• Title/Summary/Keyword: hydrothermal reaction method

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Synthesis of Imogolite by a Hydrothemal Method (이모골라이트의 합성)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Suh, Yong-Jae;Chae, Soo-Chun;Bae, In-Kook
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.3
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    • pp.283-287
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    • 2008
  • The imogolite synthesis wore performed by using tetraethoxysilane (TEOS) and aluminium-sec-butoxide (ASB) at < $100^{\circ}C$. A mixure of TEOS and ASB in a molar ratio of 1:2 was prepared under vigorous stirring and the experiments were performed under the hydrothemal refluxing condition. When the concentration of TEOS and ASB in solution was 0.5 M, a well-crystallized imogolite was synthesized, and the reflections wore shown at d = 22.4, $9.5\;\AA$ etc., after XRD analysis. DTA analysis shows 2 exothemal peaks at 68 and $249^{\circ}C$, suggesting the dehydration and the dehyroxylation reaction, respectively. The result of TG indicates 41% weight loss. And the weak and unsymmetrical peaks by the Si-O-Al stretching vibrations at 953 and $993cm^{-1}$ and by O-Si-O bending vibration at $562cm^{-1}$ were observed after IR analysis. The synthetic imogolite was fibrous and shows a spiders web like network structure.

The Mineral Carbonation Using Steelmaking Reduction Slag (제강 환원슬래그의 광물탄산화)

  • Ryu, Kyoung-Won;Choi, Sang-Hoon
    • Economic and Environmental Geology
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    • v.50 no.1
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    • pp.27-34
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    • 2017
  • Mineral carbonation for the storage of carbon dioxide is a CCS option that provides an alternative for the more widely advocated method of geological storage in underground formation. Carbonation of magnesium- or calcium-based minerals, especially the carbonation of waste materials and industrial by-products is expanding, even though total amounts of the industrial waste are too small to substantially reduce the $CO_2$ emissions. The mineral carbonation was performed with steelmaking reduction slag as starting material. The steelmaking reduction slag dissolution experiments were conducted in the $H_2SO_4$ and $NH_4NO_3$ solution with concentration range of 0.3 to 1 M at $100^{\circ}C$ and $150^{\circ}C$. The hydrothermal treatment was performed to the starting material via a modified direct aqueous carbonation process at the same leaching temperature. The initial pH of the solution was adjusted to 12 and $CO_2$ partial pressure was 1MPa for the carbonation. The carbonation rate after extracting $Ca^^{2+}$ under $NH_4NO_3$ was higher than that under $H_2SO_4$ and the carbonation rates in 1M $NH_4NO_3$ solution at $150^{\circ}C$ was dramatically enhanced about 93%. In this condition well-faceted rhombohedral calcite, and rod or flower-shaped aragonite were appeared together in products. As the concentration of $H_2SO_4$ increased, the formation of gypsum was predominant and the carbonation rate decreased sharply. Therefore it is considered that the selection of the leaching solution which does not affect the starting material is important in the carbonation reaction.

Electrochemical Properties of Using MnO2-HCS Composite for Supercapacitor (MnO2-HCS 복합체를 이용한 슈퍼커패시터의 전기화학적 특성)

  • Jin, En Mei;Jeong, Sang Mun
    • Clean Technology
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    • v.24 no.3
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    • pp.183-189
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    • 2018
  • Hollow carbon spheres (HCS) and carbon spheres (CS) were prepared by a hydrothermal reaction and they were introduced as a substrate for the deposition of $MnO_2$ nanoparticles. The $MnO_2$ nanoparticles were deposited on the carbon surface by a chemical redox deposition method. After deposition, the $MnO_2$ nanoparticles were uniformally distributed on the carbon surface in a slit-shape, and sparse $MnO_2$ slits appeared on the HCS surface. The $MnO_2-HCS$ showed an initial specific capacitance of $164.1F\;g^{-1}$ at scan rate of $20mv\;s^{-1}$, and after 1,000 cycles, the specific capacitance was maintained to $141.3F\;g^{-1}$. The capacity retention of $MnO_2-HCS$ and $MnO_2-CS$ were calculated to 86% and 78% in the cycle performance test up to 1,000 cycles, respectively. $MnO_2-HCS$ showed a good cycle stability due to the mesoporous hollow structure which can cause a faster diffusion of the electrolyte and can easily adsorb and desorb $Na^+$ ions on the surface of the electrode.

Synthesis of Prussian Blue Analogue and Magnetic and Adsorption Characteristics of MnFe2O4 (프러시안 블루 유사체의 합성 및 MnFe2O4의 자성과 흡착 특성)

  • Lee, Hye-In;Kang, Kuk-Hyoun;Lee, Dong-Kyu
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.1
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    • pp.67-74
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    • 2016
  • The Prussian Blue Analogue(PBA) has three dimensional structure and the metal - organic framework material, and it has a variety configurations depending on the type of organic ligands. PBA has been receving an attention in the fields of biosensors, optical, catalytic, and hydrogen storage device. Also, it is an environmental friendly substance with a chemical stability. In addition, PBA is widely used in the filed of adsorption art since we can adjust the size of the fine pores. In this study, we synthesized $Mn_3[Fe(CN)_6]_2$, an organometallic framework chains by using a hydrothermal synthesis method. We used $K_4[Fe(CN)_6]$ and $MnCl_2$ as precursors. We also produced a manganese iron oxide, by baking the synthesized material. The effect of the size and shape of the particles was examined by controling pH of the precursor solution, the molar concentration of the precursor, and reaction time as the experimental variables. Synthesized absorbent was analyzed by XRD, SEM, FT-IR, UV-Vis, and TG / DTA to evaluate the adsorption properties of several dyes.

Conversion of DME to Light Olefins over Mesoporous SAPO-34 Catalyst Prepared by Carbon Nanotube Template (탄소 나노튜브 주형물질에 의해 제조된 메조 세공 SAPO-34 촉매상에서 경질 올레핀으로의 DME 전환 반응)

  • Kang, Eun-Jee;Lee, Dong-Hee;Kim, Hyo-Sub;Choi, Ki-Hwan;Park, Chu-Sik;Kim, Young-Ho
    • Applied Chemistry for Engineering
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    • v.25 no.1
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    • pp.34-40
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    • 2014
  • Mesoporous SAPO-34 catalyst was successfully synthesized by the hydrothermal method using carbon nanotube (CNT) as a secondary template. The effects of CNT contents (0.5, 1.5, 2.5, and 4.5 mol%) on catalytic performances were investigated. The synthesized catalysts were characterized with XRD, SEM, nitrogen physisorption isotherm and $NH_3$-TPD. Among the synthesized catalysts, SAPO-34 catalyst prepared by the addition of 1.5 mol% CNT (1.5C-SAPO-34) observed not only the largest amounts of mesopore volume but also acid sites. However, the mesopore volume was relatively decreased by further increasing of CNT contents due to the formation of small crystalline. The catalytic lifetime and the selectivity of light olefins ($C_2{\sim}C_4$) were examined for the dimethyl ether to olefins reaction. As a result, the 1.5C-SAPO-34 catalyst showed an improvement of ca. 36% in a catalytic lifetime and a better selectivity to light olefins as compared with the general SAPO-34 catalyst.

Immobilization of As and Pb in Contaminated Soil Using Bead Type Amendment Prepared by Iron NanoparticlesImpregnated Biochar (철 나노 입자가 담지된 바이오차 기반 비드 형태 안정화제를 이용한 비소 및 납 오염토양의 안정화)

  • Choi, Yu-Lim;Kim, Dong-Su;Kang, Tae-Jun;Yang, Jae-Kyu;Chang, Yoon-Young
    • Journal of Environmental Impact Assessment
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    • v.30 no.4
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    • pp.247-257
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    • 2021
  • In this work, Iron Nano-Particles Impregnated BioChar/bead (INPBC/bead) soil amendment was developed to increase biochar's reactivity to As in soil and preventing possible wind loss. Prior to preparation of INPBC/bead, INPBC was produced utilizing lignocellulosic biomass and Fe(III) solution in a hydrothermal method, followed by a calcination process. Then, the bead type amendment, INPBC/bead was produced by cross-linking reaction of alginate with INPBC. FT-IR, XRD, BET, and SEM-EDS analyses were utilized to characterize the as-synthesised materials. The particle size range of INPBC/bead was 1-4 mm, and different oxygen-containing functional groups and Fe3O4 crystalline phase were produced on the surface of INPBC/bead, according to the characterization results. The soil cultivation test was carried out in order to assess the stabilization performance of INPBC/bead utilizing As and Pb-contaminated soil obtained from an abandoned mining location in South Korea. After 4 weeks of culture, TCLP and SPLP extraction tests were performed to assess the stabilization efficacy of the amendment. The TCLP and SPLP findings revealed that raising the application ratio improved stabilizing efficiency. The As stabilization efficiency was determined to be 81.56 % based on SPLP test findings for a 5% in (w/w) INPBC/bead treatment, and the content of Pb in extracts was reduced to the limit of detection. According to the findings of this study, INPBC/bead that can maintain pH of origin soil and minimize wind loss might be a potential amendment for soil polluted with As and heavy metals.

Effect of Carbon Dioxide Pressure on Mineral Carbonation in Acidic Solutions (산성용액에서 이산화탄소의 압력이 광물탄산화에 미치는 영향)

  • Ryu, Kyoung Won;Hong, Seok Jin;Choi, Sang Hoon
    • Economic and Environmental Geology
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    • v.53 no.1
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    • pp.1-9
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    • 2020
  • Magnesium silicate minerals such as serpentine [Mg3Si2O5(OH)4] have a high potential for the sequestration of CO2; thus, their reactivity toward dissolution under CO2-free and CO2-containing conditions in acidic solvents is a critical process with respect to their carbonation reactions. To examine the carbonation efficiency and dissolution mechanism of serpentine, hydrothermal treatment was performed to the starting material via a modified direct aqueous carbonation process at 100 and 150℃. The serpentine dissolution experiments were conducted in H2SO4 solution with concentration range of 0.3-1 M and at a CO2 partial pressure of 3 MPa. The initial pH of the solution was adjusted to 13 for the carbonation process. Under CO2-free and CO2-containing conditions, the carbonation efficiency increased in proportion to the concentration of H2SO4 and the reaction temperature. The leaching rate under CO2-containing conditions was higher than that under CO2-free conditions. This suggests that shows the presence of CO2 affects the carbonation reaction. The leaching and carbonation efficiencies at 150℃ in 1 M H2SO4 solution under CO2-containing conditions were 85 and 84%, respectively. The dissolution rate of Mg was higher than that of Si, such that the Mg : Si ratio of the reacted serpentine decreased from the inner part (approximately 1.5) to the outer part (less than 0.1). The resultant silica-rich layer of the reaction product ultimately changed through the Mg-depleted skeletal phase and the pseudo-serpentine phase to the amorphous silica phase. A passivating silica layer was not observed on the outer surface of the reacted serpentine.

Characterisitics of Redox Reaction of the Magnetite Powder Prepared by Hydrothermal Synthesis (수열합성법으로 합성된 마그네타이트 분말에 대한 산화.환원 특성)

  • Park, Sung Youl;Kang, Min Pil;Rhee, Young Woo;Nam, Sung Chan
    • Korean Chemical Engineering Research
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    • v.43 no.6
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    • pp.751-755
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    • 2005
  • Carbon dioxide, included in the flue gas from the combustion of fossil fuel, was known as a representative green house gas and various removal and utilization technologies of it has been studied for the prevention of global warming. This study was performed as an effort to find out a method to reuse carbon dioxide separated from flue gas by magnetite powder. Magnetite powder was synthesized using various oxidizers and alkalinity controlled aqueous solutions of $FeSO_4{\cdot}7H_2O$ and NaOH at 50, 80, 90, $100^{\circ}C$ and analyzed by XRD and SEM. The analysis results showed that magnetite powder synthesized at higher alkalinity and temperature had crystalline spinel and cubic structure. The reduction by hydrogen and the oxidation by carbon dioxide of synthesized powder were studied by TGA. The results showed that magnetite powder synthesized at low alkalinity and temperature was non-cubical amorphous but crystalline and cubical at high alkalinity and temperature. Comparing magnetite powders synthesized using oxidants(air and oxygen) and nitrogen, magnetite powder using more oxygen containing oxidant synthesized more crystalline magnetite powder. The experimental results of redox reaction of the synthesized magnetite powder showed that the reduction by hydrogen and the oxidation by carbon dioxide were seldom observed below $400^{\circ}C$ and observed well at $500^{\circ}C$. Magnetite powder synthesized at $100^{\circ}C$ and alkalinity(molal concentration ratio of $FeSO_4{\cdot}7H_2O$ to NaOH) of 2.0 using $O_2$ showed the highest reduction of 27.15 wt% and oxidation of 26.73 wt%, especially at reaction temperature of $500^{\circ}C$.

Glycerol Steam Reforming for Hydrogen Production on Metal-ceramic Core-shell CoAl2O4@Al Composite Structures (금속-세라믹 Core-Shell CoAl2O4@Al 구조체를 적용한 불균일계 촉매의 글리세롤 수소전환 반응특성)

  • Kim, Jieun;Lee, Doohwan
    • Clean Technology
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    • v.21 no.1
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    • pp.68-75
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    • 2015
  • In this study, we investigated the structure and properties of a highly heat conductive metal-ceramic core-shell CoAl2O4@Al micro-composite for heterogeneous catalysts support. The CoAl2O4@Al was prepared by hydrothermal surface oxidation of Al metal powder, which resulted in the structure with a high heat conductive Al metal core encapsulated by a high surface area CoAl2O4 shell. For comparison, CoAl2O4 was also prepared by co-precipitation method and also utilized for a catalyst support. Rh catalysts supported on CoAl2O4@Al and CoAl2O4 were prepared by incipient wetness impregnation and characterized by N2 adsorption, X-ray diffraction (XRD), scanning electron microscopy (SEM), CO chemisorption, and temperature-programmed reduction (TPR). The properties of catalysts were investigated for glycerol steam reforming reaction for hydrogen production at 550 ℃. Rh/CoAl2O4@Al exhibited about 2.8 times higher glycerol conversion turnover frequency (TOF) than Rh/CoAl2O4 due to facilitated heat transport through the core-shell structure. The CoAl2O4@Al and CoAl2O4 also showed some catalytic activities due to a partial reduction of Co on the support, and a higher catalytic activity was also found on the CoAl2O4@Al core-shell than CoAl2O4. These catalysts, however, displayed deactivation on the reaction stream due to carbon deposition on the catalysts surface.

Electrochemical Characteristics of LiMn2O4 Cathodes Synthesized from Various Precursors of Manganese Oxide and Manganese Hydroxide (다양한 형태 및 구조의 망간산화물 및 망간수산화물 전구체로부터 합성한 LiMn2O4양극의 전기화학적 특성 연구)

  • Lee, Jong-Moon;Kim, Joo-Seong;Hong, Soon-Kie;Lee, Jeong-Jin;Ahn, Han-Cheol;Cho, Won-Il;Mho, Sun-Il
    • Journal of the Korean Electrochemical Society
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    • v.15 no.3
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    • pp.172-180
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    • 2012
  • The $LiMn_2O_4$ cathodes for lithium ion battery were synthesized from various precursors of manganese oxides and manganese hydroxides. As the first step, nanosized precursors such as ${\alpha}-MnO_2$ (nano-sticks), ${\beta}-MnO_2$ (nano-rods), $Mn_3O_4$ (nano-octahedra), amorphous $MnO_2$(nano-spheres), and $Mn(OH)_2$ (nano-plates) were prepared by a hydrothermal or a precipitation method. Spinel $LiMn_2O_4$ with various sizes and shapes were finally synthesized by a solid-state reaction method from the manganese precursors and LiOH. Nano-sized (500 nm) octahedron $LiMn_2O_4$ showed high capacities of 107 mAh $g^{-1}$ and 99 mAh $g^{-1}$ at 1 C- and 50 C-rate, respectively. Three dimensional octahedral crystallites exhibit superior electrochemical characteristics to the other one-dimensional and two-dimensional shaped $LiMn_2O_4$ nanoparticles. After 500 consecutive charge discharge battery cycles at 10 C-rate with the nano-octahedron $LiMn_2O_4$ cathode, the capacity retention of 95% was observed, which is far better than any other morphologies studied in this work.