• Title/Summary/Keyword: Hydrothermal reaction

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Synthesis of Microporous Zeolitic Membranes and Application in Alcohol/water Separation (다공성 제올라이트 멤브레인의 합성 및 알코올 /물 분리에의 응용)

  • 김건중;남세종
    • Membrane Journal
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    • v.9 no.2
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    • pp.97-106
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    • 1999
  • A and 2SM-5 type zeoli tic crystal films were synthesized on porous supports from the reaction mixture of 1.9 ${SiO}_2$1.5 $Na_20-Al_2O_3-40$ $H_20$ and $Si0_2$-0.l3 $Na_2O$-52 $H_20$-O.l2 TPAOH composition, respectively. The zeolite films were characterized by XRD and SEM. The 2SM -5 crystals grown on the porous matrix were very closely bound together. It was so difficult to obtain the perfectly intergrown crystals in the case of A-type zeolite and this crystal was transformed into P-type zeolite membrane with a prolonged reaction time. The densely intergrown A type zeolite crystal membrane could be also synthesized by the hydrothermal treatment at 100$^{\cirt}C$ after pressing the reaction mixture without addition of water. The pervaporation performance of the synthesized porous inorganic membranes was investigated for alcohol and water mixtures. A-type zeolite membrane crystallized as a thin film showed the selective \'Jermeability of water from the mixtures through the molecular sieving activity of micropores.

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Shape-Selective Catalytic Reactions of Toluene with n-Propylalcohol Over ZSM-5 Zeolites (ZSM-5 제올라이트에서 n-프로필알코올의 톨루엔에 대한 형상 선택적 촉매반응)

  • Han-Yun Lee;Byoung Joon Ahn
    • Journal of the Korean Chemical Society
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    • v.37 no.3
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    • pp.317-326
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    • 1993
  • The acid catalytic reactions of toluene with n-propylalcohol were investigated and the adsorption experiments of dialkylbenzene isomers were carried out at 100$^{\circ}C$ over modified HZSM-5 zeolites. ZSM-5 zeolite was synthesized by the hydrothermal reaction using 4-propylammonium ion, sodium aluminate and colloidal silica etc., and several zeolite catalysts, including H-, K-, Sr-, P-Mg-HZSM-5, H-Y and H-mordenite, were prepared by conventional methods. The main reaction products of toluene with n-propylalcohol over HZSM-5 catalyst include not only xylenes, propyltoluenes, but also ethyltoluenes and high para-selectivity among dialkylbenzene isomers was observed on P-Mg-HZSM-5 zeolite. The diffusion coefficients of various p-dialkylbenzenes are nearly the same, about 1 ${times}$ 10$^{-10}$ cm$^2$/sec and that of m-xylene was about one tenth of o-xylene. These reaction and adsorption characteristics were interpreted in the light of the shape-selectivity related to related to the zeolite pore structure and the zeolitic acidity.

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Characterization of NiO and Co3O4-Doped La(CoNi)O3 Perovskite Catalysts Synthesized from Excess Ni for Oxygen Reduction and Evolution Reaction in Alkaline Solution (과량의 니켈 첨가로 합성된 NiO와 Co3O4가 도핑된 La(CoNi)O3 페로브스 카이트의 알칼리용액에서 산소환원 및 발생반응 특성)

  • BO, LING;RIM, HYUNG-RYUL;LEE, HONG-KI;PARK, GYUNGSE;SHIM, JOONGPYO
    • Transactions of the Korean hydrogen and new energy society
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    • v.32 no.1
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    • pp.41-52
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    • 2021
  • NiO and Co3O4-doped porous La(CoNi)O3 perovskite oxides were prepared from excess Ni addition by a hydrothermal method using porous silica template, and characterized as bifunctional catalysts for oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) for Zn-air rechargeable batteries in alkaline solution. Excess Ni induced to form NiO and Co3O4 in La(CoNi)O3 particles. The NiO and Co3O4-doped porous La(CoNi)O3 showed high specific surface area, up to nine times of conventionally synthesized perovskite oxide, and abundant pore volume with similar structure. Extra added Ni was partially substituted for Co as B site of ABO3 perovskite structure and formed to NiO and Co3O4 which was highly dispersed in particles. Excess Ni in La(CoNi)O3 catalysts increased OER performance (259 mA/㎠ at 2.4 V) in alkaline solution, although the activities (211 mA/㎠ at 0.5 V) for ORR were not changed with the content of excess Ni. La(CoNi)O3 with excess Ni showed very stable cyclability and low capacity fading rate (0.38 & 0.07 ㎶/hour for ORR & OER) until 300 hours (~70 cycles) but more excess content of Ni in La(CoNi)O3 gave negative effect to cyclability.

Synergistically Enhanced Oxygen Evolution Catalysis with Surface Modified Halloysite Nanotube

  • Hyeongwon Jeong;Bharat Sharma;Jae-ha Myung
    • Journal of Electrochemical Science and Technology
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    • v.14 no.1
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    • pp.96-104
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    • 2023
  • Synergistically increased oxygen evolution reaction (OER) of manganese oxide (MnO2) catalyst is introduced with surface-modified halloysite nanotube (Fe3O4-HNTs) structure. The flake shaped MnO2 catalyst is attached on the nanotube template (Fe3O4-HNTs) by series of wet chemical and hydrothermal method. The strong interaction between MnO2 and Fe3O4-HNTs maximized active surface area and inter-connectivity for festinate charge transfer reaction for OER. The synergistical effect between Fe3O4 layer and MnO2 catalyst enhance the Mn3+/Mn4+ ratio by partial replacement of Mn ions with Fe. The relatively increased Mn3+/Mn4+ ratio on MnO2@FHNTs induced 𝜎* orbital (eg) occupation close to single electron, improving the OER performances. The MnO2@FHNTs catalyst exhibited the reduced overpotential of 0.42 V (E vs. RHE) at 10 mA/cm2 and Tafel slope of (99 mV/dec), compared with that of MnO2 with unmodified HNTs (0.65 V, 219 mV/dec) and pristine MnO2 (0.53 V, 205 mV/dec). The present study provides simple and innovative method to fabricate nano fiberized OER catalyst for a broad application of energy conversion and storage systems.

Rich Se Nanoparticles Modified Mo-W18O49 as Enhanced Electrocatalyst for Hydrogen Evolution Reaction

  • Wang, Jun Hui;Tang, Jia-Yao;Fan, Jia-Yi;Meng, Ze-Da;Zhu, Lei;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.32 no.2
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    • pp.57-65
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    • 2022
  • Herein a rich, Se-nanoparticle modified Mo-W18O49 nanocomposite as efficient hydrogen evolution reaction catalyst is reported via hydrothermal synthesized process. In this work, Na2SeSO3 solution and selenium powder are used as Se precursor material. The structure and composition of the nanocomposites are characterized by X-ray diffraction (XRD), high-resolution field emission scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), EDX spectrum analysis and the corresponding element mapping. The improved electrochemical properties are studied by current density, and EIS analysis. The as-prepared Se modified Mo-W18O49 synthesized via Na2SeSO3 is investigated by FE-SEM analysis and found to exhibit spherical particles combined with nanosheets. This special morphology effectively improves the charge separation and transfer efficiency, resulting in enhanced photoelectric behavior compared with that of pure Mo-W18O49. The nanomaterial obtained via Na2SeSO3 solution demonstrates a high HER activity and low overpotential of -0.34 V, allowing it to deliver a current density of 10 mA cm-2.

Low-temperature Hydrothermal Synthesis of Organic Smectite from Siliceous Mudstone (규질 이암으로부터 유기 스멕타이트의 저온 수열합성)

  • 노진환
    • Journal of the Mineralogical Society of Korea
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    • v.17 no.1
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    • pp.49-59
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    • 2004
  • Organic smectite was hydrothermally synthesized by treating the opal-rich siliceous mudstone from the Pohang area with TMAOH solutions and 1:1 solutions of TMAOH+NaOH at $80^{\circ}C$ and concentrations ranging 10∼15%. Smectite was solely formed without accompanying any mineral products in case of TMAOH, whereas NaP and hydroxysodalite was synthesized together with smectite under the blending solution of TMAOH+NaOH. The synthesized smectite is identified as an organic smectite intercalating $TMA^{+}$ within its interlayer site, specifically corresponding to monmorillonite species, through mineralogical characterization by XRD, DTA, and IR analyses. The experimental results indicate that main precursor of the synthesized smectite is undoubtedly opal-CT, and the original sedimentary smectite included as considerable amounts in the mudstone seems to play a major role as Al-sources necessary far the smectite formation. Original inert components such as quartz and mica do not affect mostly to the synthesis reaction, and thus, are resultantly found as impurities in the synthetic products. These experimental results may imply that a new effective method for the low-temperature (less than $100^{\circ}C$) hydrothermal synthesis of organic smectite will be established if some Al-sources adequate for this synthetic system are available.

Synthesis of MnO2 Nanowires by Hydrothermal Method and their Electrochemical Characteristics (수열합성법을 이용한 망간 나노와이어 제조 및 이의 전기화학적 특성 연구)

  • Hong, Seok Bok;Kang, On Yu;Hwang, Sung Yeon;Heo, Young Min;Kim, Jung Won;Choi, Bong Gill
    • Applied Chemistry for Engineering
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    • v.27 no.6
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    • pp.653-658
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    • 2016
  • In this work, we developed a synthetic method for preparing one-dimensional $MnO_2$ nanowires through a hydrothermal method using a mixture of $KMnO_4$ and $MnSO_4$ precursors. As-prepared $MnO_2$ nanowires had a high surface area and porous structure, which are beneficial to the fast electron and ion transfer during electrochemical reaction. The microstructure and chemical structure of $MnO_2$ nanowires were characterized by scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction, and Brunauer-Emmett-Teller measurements. The electrochemical properties of $MnO_2$ nanowire electrodes were also investigated using cyclic voltammetry and galvanostatic charge-discharge with a three-electrode system. $MnO_2$ nanowire electrodes showed a high specific capacitance of 129 F/g, a high rate capability of 61% retention, and an excellent cycle life of 100% during 1000 cycles.

Physicochemical Properties of MnO2 Catalyst Prepared via Hydrothermal Process and its Application for CO Oxidation (수열방법으로 합성된 이산화망간의 물리화학적 특성과 일산화탄소 산화반응)

  • Lee, Young-Ho;Jeon, Su A;Park, Sang-Jun;Youn, Hyun Ki;Shin, Chae-Ho
    • Clean Technology
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    • v.21 no.4
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    • pp.248-256
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    • 2015
  • MnO2 was prepared by a hydrothermal process method in the range of 120-200 ℃ and 0.5-5 h, calcined at 300 ℃ after induction of precipitation using KMnO4 and MnCl2・4H2O, and its catalytic activity was compared for CO oxidation. The catalysts were characterized using by X-ray diffraction, N2-sorption, scanning electron microscopy, and temperature programmed reduction of H2 or CO. The crystalline structure of pure α-MnO2 or hybrid α/β-MnO2 was controlled by the preparation conditions. The pure α-MnO2 showed better catalytic activity and thermal stability than hybrid α/β-MnO2. Especially, α-MnO2 prepared at 150 ℃ for 1 h has the highest specific surface area 214 m2 g-1, reducibility and labile lattice oxygen species analyzed by H2, CO-TPR, respectively. It also showed the best CO oxidation activity in both conditions of temperature programmed and isothermal reaction. The results came from the physicochemical properties of catalysts like the crystalline structure, specific surface area, reducibility and lattice oxygen species, and which are correlated with catalytic performance.

A Study on the Growth of KTP$(KTiOPO_4)$ Single Crystal (KTP$(KTiOPO_4)$ 단결정의 육성에 관한 연구)

  • 차용원;최원웅;장지연;오근호;김판채
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.3 no.1
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    • pp.12-17
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    • 1993
  • Growth runs of KTP single crystals were carried out by the hydrothermal method. KTP powders used for the crystal growth were prepared as a single phase by the solid state reaction of a stoichiometric mixture of $KH_2PO_4 and TiO_2$ at TEX>$800^{\circ}C$ and subsequently by the hydrothermal treatment at $250^{\circ}C$ 4m KF solution. The most effective solvents for the crystal growth of KTP were KF and K $K_2HPO_4$ solutions. Solubilities of KTP in these solutions were positive over the range $350~450^{\circ}C$.Seed crystals of good quality could be obtained by the horizontal temperature gradient method at temperatures over the range 380~430^{\circ}C$ in these solutions. The hydrothermal conditions for the high growth rates of seed crystals are as follows: growth method; vertical temperature gradient method, solvent; 4m KF or $K_2HPO_4$ solution, temperature region; $400~450^{\circ}C$, pressure region; $1000~1500kg/cm^2$, where solubility of KTP was large enough to proceed the growth. Under such conditions, seed crystals of KTP are grown at a rate of approximately 0.06-0.08mm/day in the direction of the c-axis. Morphologies of grown crystals tended to be bounded by (100), (011) and (201) faces.

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Recycling Organic Sludge into Modification Block by Hydrothermal Carbonization (HTC) (열수가압탄화공법을 적용한 유기성 슬러지의 응용 블록 제조에 관한 연구)

  • Hyewon Park;Minah Oh;Seungjin Oh;Woori Cho;Jinman Chang;Jai-young Lee
    • Clean Technology
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    • v.29 no.2
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    • pp.102-108
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    • 2023
  • This study applied a hydrothermal carbonization (HTC) method to carbonize sewage sludge in order to satisfy the criteria of the Waste Management Act for recycled products and to explore the possibility of recycling sludge into modification blocks. Cement was mixed with carbonized sludge generated at the optimal temperature and reaction time during HTC. After that, the compressive strengths of the modification blocks were measured by conducting both a performance and leaching test. The results of the leaching test showed that heavy metals were not detected, and the specific gravity and absorption rates were less than 1.7 and 10%, respectively, indicating that all species satisfied the criteria. The results of the compressive strength test showed that a mixing ratio of 5% and 7% with cement cured for 28 days satisfied the criteria of A, B, and C type blocks but a mixing ratio of 3% with cement did not satisfy the criteria of A type blocks after 28 days. However, after additional curing for 42 days, the mixing ratio of 3% also satisfied the A type block criteria. Therefore, the optimal mixing ratio of carbonized sludge and cement was considered to be between 3% and 5% and confirmed that the modified blocks could be utilized as aggregates.