• 제목/요약/키워드: Solvent Decomposition

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

  • 김대건;유인상;김세훈;김진호
    • 한국재료학회지
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    • 제22권12호
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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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    • 제31권7호
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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.

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

  • 김성배;김창준
    • KSBB Journal
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    • 제20권4호
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    • pp.317-322
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    • 2005
  • 섬유성 기질을 물 가수분해하여 생긴 당을 최대한 회수하는 여러 회수방법을 조사하였다. 사용한 전처리 조건은 반응온도가 $170\~180^{\circ}C$, 반응시간이 1시간이었다. 반응 온도가 170에서 $180^{\circ}C$로 증가함에 따라 xylan의 용해율은 증가하지만 $180^{\circ}C$ 이상에서는 상당양의 당이 분해됨을 알 수 있었다. 가수분해 결과로부터 남은 고체기질과 당화액에서 얻은 당의 물질수지를 조사하였는데 glucan의 경우는 비교적 잘 맞으나, 헤미셀룰로오스는 처리되지 않은 기질에 포함된 초기양과 비교할 때 상당한 차이가 났다. 그래서 여러가지 회수방법을 고안하여 당의 물질수지를 조사한 결과 회수기간동안 열을 가하거나 초음파를 조사하는 방법과 같은 물리적인 자극을 주면 액상에서 헤미셀룰로오스 회수율이 증가되는 것이 확인되었다. 이런 사실로부터 당 회수시 기질이 크고 전처리 후 침출용매를 많이 사용할 수 없는 상업적인 공정의 경우 상당양의 올리고당이 고체기공내 갇혀 액상으로 회수되지 못할 것으로 생각된다.

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

  • 임형미;현미경;정상옥;이동진;이승호
    • 한국세라믹학회지
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    • 제48권6호
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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.

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

  • 이영성;;송정환
    • 한국재료학회지
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    • 제21권8호
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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.

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

  • 지웅길;이계원;박목순
    • Journal of Pharmaceutical Investigation
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    • 제22권3호
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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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    • 제34권10호
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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.

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

  • 김천한
    • 대한화학회지
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    • 제41권8호
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    • pp.392-398
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    • 1997
  • 무기수은과 유기수은을 분리하여 각각을 정량하는 방법을 연구하였다. 고분자량 알킬의 4차아민의 염, Aliquat 336의 $CHCl_3$ 용액을 이용하여 수용액 중에 함유된 무기수은이온, $Hg^{2+}$을 티오시안 착이온으로서, 그리고 유기수은 화합물, $CH_3HgCl$$C_2H_3O_2$ $HgC_6H_5$ 등을 동시에 추출농축한 다음 무기수은은 3 M $HClO_4 $ 용액으로 선택적인 역추출을 하여 CVAAS로 정량하고, 유기수은은 추출액의 $CHCl_3$ 을 증발 제거한 후 그 찌끼를 4% $KMnO_4 $-1M $H_2$$S0_4 $ 용액으로 분해하여 무기수은 이온으로 만들어서 역시 CVAAS로 정량하였다. 시료용액 50 mL 중에 함유된 Hg로서 1 ${\mu}g$의 무기수은과 유기수은 혼합용액(0.02 ${\mu}gHg/mL$)을 분석한 결과 절대오차 ${\pm}6%$ 이내의 결과를 얻었다.

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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
    • 청정기술
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    • 제22권4호
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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.

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

  • 이동창;이종집
    • 한국산학기술학회논문지
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    • 제18권2호
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    • pp.711-718
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    • 2017
  • Poly(N-vinylcarbazole) (PVK)-cellulose triacetate (CTA) 복합체를 합성하고, 필름에 기공을 형성시킨 뒤, 화학적 환원법을 통해 은 나노입자를 부착하는 것을 연구하였다. PVK-CTA 복합체는 CTA-chloroform 용액에서 iron(III) chloride를 산화제로 사용하여 N-vinylcarbazole을 중합시켜 복합체를 합성하였고, 얻어진 복합체를 습한 환경에서 휘발성용매로 적셔 수증기를 적용하여 macropore가 균일하게 형성된 구조인 Honeycomb-pattern을 형성시켰다. 이후 환원제로 Tetrathiafulvalene (TTF)와 분산제로 polyvinylpyrrolidone (PVP)를 사용하여 화학적 환원법을 이용해 은 나노입자를 Honeycomb-pattern이 형성된 복합체 표면에 부착시켰다. FT-IR과 UV-Vis spectrometer을 이용하여 복합체의 형성여부를 확인하였고, N-vinylcarbazole의 함량을 달리하여 중합한 뒤 복합체의 열 분해도를 측정하였다. Scanning electron microscope (SEM)을 통해 복합체 표면에 형성된 기공의 균일도와 부착된 은 나노입자들의 분산성을 분석하였으며, 환원제, 분산제, 전구체 용액의 농도를 달리하여 은나노입자의 분산성을 확인하였다.