• Title/Summary/Keyword: Solvent Decomposition

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Influence of PVP on the Thickness of Ferroelectric (Na,K)NbO3 Film by Sol-Gel (솔-젤 법을 통해 제조된 강유전체 (Na,K)NbO3 막의 두께에 미치는 PVP의 영향)

  • Kim, Dae-Gun;Yoo, In-Sang;Kim, Sae-Hoon;Kim, Jin-Ho
    • Korean Journal of Materials Research
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    • v.22 no.12
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    • pp.696-700
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    • 2012
  • (Na, K) $NbO_3$ thick film was successfully achieved using a sol-gel coating process with the addition of polyvinylpyrrolidone (PVP) to a metal alkoxide solution. The transparent coating solution, mixed with Nb:PVP = 1:1 in a molar ration, was synthesized by evaporating the solvent to over 62.5 wt%. Additive PVP increased the viscosity of the solution so that the coating thickness could be enhanced. The thickness of the (Na, K) $NbO_3$ film assisted by PVP was ca. 320 nm at the time of deposition; this value is four times thicker than that of the sample fabricated without PVP. Also, due to PVP binding with the OH groups of the metal alkoxide, the condensation reaction in the film was suppressed. The crystalline size of the (Na, K) $NbO_3$ films assisted by PVP was ca. 15 nm smaller than that of the film fabricated without PVP. After the sintering process at $700^{\circ}C$, the (Na, K) $NbO_3$ films were mainly composed of randomly oriented (Na, K) $NbO_3$ phase of perovskite crystal structure, including a somewhat secondary phase of $K_2Nb_4O_{11}$. However, by adding PVP, the content of the secondary phase became quite smaller than that of the sample without PVP. It was thought that the addition of PVP might have the effect of restraining the loss of potassium and that PVP could hold metalloxane by strong hydrogen bonding before complete decomposition. Therefore, the film thickness of the (Na, K) $NbO_3$ films could be considerably advanced and made more crack-free by the addition of PVP.

EDTA Surface Capped Water-Dispersible ZnSe and ZnS:Mn Nanocrystals

  • Lee, Jae-Woog;Lee, Sang-Min;Huh, Young-Duk;Hwang, Cheong-Soo
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1997-2002
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    • 2010
  • ZnSe and ZnS:Mn nanocrystals were synthesized via the thermal decomposition of their corresponding organometallic precursors in a hot coordinating solvent (TOP/TOPO) mixture. The organic surface capping agents were substituted with EDTA molecules to impart hydrophilic surface properties to the resulting nanocrystals. The optical properties of the water-dispersible nanocrystals were analyzed by UV-visible and room temperature solution photoluminescence (PL) spectroscopy. The powders were characterized by X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), and confocal laser scanning microscopy (CLSM). The solution PL spectra revealed emission peaks at 390 (ZnSe-EDTA) and 597 (ZnS:Mn-EDTA) nm with PL efficiencies of 4.0 (former) and 2.4% (latter), respectively. Two-photon spectra were obtained by fixing the excitation light source wavelengths at 616 nm (ZnSe-EDTA) and 560 nm (ZnS:Mn-EDTA). The emission peaks appeared at the same positions to that of the PL spectra but with lower peak intensity. In addition, the morphology and sizes of the nanocrystals were estimated from the corresponding HR-TEM images. The measured average particle sizes were 5.4 nm (ZnSe-EDTA) with a standard deviation of 1.2 nm, and 4.7 nm (ZnS:Mn-EDTA) with a standard deviation of 0.8 nm, respectively.

Hemicellulose Recovery from Lignocellulosic Material Hydrolyzed by Water (물로 가수분해된 섬유성 기질로부터 hemicellulose 회수)

  • Kim, Sung-Bae;Kim, Chang, Joon
    • KSBB Journal
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    • v.20 no.4
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    • pp.317-322
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    • 2005
  • Various recovery methods were investigated to maximize hemicellulose recovery from lignocellulosic material hydrolyzed by pure water. The pretreatment conditions of water hydrolysis were $170\~180^{\circ}C$ and 1 hour of reaction time. The percentage of hemicellulose solubilized increased as the temperature increased from 170 to $180^{\circ}C$. However, significant decomposition of sugar was observed at temperature of $180^{\circ}C$. From the results of water hydrolysis, the total amount of glucan in solid residue and liquid hydrolyzate was close to the total glucan in the original biomass. For hemicellulose, however, there was a significant difference between both contents. To prove this difference, various recovery methods were proposed. From the total sugar accountability (sugar in liquid + sugar in solid), it was confirmed that hemicellulose recovery in the hydrolyzate was increased if the product including both hydrolyzate and solid residue was physically stimulated by such as heating and ultrasound irradiation. This indicated that, in commercial scale processes that much bigger substrate sizes are used and a sufficient amount of leaching solvent can not be used after pretreatment, a significant amount of oligomers could be trapped in the solid matrix.

Preparation of Mg(OH)2 Dispersion and its Application to PET Non-woven Textile as Flame Retardant Coating (수산화마그네슘 분산상의 제조와 PET 부직포 섬유의 난연 코팅제 적용)

  • Lim, Hyung-Mi;Hyun, Mi-Kyung;Jeong, Sang-Ok;Lee, Dong-Jin;Lee, Seung-Ho
    • Journal of the Korean Ceramic Society
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    • v.48 no.6
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    • pp.537-542
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    • 2011
  • Magnesium hydroxide as a non-halogen flame retardant has increasing attention due to its non-toxicity, high decomposition temperature and smoke suppressant ability during combustion. For the application of magnesium hydroxide retardant to the textile by soaking and coating method, the prerequisite for the coating is a small particle size, stable dispersion, and adhesion to the textile. The dispersion of $Mg(OH)_2$ particles and stability of the coating was checked by monitoring the change of transmittance and backscattering by varying the types of dispersion agents, binder, solvent, and $Mg(OH)_2$ source, and their compositions in the coating. The $Mg(OH)_2$ dispersion coating was applied to PET(poly(ethylene terephthalate)) non-woven textile. The physical properties are characterized by surface morphology, amount of coating, particle dispersion, and adhesion test. The flame retardant $Mg(OH)_2$ coated textile has been compared by limited oxygen index(LOI) and thermal gravimetry and differential scanning calorimetry(TG-DSC). It was found that phosphorous additive may give synergistic effect on $Mg(OH)_2$ flame retardant coating to make the flame retardant PET non-woven textile.

Fabrication and NOx Gas Sensing Properties of LaMeO3 (Me = Cr, Co) by Polymeric Precursor Method (Polymeric Precursor법에 의한 LaMeO3 (Me = Cr, Co)의 제조 및 NOx 가스 검지 특성)

  • Lee, Young-Sung;Shimizu, Y.;Song, Jeong-Hwan
    • Korean Journal of Materials Research
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    • v.21 no.8
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    • pp.468-475
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    • 2011
  • [ $LaMeO_3$ ](Me = Cr, Co) powders were prepared using the polymeric precursor method. The effects of the chelating agent and the polymeric additive on the synthesis of the $LaMeO_3$ perovskite were studied. The samples were synthesized using ethylene glycol (EG) as the solvent, acetyl acetone (AcAc) as the chelating agent, and polyvinylpyrrolidone (PVP) as the polymer additive. The thermal decomposition behavior of the precursor powder was characterized using a thermal analysis (TG-DTA). The crystallization and particle sizes of the $LaMeO_3$ powders were investigated via powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and particle size analyzer, respectively. The as-prepared precursor primarily has $LaMeO_3$ at the optimum condition, i.e. for a molar ratio of both metal-source (a : a) : EG (80a : 80a) : AcAc (8a) inclusive of 1 wt% PVP. When the as-prepared precursor was calcined at $700^{\circ}C$, only a single phase was observed to correspond with the orthorhombic structure of $LaCrO_3$ and the rhombohedral structure of $LaCoO_3$. A solid-electrolyte impedance-metric sensor device composed of $Li_{1.5}Al_{0.5}Ti_{1.5}(PO_4)_3$ as a transducer and $LaMeO_3$ as a receptor has been systematically investigated for the detection of NOx in the range of 20 to 250 ppm at $400^{\circ}C$. The sensor responses were able to divide the component between resistance and capacitance. The impedance-metric sensor for the NO showed higher sensitivity compared with $NO_2$. The responses of the impedance-metric sensor device showed dependence on each value of the NOx concentration.

Stability and Bioavailability on Prodrug of 5-Flurouracil (I). Synthesis, Physicochemical Properties, Stabilities and Antitumor Activities of 1-Glycyloxymethyl-5-fluorouracil Hydrochloride (5-Fluorouracil의 Prodrug에 대한 안정성 및 생체이용율에 관한 연구(I). 1-Glycyloxymethyl-5-fluorouracil HCl의 제조, 물리화학적 성질, 안정성 및 항암효과)

  • Jee, Ung-Kil;Lee, Gye-Won;Park, Mork-Soon
    • Journal of Pharmaceutical Investigation
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    • v.22 no.3
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    • pp.185-196
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    • 1992
  • To assess its suitability as a prodrug of 5-fluorouracil (5-FU), 1-glycyloxymethyl-5-FU HCl (GFU), a 5-fluorouracil derivative having a glycyloxymethyl group at the N-l position was synthetized. Its physicochemical properties and hydrolysis kinetics, in aqueous solution of pH $1{\sim}10$ and in the presence of human plasma or rat liver homogenate were studied. Its acute toxicity and antitumor activity against sarcoma 180 were also examined, GFU showed higher lipid/water partition coefficient than 5-FU. The calculated $pK_{\alpha}$ values of 5-FU and GFU were 8.02 and 7,20, respectively. The decomposition rates of GFU in aqueous solution showed a pH-dependence over the pH range used, which could be ascribed to solvent catalysed hydrolysis reaction at pH lower than 4,16 and to specific hydroxide ion hydrolysis reaction at pH higher than 4,16, The half-life of GFU was 6,9 min in 80% human plasma solution and less than 3 min in rat liver homogenate at $37^{\circ}C$, The $LD_{50}$ value of 5-FU was 240 mg/kg while that of GFU was 440.6 mg/kg (226 mg as 5-FU). Both of 5FU and GFU showed a strong antitumor activity, Therapeutic ratios of 5-FU and GFU were 3.07 and 3.55, respectively.

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Direct Synthesis of H2O2 over Ti-Containing Molecular Sieves Supported Gold Catalysts: A Comparative Study for In-situ-H2O2-ODS of Fuel

  • Zhang, Han;Liu, Guangliang;Song, Haiyan;Chen, Chunxia;Han, Fuqin;Chen, Ping;Zhao, Zhixi;Hu, Shaozheng
    • Bulletin of the Korean Chemical Society
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    • v.34 no.10
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    • pp.3065-3072
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    • 2013
  • Direct synthesis of $H_2O_2$ and in situ oxidative desulfurization of model fuel over Au/Ti-HMS and Au/TS-1 catalysts has been comparatively investigated in water or methanol. Maximum amount (82%) of active $Au^0$ species for $H_2O_2$ synthesis was obtained. Au/Ti-HMS and Au/TS-1 exhibited the contrary performances in $H_2O_2$ synthesis as $CH_3OH/H_2O$ ratio of solvent changed. $H_2O_2$ decomposition and hydrogenation in water was inhibited by the introduction of methanol. Effect of $O_2/H_2$ ratio on $H_2O_2$ concentration, $H_2$ conversion and $H_2O_2$ selectivity revealed a relationship between $H_2O_2$ generation and $H_2$ consumption. The highest dibenzothiophene removal rate (83.2%) was obtained over Au/Ti-HMS in methanol at 1.5 of $O_2/H_2$ ratio and $60^{\circ}C$. But removal of thiophene over Au/TS-1 should be performed in water without heating to obtain a high removal rate (61.3%). Meanwhile, $H_2$ conversion and oxidative desulfurization selectivity of $H_2$ were presented.

A Selective Determination Method of Inorganic and Organic Mercury (무기수은과 유기수은의 선택정량)

  • Kim, Chon Han
    • Journal of the Korean Chemical Society
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    • v.41 no.8
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    • pp.392-398
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    • 1997
  • A method of selective determination of inorganic and organic mercury compounds has been described. The $CHCl_3$ solution of a high molecular quaternary alkylammonium salt, Aliquat 336 was used for the simultaneous preconcentration of both inorganic, $Hg^{2+}$ as its thiocyanate complex, and organic mercury compounds, $CH_3HgCl$ and $C_2H_3O_2$ $HgC_6H_5$ by extraction from their aqueous solution. Selective separation of the inorganic mercury from the extract was followed by stripping with 3 M $HClO_4 $ solution for the subsequent determination by CVAAS. Organic mercury was also determined by CVAAS after removal of $CHCl_3solvent$ from the extract and decomposition of the residue with 4% $KMnO_4 $-1 MH_2$S0_4$. The mixtures of inorganic and organic mercury compounds contained 1.0 $\mug$ as Hg in 50 mL of sample solution(0.02 ${\mu}gHg/mL$) were analysed within ${\pm}6%$ by absolute errors.

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Clean and Efficient Synthesis of Furfural From Xylose by Microwave-Assisted Biphasic System using Bio-Based Heterogeneous Acid Catalysts

  • Vo, Anh Thi Hoang;Lee, Hong-shik;Kim, Sangyong;Cho, Jin Ku
    • Clean Technology
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    • v.22 no.4
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    • pp.250-257
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    • 2016
  • As an attempt to replacing petroleum-based chemicals with bio-based ones, synthesis of furfural from biomass-derived xylose attracts much attention in recent days. Conventionally, furfural from xylose has been produced via the utilization of highly corrosive, toxic, and environmentally unfriendly mineral acids such as sulfuric acid or hydrochloric acid. In this study, microwave-assisted biphasic reaction process in the presence of novel bio-based heterogeneous acid catalysts was developed for the eco-benign and effective synthesis of furfural from xylose. The microwave was irradiated for reaction acceleration and a biphasic system consisting of $H_2O$ : MIBK (1 : 2) was designed for continuous extraction of furfural into the organic phase in order to reduce the undesired side products formed by decomposition/condensation/oligomerization in the acidic aqueous phase. Moreover, sulfonated amorphous carbonaceous materials were prepared from wood powder, the most abundant lignocellulosic biomass. The prepared catalysts were characterized by FT-IR, XPS, BET, elemental analysis and they were used as bio-based heterogeneous acid catalysts for the dehydration of xylose into furfural more effectively. For further optimization, the effect of temperature, reaction time, water/organic solvent ratio, and substrate/catalyst ratio on the xylose conversion and furfural yield were investigated and 100% conversion of xylose and 74% yield of furfural was achieved within 5 h at $180^{\circ}C$. The bio-based heterogeneous acid catalysts could be used three times without any significant loss of activity. This greener protocol provides highly selective conversion of xylose to furfural as well as facile isolation of product and bio-based heterogeneous acid catalysts can alternate the environmentally-burdened mineral acids.

Study on Synthesis of Honeycomb-patterned Resin Dispersed Silver Nanoparticles (은 나노입자가 분산된 Honeycomb-patterned 수지 합성에 대한 연구)

  • Lee, Dong Chang;Lee, Jong Jib
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.18 no.2
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    • pp.711-718
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    • 2017
  • Silver nanoparticles were attached by chemical reduction after synthesizing a porous PVK-CTA complex. The PVK-CTA complex was synthesized by polymerizing N-vinylcarbazole in a CTA-chloroform solution using iron(III) chloride as an oxidizing agent and a honeycomb-pattern with uniformly formed macropores was formed by applying steam to the complex surface soaked with a volatile solvent under humid conditions. Using TTF as a reducing agent and PVP as a dispersant, silver nanoparticles were attached on the Honeycomb-pattern complex surface through chemical reduction. The formation of the complex was confirmed by FT-IR and UV-Vis spectrometry, and the degree of thermal decomposition of the complexes was analyzed after N-vinylcarbazole was polymerized by varying its concentration. The uniformity of the pores on the composite surface and the dispersibility of the attached silver nanoparticles were investigated by SEM. The dispersibility of the silver nanoparticles was also analyzed by varying the concentrations of reducing agent and dispersant and precursor.