• Bulletin of the Korean Chemical Society
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• 제27권11호
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• pp.1839-1843
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• 2006

Hydrothermal reactions of $Ln(NO_3)_3{\cdot}5H_2O $ (Ln = Eu (1), Sm (2), Ho (3), Dy (4)) with 3,5-pyridinedicarboxylic acid (3,5-pdcH2) in the presence of 4,4'-bipyridine led to the formation of the 3-D Ln(III)-coordination polymers with a formula unit of $[Ln_2(3,5-pdc)_2(C_2O_4)(H_2O)_4]{\cdot}2H_2O$. These polymers contain a bridging oxalate ligand ($C_2O_4\;^2$). On the basis of GCMS study of the mother liquor remaining after the reaction, we proposed that the $C_2O_4\;^2$ formation proceeds in three steps: (1) Ln(III)-mediated decarboxylation of $3,5-pdcH_2$ to give $CO_2$, (2) the reduction of $CO_2$ to $CO_2\;^{\cdot}$ by the Ln(II) species, and (3) the reductive coupling of the two $CO_2\;^{\cdot}$ radicals to the oxalate ($C_2O_4\;^2$) ion. All polymers were structurally characterized by X-ray diffraction.

• 자원리싸이클링
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• 제18권4호
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• pp.38-43
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• 2009

수산화알루미늄을 원료물질로 하여 알루미늄 유기화합물인 aluminum oxalate 합성실험을 수행하였다. 이를 위해 국산 99.7% 순도의 수산화알루미늄을 옥살산으로 용해하는 방법으로 알루미늄 수용액을 제조하였으며, 실험결과 옥살산 농도 1.0 mole/l, 반응온도 $90^{\circ}C$에서 16시간 용해시 거의 100%에 가까운 용해율을 얻을 수 있었다. 알루미늄 수용액으로부터 aluminum oxalate를 합성하기 위해서는 ethanol/Al solution 혼합비율을 2.0이상으로 유지하여야 하는 것으로 나타났다. 또한, 90% 이상의 회수율을 얻기 위해서는 혼합액의 pH를 8.2이상으로 조절하여야 하는 것으로 나타났다. 합성반응을 통해 얻은 aluminum oxalate의 화학분석결과 $NH_4$ 14.5%, Al 7.18% 및 C 17.4%이었으며, 이의 화학식은 $(NH_4)_3Al(C_2O_4)_3$ $3H_2O$임을 확인할 수 있었다.

• 대한화학회지
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• 제9권2호
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• pp.71-74
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• 1965

Reduction of Ti(Ⅳ)-oxalate complex on dropping mercury electrode has been studied as a function of oxalate concentration and of pH varied with HCl. Assuming there are equilibrium $TiO(C_2O_4)_2= \;+\;2H^+\;=\;Ti^{+4}\;+\;2C_2O_4\;=\;+\;H_2O,\;K_4$ in addition to $TiO(C_2O_4)_2\;^=\;=\;TiO^{++}\;+\;2C_2O_4=\;K_2\;Ti(C_2O_4)_2\;^-\;=\;Ti^{+3}\;+\;2C_2O_4=\;K_3$ in the system cathodic wave has been well explained for that pH is higher than 0.5. The equilibrium constants $K_2,\;K_3$ and $K_4$ have been to be $2{\times}10^{-12},\;5{\times}10^{-13}$ and $10^{-11}$, respectively. The reduction of Ti(Ⅳ)-oxalate system is $Ti^{+4}\;+\;e\;{\to}\;Ti^{+3}$ in the concentration of hydrochloric acid, higher than 3M.

• 청정기술
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• 제29권1호
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• pp.46-52
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• 2023

옥살산(oxalic acid)은 기존에 질산을 사용한 carbohydrates의 산화 공정에 의해 얻어질 수 있으며 여러 분야에서 사용되고 있다. 하지만 이 반응은 다양한 질소 산화물을 형성하고 많은 증간 생산물의 분리를 필요로 하기에 복잡하고 환경에 유해하다. 한편, 이산화탄소로부터 전기화학적 방법에 의해 옥살산을 높은 효율로 얻을 수 있는 방법이 제안되었다. 아연 전극 산화에 의해 생성된 Zn²⁺이온과 CO₂ 환원에 의한 oxalate이온의 반응으로 zinc oxalate(ZnC₂O₄)가 얻어진다. 이후 산처리에 의해 옥살산이 생성될 수 있으나 강산과 열을 필요로 한다. 본 연구에서는 CO₂의 전기화학적 전환으로 형성된 ZnC₂O₄을 강산을 사용하지 않고, 간단하고 분리가 쉬운 방법을 적용하여 옥살산으로 전환하고자 한다. 또한, 고부가 물질인 글리콜산으로 더 전환시킴으로써 이산화탄소에서 고부가 물질로의 전환 가치를 높이고자 하였다. ZnC₂O₄를 상온, 상압에서 화학적 방법 및 여과 과정을 통해 효과적으로 Zn(OH)₂ 입자와 oxalate 용액으로 분리하였으며 얻어진 Zn(OH)₂와 oxalate는 전기화학적 방법을 사용하여 각각 Zn, 글리콜산으로 전환되었다.

• 한국세라믹학회지
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• 제32권4호
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• pp.455-461
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• 1995

To investigate the synthesis of $\beta$-Al2O3 and its crystallization behavior by oxalate coprecipitation method, the optimum pH range for oxalate coprecipitates has been theoretically calculated from the solubility products and the equilibrium constans of each metal ionic species and their solubility diagram wa obtained. The optimum pH range for oxalate coprecipitates at room temperature was estimated as <4. In experiment, we found that the optimum condition for oxalate coprecipitates was pH<1, which was not doped with pH controller. The Na+ ions were easily exchanged for the NH4+ ions of NH4OH which was used as pH controller, and those NH4+ ions were supposed to affect the crystallization behavior of $\beta$-Al2O3. The thermal decomposition of all complexes was almost complete below 40$0^{\circ}C$. The primary product of the decomposition process was m-Al2O3, which transformed to $\beta$"- or $\beta$-Al2O3 at temperature higher than 100$0^{\circ}C$. We found that the powder prepared at 120$0^{\circ}C$ had only $\beta$"- and $\beta$-Al2O3.EX>-Al2O3.

• 한국세라믹학회지
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• 제36권7호
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• pp.698-704
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• 1999

Li rich Li1+xMn2-xO4(x=0.07) spinel powders were prepared by an oxalate precipitation of wet chemical methods at temperature lower than $600^{\circ}C$. The FTIR results showed that the powders prepared at $600^{\circ}C$ had high degree of crystal quality comparing with the spinel powders prepared by solid state reaction at 75$0^{\circ}C$ which was the lowest synthesis temperature of the solid state reaction method. The particle size of powders prepared by the oxalate precipitation at $600^{\circ}C$ was smaller than 0.2${\mu}{\textrm}{m}$ and the specific surface area was 11.01 m2/g A heat treatment over 90$0^{\circ}C$ formed second phase in the precipitates. It was shown that there were phase transitions at temperatures. T1,T2 and T2. The transitions involved weight loss and gain during heating and cooling. The low temperature synthesis below $600^{\circ}C$ avoided the second phase formation and the prepared powders showed improved compositional and physical properties for secondary lithium battery applications.

• 한국세라믹학회지
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• 제44권8호
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• pp.457-463
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• 2007

Y, Ba and Cu nitrates were precipitated by oxalic acid at pH 4. The Y, Ba and Cu oxalate powders were vacuum dried and characterized by XRD, DT/TGA and etc. Yttrium nitrate precipitated as $NH_4Y(C_2O_4){_2}H_2O$ and converted to $Y_2O_3$ above $450^{\circ}C$. Ba precipitated with two phases, $Ba(HC_2O_4){_2}2H_2O\;and\;Ba(C_2O_4)$. The amount of each precipitates was 4 : 1, Cu precipitated non-hydrated form, $Cu(C_2O_4)$. The vacuum drying was successful to characterize precipitated powder, which had been generally known as amorphous gel.

• 한국환경과학회지
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• 제21권5호
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• pp.555-562
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• 2012

The experimental determination of equilibrium constants is required to estimate concentrations of reagents and/or products in environmental chemical reactions. For an example, the choice of copper (Cu) complexation reactions was motivated by their fast kinetics and the ease of measurement of Cu by an ion-sensitive electrode. Each individual titrant of sulfate ($SO{_4}^{2-}$) and oxalate ($C_2O{_4}^{2-}$) was expected to have its own unique characteristics, depending on the bonding in Culigands connected to the aqueous species. The complexation reaction of Cu with $SO{_4}^{2-}$ somewhat fast reached equilibrium status compared with $C_2O{_4}^{2-}$. The experimental equilibrium constants ($K_{eq}$) of copper sulfate ($CuSO_4$) and copper oxalate ($CuC_2O_4$) were determined $10^{2.2}$ and $10^{3{\sim}4.3}$, respectively.

• 한국세라믹학회지
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• 제28권3호
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• pp.215-224
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• 1991

The synthesis of SrTiO3 powders having high purity and homogeneous submicron particle size was attempted by the oxalate method. The microstructure and dielectric properties of SrTiO3 based boundary layer capacitor (BLC) were investigated. Strontium titanyl oxalate[SrTiO(C2O4)2.4H2O] was prepared from the mixing solution of (Sr, Ti) using oxalic acid(H2C2O4) as a precipitating agent at 8$0^{\circ}C$. The crystalline SrTiO3 powder was obtained by thermal decomposition of the precipitate above $600^{\circ}C$. The crystalline SrTiO3 powder containing Nb2O5 as a dopant, TiO2 and SiO2 as additives was sintered at 1360~144$0^{\circ}C$ in the reducing atmosphere to get semiconductive SrTiO3. Insulating material containing PbO-Bi2O3-B2O3 frit was printed on the sintered semiconductive SrTiO3 and fired at 120$0^{\circ}C$ for 2h to get the grain boundary diffusion.

• 분석과학
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• 제10권1호
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• pp.31-34
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• 1997

pH 4~5에서$ Ti^{4+}$ 이온을 여분의 옥살산 음이온으로 안정화시킨 다음 같은 당량의 $Ba^{2+}$ 이온이 첨가된 환경수 시료와 일시에 혼합시켜 줌으로써 barium titanate의 선구물질인 barium titanyl oxalate를 합성하였다. 이 때 환경수 시료 속에 미량으로 존재하는 $Cd^{2+}$ 및 $Pb^{2+}$ 이온이 정량적으로 공침되었으며, 이 공침법은 이들 원소의 분석을 위한 사전 농축법으로 활용 가능하였다.