• 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 IEEK Conference
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• 2001.10a
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• pp.259-263
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• 2001

There are several steps such as slicing, lapping, chemical etching and mechanical polishing in the silicon wafer production process. The chemical etching step is necessary to remove damaged layer caused In the slicing and lapping steps. The typical etching liquor is the acid mixture comprising nitric acid, acetic acid and hydrofluoric acid. At present, the waste acid is treated by a neutralization method with a high alkali cost and balky solid residue. A solvent extraction method is applicable to separate and recover each acid. Acetic acid is first separated from the waste liquor using 2-ethlyhexyl alcohols as an extractant. Then, nitric acid is recovered using TBP(Tri-butyl phosphate) as an extractant. Finally hydrofluoric acid is separated with the TBP solvent extraction. The expected recovered acids in this process are 2㏖/l acetic acid, 6㏖/1 nitric acid and 6㏖/l hydrofluoric acid. The yields of this process are almost 100% for acetic acid and nitric acid. On the other hand, it is important to recover and reuse the metal values contained in various industrial wastes in a viewpoint of environmental preservation. Most of industrial products are made through the processes to separate impurities in raw materials, solid and liquid wastes being necessarily discharged as industrial wastes. Chemical methods such as solvent extraction, ion exchange and membrane, and physical methods such as heavy media separation, magnetic separation and electrostatic separation are considered as the methods for separation and recovery of the metal values from the wastes. Some examples of the application of solvent extraction to the treatment of wastes such as Ni-Co alloy scrap, Sm-Co alloy scrap, fly ash and flue dust, and liquid wastes such as plating solution, the rinse solution, etching solution and pickling solution are introduced.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.27 no.6
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• pp.303-308
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• 2017

The $FeCl_3$ waste solution used to etch various metals contains valuable metal such as nickel. In this study, we recovered as high purity nickel carbonate crystalline powders from nickel-containing etching waste solution after regeneration of iron chloride. Firstly we eliminated about of the iron impurities under the condition of pH 4 using 5 % NaOH aqueous solution and then removed the remaining impurities such as Ca, Mn and Zn etc. by using solvent extractant D2EHPA (Di-(2-ethylhexyl) phosphoric acid). Thereafter, nickel carbonate powder having a purity of 99.9 % or more was obtained through reaction with sodium carbonate in a nickel chloride 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.

• 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.

• Applied Chemistry for Engineering
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• v.7 no.4
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• pp.614-622
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• 1996

Efficient removal of nickel from the ferric chloride etching solution has been studied. At first, $Fe^{3+}$ was reduced to $Fe^{2+}$ by the electrolytic iron flake or the waste shadow mask iron plate. And then, $Ni^{2+}$ was removed from the solution by electrolytic iron powder. Under the optimum conditions the reduced rates of nickel were 99 % and 98%, respectively at the initial $Ni^{2+}$ concentrations of 1.0% and 0.1%. Sludge formed during reduction of $Fe^{3+}$ in the solution were analyzed by XRD and SEM.

• 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.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.22 no.6
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• pp.286-290
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• 2012

Boehmite (AlOOH) powder was synthesized using waste aluminium etching solution. In waste solution, precipitated phase was gibbsite ($Al(OH)_3$), and boehmite (AlOOH) phase was obtained at pH of 7 and 8 controlled by addition of acid. Boehmite powder was obtained by washing process to remove the Na ion in precipitated solution. Mean particle size of obtained powder was 40 nm. Boehmite phase transformed to ${\alpha}-Al_2O_3$ phase via ${\gamma}-Al_2O_3$, ${\delta}-Al_2O_3$, and ${\Theta}-Al_2O_3$.

• Clean Technology
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• v.25 no.1
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• pp.14-18
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• 2019

In general after the etching process, waste etching solution contains metals. (ex. Nickel (Ni), Chromium (Cr), Zinc (Zn), etc.) In this work, we proposed a recycling process for waste etching solution and refining from waste liquid contained nickel to make nickel metal nano powder. At first, the neutralization agent was experimentally selected through the hydrolysis of impurities such as iron by adjusting the pH. We selected sodium hydroxide solution as a neutralizing agent, and removed impurities such as iron by pH = 4. And then, metal ions (ex. Manganese (Mn) and Zinc (Zn), etc.) remain as impurities were refined by D2EHPA (Di-(2-ethylhexyl) phosphoric acid). The nickel powders were synthesized by liquid phase reduction method with hydrazine ($N_2H_4$) and sodium hydroxide (NaOH). The resulting nickel chloride solution and nickel metal powder has high purity ( > 99%). The purity of nickel chloride solution and nickel nano powders were measured by EDTA (ethylenediaminetetraacetic) titration method with ICP-OES (inductively coupled plasma optical emission spectrometer). FE-SEM (field emission scanning electron microscopy) was used to investigate the morphology, particle size and crystal structure of the nickel metal nano powder. The structural properties of the nickel nano powder were characterized by XRD (X-ray diffraction) and TEM (transmission electron microscopy).

• 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.