3.5% copper, and it was recovered through cementation using iron samples. The effect of cementation with plate, chip, and powder iron samples was investigated. The molar ratio (m/r) of iron to copper was used as a variable in order to increase the recovery rate of copper. As the molar ratio increased, the copper content in the solution rapidly decreased at the beginning of the cementation reaction. Before and after the reaction, the copper content of the solution was determined by Inductively Coupled Plasma (ICP) using copper concentration according to time. After cementation at room temperature for 1 hour, the recovery rate of copper had increased the most in the iron powder sample, having the largest specific surface area of the samples, followed by the chip and plate samples. The recovered copper powder was characterized for its crystalline phase, morphology, and elemental composition by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Energy-dispersive X-ray spectroscopy (EDS), respectively. Copper and unreacted iron were present together in the iron powder samples. The optimum condition for recovering copper was obtained using iron chips with a molar ratio of iron to copper of 4 giving a recovery rate of about 98.4%.