• Title/Summary/Keyword: Pure organic solvent

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Synthesis of Ni-Ag Core-shell Nanoparticles by Polyol process and Microemulsion Process

  • Nguyen, Ngoc Anh Thu;Park, Joseph G.;Kim, Sang-Hern
    • Bulletin of the Korean Chemical Society
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    • v.34 no.10
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    • pp.2865-2870
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    • 2013
  • Ni-Ag core-shell nanoparticles were synthesized by polyol process and microemulsion technique successfully. In the polyol process, a chemical reduction method for preparing highly dispersed pure nickel and Ag shell formation have been reported. The approach involved the control of reaction temperature and reaction time in presence of organic solvent (ethylene glycol) as a reducing agent for Ag cation with poly(vinyl-pyrrolidone) (PVP. Mw = 40000) as a capping agent. In microemulsion method, the emulsion was prepared by water/cetyltrimetylammonium bromide (CTAB)/cyclohexane. The size of microemulsion droplet was determined by the molar ratio of water to surfactant (${\omega}_o$). The core-shell formation along with the change in structural phase and stability against oxidation at high temperature heat treatments of nanoparticles were investigated by X-ray diffraction and TEM analysis. Under optimum conditions the polyol process gives the Ni-Ag core-shell structures with 13 nm Ni core covered with 3 nm Ag shell, while the microemulsion method gives Ni core diameter of 8 nm with Ag shell of thickness 6 nm. The synthesized Ni-Ag core-shell nanoparticles were stable against oxidation up to $300^{\circ}C$.

The Effect of Mercaptoundecanoic Acid (MUA) Coating on Dispersion Property of Au Nanoparticles in Synthesis of Au/TiO2 Core-shell Nanoparticles (Au/TiO2 core-shell 나노입자의 합성에 있어서 Au 나노입자의 분산특성에 미치는 Mercaptoundecanoic acid (MUA)의 피복 효과)

  • Yu, Yeon-Tae;Kim, Byoung-Gyu
    • Korean Journal of Materials Research
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    • v.16 no.12
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    • pp.754-760
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    • 2006
  • Mercaptoundecanoic acid (MUA) has been used to enhance the dispersity of Au nanoparticles in organic solvent and the affinity between the Au nanoparticles surface and titanium dioxide shell in the synthesis of $Au/TiO_2$ core-shell composite nanoparticles. The dispersity of the MUA-coated Au nanoparticles in ethanol aqueous solution with different concentration of $H_2O$ was investigated by UV-Vis. absorption spectrum and the coating amount of MUA was varied from 0.02 mM to 1.0 mM. The MUA-coated Au nanoparticles were highly dispersed in pure $H_2O$ in the wide range of the coating amount of MUA. On the contrary, the MUAcoated Au nanoparticles showed an enhanced stability in the ethanol/$H_2O$=8/2 mixed solution only when the coating amount of MUA was 0.05 mM, and in the ethanol/$H_2O$=7/3 mixed solution when the coating amount of MUA was in the range from 0.02 mM to 0.17 mM. From this systematic study, it can be inferred that the stability and the dispersibility of Au nanoparticles in organic solvents are highly sensitive towards the amount of MUA coating.

Effects of Modifiers on the Supercritical $CO_{2}$ Extraction of Glycyrrhizin from Licorice and the Morphology of Licorice Tissue after Extraction

  • Kim Hyun Seok;Lee Sang Yun;Kim Byung Yong;Lee Eun Kyu;Ryu Jong Hoon;Lim Gio Bin
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.9 no.6
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    • pp.447-453
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    • 2004
  • Optimal conditions for the supercritical carbon dioxide $(scCO_{2})$ extraction of glycyr­rhizin from licorice (Glycyrrhiza glabra) were investigated, with an emphasis on the types and levels of modifiers. The morphology of the licorice tissue remaining after the $scCO_{2} $ extraction of glycyrrhizin was examined by scanning electron microscopy, coupled with measurements of ab­solute density. Conventional organic solvent extraction was also carried out for purpose of quantitative comparison. At 50 MPa and $60^{circ}C$ glycyrrhizin could not be extracted with pure $scCO_{2}$, while a considerable amount of glycyrrhizin was extracted when water was added to $scCO_{2}$ as a modifier. The highest recovery was found to be about $97\%$ when $70\%$ aqueous methanol was added to $scCO_{2}$ at a concentration of $15\%$. The optimal pressure and temperature for the supercritical fluid extraction of glycyrrhizin were observed to be 30 M Pa and $60^{circ}C$, respectively. Under these conditions, the percentage recovery of glycyrrhizin attained a maximum value of 102.67\pm$ $1.13\%$ within 60 min. Furthermore, in the case of $scCO_{2}$ modified with $70\%$ aqueous methanol, the licorice tissue obtained after extraction was found to be severely de­graded by excessive swelling, and the absolute density of the licorice residues was observed to be the highest.

Fatty Acid Composition Analysis of Major Oil Crops by One-Step Extraction/Methylation Method (일단계 추출 및 메칠화법에 의한 유료작물의 지방산 분석)

  • 김진경;김남희;방진기;이병규;박충범;이봉호
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.45 no.3
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    • pp.211-215
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    • 2000
  • Lipid extraction preceding fatty acid methyl esters preparation for gas-liquid chromatography is time-consuming and cumbersome. We performed one-step extraction/methylation method with a mixture of methanol-heptane-benzene-DMP-H$_2$SO$_4$ without prior fat extraction. The simultaneous digestion and lipid transmethylation takes place at 8$0^{\circ}C$ in a single phase. After cooling till room temperature, two phases are formed. The upper one of the phases contains the fatty acid methyl esters ready for GLC. The fatty acid composition of major industrial crops obtained by the one step extraction/methylation method (method 1 and 2) was almost identical with the fatty acid composition of the pure fats extracted with hexane by the Soxtec instrument (method 3). Due to its simplicity, speed, and reduced organic solvent the one-step extraction/methylation method (method 1 and 2) should be useful to determine overall fatty acid composition, especially in situations where many samples have to be analyzed.

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Fabrication of PHBV/Keratin Composite Nanofibrous Mats for Biomedical Applications

  • Yuan, Jiang;Xing, Zhi-Cai;Park, Suk-Woo;Geng, Jia;Kang, Inn-Kyu;Yuan, Jiang;Shen, Jian;Meng, Wan;Shim, Kyoung-Jin;Han, In-Suk;Kim, Jung-Chul
    • Macromolecular Research
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    • v.17 no.11
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    • pp.850-855
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    • 2009
  • Keratin is an important protein used in wound healing and tissue recovery. In this study, keratin was modified chemically with iodoacetic acid (IAA) to enhance its solubility in organic solvent. Poly(hydroxybutylate-co-hydroxyvalerate) (PHBV) and modified keratin were dissolved in hexafluoroisopropanol (HFIP) and electrospun to produce nanofibrous mats. The resulting mats were surface-characterized by ATR-FTIR, field-emission scanning electron microscopy (FE-SEM) and electron spectroscopy for chemical analysis (ESCA). The pure m-keratin mat was cross-linked with glutaraldehyde vapor to make it insoluble in water. The biodegradation test in vitro showed that the mats could be biodegraded by PHB depolymerase and trypsin aqueous solution. The results of the cell adhesion experiment showed that the NIH 3T3 cells adhered more to the PHBV/m-keratin nanofibrous mats than the PHBV film. The BrdU assay showed that the keratin and PHBV/m-keratin nanofibrous mats could accelerate the proliferation of fibroblast cells compared to the PHBV nanofibrous mats.

Synthesis of Organic-inorganic Core-shell Nanoparticle Powder using Immersion Annealing Process (담금 어닐링을 이용한 유·무기 코어-쉘 나노입자 파우더 합성법)

  • Choi, Young Joong;Jung, Hyunsung;Bang, Jiwon;Park, Woon Ik
    • Journal of the Microelectronics and Packaging Society
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    • v.25 no.4
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    • pp.35-40
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    • 2018
  • Simple and useful synthetic process to control the morphology of block copolymers (BCPs) is required for implementation in various device applications. However, the conventional method to use colloidal templates is not enough to realize the production of pure and massive core-shell nanoparticles due to the cost-intensive complex process. Here, we introduce a novel and facile synthesis method to realize the formation of core-shell $SiO_x$ nanoparticle power by employing an immersion annealing of a sphere-forming poly(styrene-b-dimethylsiloxane) (PS-b-PDMS) BCP. We successfully obtained a PS-encapsulated $SiO_x$ nanoparticle with a diameter of ~20 nm. In addition, we analyzed how the mixing ratio of heptane/ethanol affects the BCP morphology of self-assembled PS-b-PDMS nanoparticles, showing a worm-like structure under the optimum immersion conditions. This useful approach is expected to be extendable to other solvent-based BCP synthesis, providing a new guideline for unique BCP production.

Purification, Characterization and Immobilization of Lipase from Proteus vulgaris OR34 for Synthesis of Methyl Oleate

  • Misbah, Asmae;Koraichi, Saad Ibnsouda;Jouti, Mohamed Ali Tahri
    • Microbiology and Biotechnology Letters
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    • v.48 no.4
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    • pp.491-505
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    • 2020
  • A newly isolated strain, Proteus vulgaris OR34, from olive mill waste was found to secrete an alkaline extracellular lipase at 11 U·ml-1 when cultivated on an optimized liquid medium. This lipase was purified 94.64-fold with a total yield of 9.11% and its maximal specific activity was shown to be 3232.58 and 1777.92 U·mg-1 when evaluated using the pH-stat technique at 55℃ and pH 9 and Tributyrin TC4 or olive oil as the substrate. The molecular mass of the pure OR34 lipase was estimated to be around 31 kDa, as revealed by SDS-PAGE and its substrate specificity was investigated using a variety of triglycerides. This assay revealed that OR34 lipase preferred short and medium chain fatty acids. In addition, this lipase was stable in the presence of high concentrations of bile salt (NaDC) and calcium ions appear not to be necessary for its activity. This lipase was inhibited by THL (Orlistat) which confirmed its identity as a serine enzyme. In addition, the immobilization of OR34 lipase by adsorption onto calcium carbonate increased its stability at higher temperatures and within a larger pH range. The immobilized lipase exhibited a high tolerance to organic solvents and retained 60% of its activity after 10 months of storage at 4℃. Finally, the OR34 lipase was applied in biodiesel synthesis via oleic acid mediated esterification of methanol when using hexane as solvent. The best conversion yield (67%) was obtained at 12 h and 40℃ using the immobilized enzyme and this enzyme could be reused for six cycles with the same efficiency.

Solution-Processed Nontoxic and Abundant $Cu_2ZnSnS_4$ for Thin-Film Solar Cells

  • Mun, Ju-Ho
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2012.05a
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    • pp.65-65
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    • 2012
  • Copper zinc tin sulfide ($Cu_2ZnSnS_4$, CZTS) is a very promising material as a low cost absorber alternative to other chalcopyrite-type semiconductors based on Ga or In because of the abundant and economical elements. In addition, CZTS has a band-gap energy of 1.4~1.5eV and large absorption coefficient over ${\sim}10^4cm^{-1}$, which is similar to those of $Cu(In,Ga)Se_2$(CIGS) regarded as one of the most successful absorber materials for high efficient solar cell. Most previous works on the fabrication of CZTS thin films were based on the vacuum deposition such as thermal evaporation and RF magnetron sputtering. Although the vacuum deposition has been widely adopted, it is quite expensive and complicated. In this regard, the solution processes such as sol-gel method, nanocrystal dispersion and hybrid slurry method have been developed for easy and cost-effective fabrication of CZTS film. Among these methods, the hybrid slurry method is favorable to make high crystalline and dense absorber layer. However, this method has the demerit using the toxic and explosive hydrazine solvent, which has severe limitation for common use. With these considerations, it is highly desirable to develop a robust, easily scalable and relatively safe solution-based process for the fabrication of a high quality CZTS absorber layer. Here, we demonstrate the fabrication of a high quality CZTS absorber layer with a thickness of 1.5~2.0 ${\mu}m$ and micrometer-scaled grains using two different non-vacuum approaches. The first solution-processing approach includes air-stable non-toxic solvent-based inks in which the commercially available precursor nanoparticles are dispersed in ethanol. Our readily achievable air-stable precursor ink, without the involvement of complex particle synthesis, high toxic solvents, or organic additives, facilitates a convenient method to fabricate a high quality CZTS absorber layer with uniform surface composition and across the film depth when annealed at $530^{\circ}C$. The conversion efficiency and fill factor for the non-toxic ink based solar cells are 5.14% and 52.8%, respectively. The other method is based on the nanocrystal dispersions that are a key ingredient in the deposition of thermally annealed absorber layers. We report a facile synthetic method to produce phase-pure CZTS nanocrystals capped with less toxic and more easily removable ligands. The resulting CZTS nanoparticle dispersion enables us to fabricate uniform, crack-free absorber layer onto Mo-coated soda-lime glass at $500^{\circ}C$, which exhibits a robust and reproducible photovoltaic response. Our simple and less-toxic approach for the fabrication of CZTS layer, reported here, will be the first step in realizing the low-cost solution-processed CZTS solar cell with high efficiency.

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Separation of Nitric Acid and Gold from Gold Bearing Aqua Regia Solution by Solvent Extraction with TBP(tributyl phosphate) (금이 함유된 왕수용액으로부터 TBP(tributyl phosphate) 용매추출에 의한 질산과 금의 분리)

  • Bae, Mooki;Srivastava, Rajiv R.;Kim, Sookyung;Lee, Jae-chun
    • Resources Recycling
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    • v.26 no.1
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    • pp.51-58
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    • 2017
  • The present study to develop a process for extracting nitric acid and gold from aqua regia leach solution using TBP(tributyl phosphate) was conducted. The pure aqua regia was used to investigate the extractive behavior of nitric acid depending on the concentration of extractant, concentration ratio of nitric and hydrochloric acid. The extraction rate of nitric acid and gold from the gold bearing aqua regia was also examined. The theoretical extraction number was verified by counter current using the number of operations and the phase ratio obtained from McCabe-Thiele diagram. Stripping experiments were carried out for continuous recovery of nitric acid and gold in loaded organic. Considering the effect of extraction acid and gold, the simulation showed that greater than 99.9% extraction of $103.0mg{\cdot}L^{-1}$ gold and 98.0% of $151.2g{\cdot}L^{-1}$ nitric acid could be attained in a two and three-stage counter-current extraction at an O/A phase ratio of 1:0.85. Distilled water and sodium thiosulfate were used as the nitric acid and gold stripping solution. The stripping rates were 99.5% and 92.0%, respectively. The study revealed that the recovery of nitric acid and gold from gold bearing aqua regia was a plausible approach through simultaneous extraction and continuous stripping of nitric acid and gold.

Mesoporous Silica-Carbon Composite Membranes for Simultaneous Hydrolysis and Separation of Chiral Epoxide (카본/메조세공 실리카 복합 막을 응용한 키랄 에폭사이드의 가수분해반응과 동시 분리)

  • Choi, Seong Dae;Jeon, Sang Kwon;Park, Geun Woo;Yang, Jin Young;Kim, Geon-Joong
    • Applied Chemistry for Engineering
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    • v.25 no.5
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    • pp.503-509
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    • 2014
  • The carbon/porous silica composite membrane was fabricated in a simple manner, which could be successfully for the simultaneous separation and production of chiral epoxides and 1,2-diols, based on their differences in hydrophilic/hydrophobic natures. The chiral Co(III)-$BF_3$ salen catalyst adopted in the membrane reactor system has given the very high enantioselectivity and recyclability in hydrolysis of terminal epoxides such as ECH, 1,2-EB, and SO. The optically pure epoxide and the chiral catalyst were collected in the organic phase after hydrolysis reaction. The hydrophilic water-soluble 1,2-diol product hydrolyzed by chiral salen diffused into the aqueous phase through the SBA-16 or NaY/SBA-16 silica composite layer during the reaction. The water acted simultaneously as a reactant and a solvent in the membrane system. One optical isomer was obtained with high purity and yield, and furthermore the catalysts could be recycled without observable loss in their activity in the continuous flow-type membrane reactor.