• Bulletin of the Korean Chemical Society
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• v.30 no.7
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• pp.1603-1606
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• 2009

A new 1D oxalato bridged compound Ni(en)(ox)-2$H_2$O, (ox = oxalate; en = ethylenediamine) has been hydrothermally synthesized and characterized by single crystal X-ray diffraction, IR spectrum, TG analysis, and magnetic measurements. In the structure the Ni atoms are coordinated with four oxygen atoms in two oxalate ions and two nitrogen atoms in one ethylenediamine molecule. The oxalate anion acts as a bis-bidentate ligand bridging Ni atoms in cis-configuration. This completes the infinite zigzag neutral chain, [Ni(en)(ox)]. The interchain space is filled by water molecules that link the chains through a network of hydrogen bonds. Thermal variance of the magnetic susceptibility shows a broad maximum around 50 K characteristic of one-dimensional antiferromagnetic coupling. The theoretical fit of the data for T > 20 K led to the nearest neighbor spin interaction J = -43 K and g = 2.25. The rapid decrease in susceptibility below 20 K indicate this compound to be a likely Haldane gap candidate material with S = 1.

• Journal of Powder Materials
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• v.30 no.6
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• pp.502-508
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• 2023

With the increasing demand for electronic products, the amount of multilayer ceramic capacitor (MLCC) waste has also increased. Recycling technology has recently gained attention because it can simultaneously address raw material supply and waste disposal issues. However, research on recovering valuable metals from MLCCs and converting the recovered metals into high-value-added materials remains insufficient. Herein, we describe an electrospinning (E-spinning) process to recover nickel from MLCCs and modulate the morphology of the recovered nickel oxide particles. The nickel oxalate powder was recovered using organic acid leaching and precipitation. Nickel oxide nanoparticles were prepared via heat treatment and ultrasonic milling. A mixture of nickel oxide particles and polyvinylpyrrolidone (PVP) was used as the E-spinning solution. A PVP/NiO nanowire composite was fabricated via E-spinning, and a nickel oxide nanowire with a network structure was manufactured through calcination. The nanowire diameters and morphologies are discussed based on the nickel oxide content in the E-spinning solution.

• Journal of Surface Science and Engineering
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• v.3 no.1
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• pp.7-12
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• 1970

Only mannitol or glycerine is generally used for the determination of boric acid in a nickel plating solution in order to make its acidic property so strong that it can be titrated with NaOH. However, these solutions give very amgiguous color change of indicator due to the precipitation of nickel salts . Therefore, only experienced dchemistsorwell trained workimen can accurately confirm the actual end point of the titratiion. For eliminating such interference of nickel salts and easily confirming the end point by any persons , the author attempted to find out a solution which produces no precipitates during the titration in these experiments, and also he tried to funish the reason for ambiguousness in titration. The following results were obtained after many experiments. (1) In any titrations which produce nickel salts such nI(oh)$_2$, the salt is formed umption very approximate to the end point, which shows some error by the consumption of titrant(NaOH) . Then, the pink color of phenolphthalein is absorbed by Ni(OH)$_2$ and the pH jumping at the end pint is also diminished to as little as less than 15% of the total phenophthalein ph range. (2) Known methods by complex salts of citrate,w hich do not produce precipitates of Ni(OH)$_2$, are also not very satisfactory, because, the pH jumping at the end point is only about 35% and the color change of phenolphthalein is form blue-green to purple-blue. (3) New method by complex salts of oxalate were attempted in these experiments. They also did not produce precipitates of Ni(OH)$_2$ and were very satisfactory in color change at the end of point was about 65% and the color change was from blue-green to purpled. In this methods, analytica cost was minimized by the use of less amounts of cheaper chemicals than the conventional citrates complex methods. The mixture of chemicals used was composed methods. The mixture of chemical used was composed of 37g/ι of sodium oxalate(Na$_2$C$_2$O$_4$$.$5H$_2$O), 2g/ι of phenolphthalein, and 400ml /ι of glycerin. The accuracy of analysis was within the error of 0.5%. (4) The procedure of analysis was as follows. One ml of nickel plating solution was taken out and to it were added 20ml of water and 20 ml of the above mixture for the indicator. The solution was titrated with 0.1N NaOH. The quantity of boric acid was calculated by the following equation. Boric acid (g/ι) = 6.184${\times}$F${\times}$ml .

• Journal of Surface Science and Engineering
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• v.4 no.1
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• pp.5-15
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• 1971

"Rapid Determination of Boric Acid in Nickel Plating Solution" by the addition of Na$_2$C$_2$O$_4$ and thus preventing the precipitation of i(OH)$_2$ during titiration , has previously been reported. In this paper, the exact amount of glycerine and the complexing possibility of oxalate with nickel has been determined by measn of conductivity titrations. This experimental work has been supported by the mathematical application of the Debye-Huckel and mass action equitions as well as statistical analysis. The results were ; (1) Fro determining boric acid in nickel plating solution, 20 ml of 400ml/ι glycerine was sufficient, since 97% of the H$_3$BO$_3$ was dissoicated by this addition. (2) In the absence of Na$_2$C$_2$O$_4$ the continious precipitation of Ni(OH)$_2$ during titration with NaOH even past end -point for boric acid determination resulted in considerable anlaytical error. (3) In the presence of Na$_2$C$_2$O$_4$ during titration , Ni++ combined with C$_2$O$_4$-to form NiC$_2$O$_4$. The solution with this precititate of very fine, colloidal , trantsparent particles, remained quite clear for approximately 2 hours. Therefore it was shown that the presence of Na$_2$C$_2$O$_4$ prevents the formation of gross Ni(OH)$_2$ precititation by forming NiC$_2$O$_4$ instead of a complex salt with Ni++ , which did not interfere with the visible determination of the end point for boric acid with NaOH titation. This observous may be interpreted in the light of the previously published solubility ratio for NiC$_2$O$_4$ and Ni(OH)$_2$, 0.3mg/100g H$_2$O(25$^{\circ}C$), respectively. Precipitation of the less soluble , albeit transparent salt, NiC$_2$O$_4$ precluded therefore the precipitation of the Ni(OH)$_2$ salt.

• Applied Chemistry for Engineering
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• v.19 no.6
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• pp.668-673
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• 2008

The objective of this study is to optimize the leaching conditions of sequential leaching and extracting processes for selective Ni recovery from spent Ni-Mo-based catalyst. The selective Ni recovery process consists of two processes of leaching and extracting process. In this 2-step process, Ni component is dissolved from solid spent Ni-Mo-based catalyst into leaching agent in leaching process and sequentially extracted to Ni complex with an extracting agent in the extracting process. The solutions of nitric acid ($HNO_3$), ammonium carbonate ($(NH_4)_2CO_3$) and sodium carbonate ($Na_2CO_3$) were used as a leaching agent in leaching process and oxalic acid was used as an extracting agent in extracting process. $HNO_3$ solution is the most efficient leaching agent among the various leaching agent. Also, the optimized leaching conditions for the efficient and selective Ni recovery were the leaching temperature of $90^{\circ}C,\;HNO_3$ concentration of 6.25 vol% and elapsed time of 3 h. As a result, Nickel oxalate having the highest yield of 88.7% and purity of 100% was obtained after sequentially leaching and extracting processes under the optimized leaching conditions.

• Resources Recycling
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• v.30 no.6
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• pp.36-42
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• 2021

Spent lithium-ion batteries are treated by reduction-smelting at high temperatures to recover valuable metals. Solvent extraction and precipitation of the HCl leaching solution of reduction-smelted metallic alloys resulted in a filtrate containing Ni(II) and a small amount of Si(IV). Adsorption and precipitation experiments were conducted to recover pure Ni(II) compounds from the filtrate. Si(IV) was selectively loaded onto polyacrylamide, but this method did not efficiently filter the solution due to an increase in viscosity. The addition of Na₂CO₃ as a precipitant to the filtrate led to the simultaneous precipitation of Ni(II) and Si(IV). However, it was possible to recover nickel oxalate with a purity higher than 99.99% by selectively precipitating Ni(II) with the addition of Na₂C₂O₄ as a precipitant.