• Title/Summary/Keyword: Low temperature synthesis

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Formation of Layered Bi5Ti3FeO15 Perovskite in Bi2O3-TiO2-Fe2O3 Containing System

  • Borse, Pramod H.;Yoon, Sang-Su;Jang, Jum-Suk;Lee, Jae-Sung;Hong, Tae-Eun;Jeong, Euh-Duck;Won, Mi-Sook;Jung, Ok-Sang;Shim, Yoon-Bo;Kim, Hyun-Gyu
    • Bulletin of the Korean Chemical Society
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    • v.30 no.12
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    • pp.3011-3015
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    • 2009
  • Structural and thermo-analytical studies were carried out to understand the phase formation kinetics of the single phase $Bi_5Ti_3FeO_{15}$ (BTFO) nanocrystals in $Bi_2O_3-Fe_2O_3-TiO_2$, during the polymerized complex (PC) synthesis method. The crystallization of Aurivillius phase $Bi_5Ti_3FeO_{15}$ layered perovskite was found to be initiated and achieved under the temperature conditions in the range of ${\sim}$800 to 1050$^{\circ}C$. The activation energy for grain growth of $Bi_5Ti_3FeO_{15}$ nanocrystals (NCs) was very low in case of NCs formed by PC (2.61 kJ/mol) than that formed by the solid state reaction (SSR) method (10.9 kJ/mol). The energy involved in the phase transformation of Aurivillius phase $Bi_5Ti_3FeO_{15}$ from $Bi_2O_3-Fe_2O_3-TiO_2$ system was ${\sim}$ 69.8 kJ/mol. The formation kinetics study of $Bi_5Ti_3FeO_{15}$ synthesized by SSR and PC methods would not only render a large impact in the nanocrystalline material development but also in achieving highly efficient visible photocatalysts.

The Study on Thermal Analysis and Thermodynamic Characteristics of Spinel Compounds(ZnCo2O4, NiCo2O4) (스피넬 구조를 가지는 전이금속화합물(ZnCo2O4, NiCo2O4)의 열적 분석 및 열역학적 특성 연구)

  • Kim, Jae-Uk;Ji, Myoung-Jin;Cha, Byung-Kwan;Kim, Chul-Hyun;Jang, Won-Cheoul;Kim, Jong-Gyu
    • Journal of the Korean Chemical Society
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    • v.54 no.2
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    • pp.192-197
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    • 2010
  • The spinel compound was obtained by the thermal decomposition of Zn-Co and Zn-Ni gel prepared by sol-gel method using oxalic acid as a chelating agent. The formation of spinel compound has been comfirmed by thermogravimetric analysis (TGA), x-ray powder diffraction (XRD) and infrared spectroscopy (IR). The particle size of 13 nm~16 nm was calculated by Scherrer's equation. The sol-gel method provides a practicable and effective route for the synthesis of the spinel compound at low temperature ($350^{\circ}C$). The kinetic parameters such as activation energy (Ea) and pre-exponential factor (A) for each compound were found by means of the Kissinger method and Arrhenius equation. The decomposition of spinel compound has an activation energy about 155 kJ/mol. Finally, the thermodynamic parameters (${\Delta}G^{\varphi}$, ${\Delta}H^{\varphi}$, ${\Delta}S^{\varphi}$) for decomposition of spinel compound was determined.

CO2 decomposition characteristics of Ni-ferrite powder (Ni-페라이트 분말을 이용한 CO2 분해 특성)

  • Nam, Sung-Chan;Yoon, Yeo-Il
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.12 no.11
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    • pp.5376-5383
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    • 2011
  • The objective of this study is the development of carbon-recycle technology, that converts carbon dioxide captured from flue gas to carbon monoxide or carbon for reuse in industrial fields. It is difficult to decompose $CO_2$ because $CO_2$ is very stable molecule. And then metal oxide was used as an activation agent or catalyst for the decomposition of $CO_2$ at low temperature. Metal oxides, which converts $CO_2$ to CO or C, were prepared using Ni-ferrite by solid state method and hydrothermal synthesis in this study. TPR/TPO and TGA were used as an analysis method to analyze the decomposition characteristics of $CO_2$. As the results, the reduction area of $H_2$ was high value at 15 wt% of NiO and the decomposition area of $CO_2$ was superior capacity at 5 wt% of NiO. However, TGA data showed contrary results that reduction area of $H_2$ was 28.47wt% and oxidation area by $CO_2$ was 26.95wt% at 2.5 wt% of NiO, one of the Ni-ferrite powders synthesized using solid state method. $CO_2$ decomposition efficiency was 94.66% and it is excellent results in comparison with previous studies.

CO2 decomposition characteristics of Ba-ferrite powder (Ba-페라이트 분말을 이용한 이산화탄소 분해 특성)

  • Nam, Sung-Chan;Park, Sung-Youl;Jeon, Soon-Kwan;Yoon, Yeo-Il
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.12 no.11
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    • pp.5357-5364
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    • 2011
  • The objective of this study is development of carbon recycle technology which convert carbon dioxide captured from flue gas to carbon monoxide or carbon and reuse in industrial fields. Since carbon dioxide is very stable and difficult to decompose, metal oxide was used as activation agent for the decomposition of carbon dioxide at low temperature. Metal oxides which convert $CO_2$ to CO or carbon were prepared using Ba-ferrite by solid and hydrothermal synthesis. TPR/TPO and TGA were used in this study. The results of TPR by H2 and TPO by $CO_2$ showed that Ba-ferrite powders synthesized by hydrothermal method were better than those by solid method. TGA showed contrary results that reduction of Ba-ferrite powders synthesized using solid method by $H_2$ was 21.96 wt%, oxidation by $CO_2$ was 21.24 wt% and 96.72 wt% of $CO_2$ decomposition efficiency showing excellent oxidation-reduction characteristics at $500^{\circ}C$.

Photocatalytic Decomposition of Rhodamine B over BiVO4 Doped with Samarium Ion (Sm 이온이 도핑된 BiVO4에서 로다민 B의 광촉매 분해 반응)

  • Hong, Seong-Soo
    • Clean Technology
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    • v.27 no.2
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    • pp.146-151
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    • 2021
  • Pure and Sm ion doped BiVO4 catalysts were synthesized using a conventional hydrothermal method and characterized by XRD, DRS, SEM, and PL. We also examined the activity of these materials on the photocatalytic decomposition of rhodamine B under visible light irradiation. The doping of Sm ion into BiVO4 catalyst changed the ms-BiVO4 crystal structure into the tz-BiVO4 crystal structure in the low synthesis temperature. Light absorption analysis using DRS showed that all the catalysts displayed strong absorption in the visible range of the electromagnetic spectrum regardless of Sm ion doping. In addition, an amorphous morphology was shown in the pure BiVO4 catalyst, but the morphology of the BiVO4 catalyst doped with Sm ion was changed into an ellipse shape and also the particle size decreased. In the photocatalytic decomposition of rhodamine B, Sm ion doped BiVO4 catalyst showed higher photocatalytic activity than the pure BiVO4 catalyst. In addition, the Sm3-BVO catalyst doped with 3% Sm ion showed the highest photocatalytic activity, as well as the highest formation rate of OH radicals (•OH) and the highest PL peak. This result suggests that the formation rate of OH radicals produced in the interface between the photocatalyst and water is well correlated with the photocatalytic activity.

Synthesis and Characterization of Collagen Peptide Based Copolymer from Shaving Scrap (셰이빙 스크랩으로부터 콜라겐 펩타이드계 공중합체 합성과 특성)

  • Park, Min Seok;Shin, Soo Beom;Kim, Ho Soo;Kim, Min Soo;Kim, Ha Sun;Jang, Jae Hyeok;Lee, Jin Kye;Lee, Dong Kuk
    • Applied Chemistry for Engineering
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    • v.33 no.6
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    • pp.581-587
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    • 2022
  • The leather industry generates a large amount of hazardous leather waste of various types every year. Among them, shaving scrap is difficult to recycle because it contains chromium ions. Many studies in recent years have shown that shaving scraps can be processed into various types of valuable products, such as adsorbent, filler, and poultry feed. In this study, collagen peptides were extracted from shaving scraps and structurally modified to be developed as new materials with improved physicochemical properties. First, the chromium ions contained in the shaving scraps were removed using a sodium hydroxide solution, and purified through concentration and low-temperature crystallization. The purified collagen peptide was used to prepare the powder using a spray dryer. The extracted collagen peptides were structurally modified by introducing double bonds by reacting with methacrylic anhydride (MAA), and the product was confirmed by 1H NMR spectroscopy. Next, a copolymer was prepared by redox polymerization of the modified collagen peptide (MCP) and 2-ethylhexyl acrylate (2-EHA). The structure of the copolymer was qualitatively confirmed by FT-IR. In conclusion, this study confirmed that collagen peptides can be extracted from shaving scrap and converted into new eco-friendly materials through certain treatments.

Changes of Isoflavone Contents During Maturation under Different Planting Dates in Black Soybean (파종기 차이에 따른 등숙기간 중 검정콩의 아이소플라본 함량 변화)

  • Yi, Eun-Seob;Yoon, Seong-Tak
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.57 no.4
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    • pp.424-429
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    • 2012
  • This study was carried out to investigate the influence of different planting time on the synthesis of isoflavone in black soybean, Three varieties used in this experiment were lpumgeomjeongkong, Cheongjakong and Heugcheongkong which had different ecotypes, repectively. Seeds were sown at different time, May 15th, May 30th and June 15th with planting density of $60{\times}15cm$. In order to analyze the content of isoflavone, we collected sample every 5 days from 30 days after flowering to harvest and analyzed them with UPLC. As sowing was delayed, the content of isoflavone increased in all of three varieties. The content of genistein was greater than daidzein and glycitein. Increase of Glycitein was not distinct from 55 days after flowering(DAF) and it was stable against temperature change during the seed developing period. Although the content of genistein in Ilpumgeomjeongkong from 50 to 55 DAF, in Cheongjakong from 40 to 55 DAF and in Heugcheongkong from 60 to 65 DAF was lower than the content of daidzein, it was higher than that of daidzein afterward. In the statistical analysis on the relationship between average temperature and the content of aglycone isoflavone at 5-day intervals from 30 DAF during the grain filling period, genistein in Ilpumgeomjeongkong showed meaningful correlation as y=-15.28x+407.9 ($R^2=0.505^*$), diadzein in Cheongjakong showed meaningful correlation as y=-6.188x-164.5($R^2=0.454^*$), and genistein showed significantly high correlation as y=-11.59x+297.6 ($R^2=0.545^{**}$). Taking all the above results into consideration, it was suggested that the regions suitable for high content of isoflavone in black soybean be the northern area of Gyeonggi-do and Gangwon-do, Chungcheongbuk-do and inland area of Gyeongsangbuk-do, where are relatively low average temperature from flowering stage($R_2$) during the grain filling period.

Characterization of a Psychrophilic Metagenome Esterase EM2L8 and Production of a Chiral Intermediate for Hyperlipemia Drug (메타게놈유래의 저온성 에스터라제 EM2L8의 효소적 특성과 이를 활용한 고지혈증 치료제 키랄소재의 생산)

  • Jung, Ji-Hye;Choi, Yun-Hee;Lee, Jung-Hyun;Kim, Hyung-Kwoun
    • Microbiology and Biotechnology Letters
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    • v.37 no.2
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    • pp.118-124
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    • 2009
  • Esterase EM2L8 gene isolated from deep sea sediment was expressed in Escherichia coli BL21 (DE3) and the esterase activity of the cell-free extract was assayed using p-nitrophenyl butyrate-spectrophotometric method. Its optimum temperature was $40-45^{\circ}C$ and 45% activity of the maximum activity was retained at $15^{\circ}C$. The activation energy at $15-45^{\circ}C$ was calculated to be 4.9 kcal/mol showing that esterase EM2L8 was a typical cold-adapted enzyme. Enzyme activity was maintained for 6 h and 4 weeks at $30^{\circ}C$ and $4^{\circ}C$, respectively. When each ethanol, methanol, and acetone was added to the reaction mixture to 15% concentration, enzyme activity was maintained. In the case of DMSO, enzyme activity was kept up to 40% concentration. (S)-4-Chloro-3-hydroxy butyric acid is a chiral intermediate for the synthesis of Atorvastatin, a hyperlipemia drug. When esterase EM2L8 (40 U) was added to buffer solution (1.2 mL, pH 9.0) containing ethyl-(R,S)-4-chloro-3-hydroxybutyrate (38 mM), it was hydrolyzed into 4-chloro-3-hydroxy butyric acid with a rate of $6.8\;{\mu}mole/h$. The enzyme hydrolyzed (S)-substrate more rapidly than (R)-substrate. When conversion yield was 80%, e.e.s value was 40%. When DMSO was added, hydrolysis rate increased to $10.4\;{\mu}mole/h$. The plots of conversion yield vs e.e.s in the presence or absence of DMSO were almost same, implying that the reaction enantioselectivity was not changed by the addition of DMSO. Taken together, esterase EM2L8 had high activity and stability at low temperatures as well as in various organic solvents/aqueous solutions. These properties suggested that it could be used as a biocatalyst in the synthesis of useful pharmaceuticals.

On the Utilization of Inactive BHC isomers -Synthesis of 3-(2,4,5-trichlorophenyl)-1-methyl urea as a herbicide- (BHC 이성질체(異性質體)의 활용(活用)에 관(關)한 연구(硏究) -제초제(除草劑)로서 3-(2,4,5-trichlorophenyl)-1- methyl urea의 합성(合成)-)

  • Lee, Kyu-Seung;Park, Chang-Kyu
    • Applied Biological Chemistry
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    • v.22 no.2
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    • pp.109-122
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    • 1979
  • Present study was carried out to reduce residual toxicity of BHC insecticides inherent in the organochlorine pesticides. For This end, r-isomer, the most potent insecticidal component among the BHC stereoisomers, was isolated and thus fortified by means of solvent precipitation. In parallel, 3-(2,4,5-trichlorophenyl)-1-methyl urea was prepared in good yield from technical BHC via 1,2,4-trichlorobenzene, 1,2,4,-trichloronitrobenzene, and 2,4,5-trichloroaniline. In addition, certain merit of the compound which make it possible to use as a herbicide is discussed. The results are summarized as follows; 1. Recrystallizing technical BHC from methanol-water binary solvent system, r-isomer was enriched to 49.7% at 95% recovery of r-isomer. 2. By partitioning technical BHC in 85% of methanolic solution into chloroform, r-isomer was fortified to 89.6% at 90.5% recovery of r-isomer. 3. Yield of 1,2,4-trichlorobenzene from technical BHC was greatly dependent upon concentration of alkalies and to less degree on the alkalies. 4. Surfactants, in particular cationic a quartenary ammonium salt, increased yield of 1,2,4-trichlorobenzene from technical BHC by alkaline hydrolysis. 5. Conversion of 1,2,4-trichlorobenzene to 2,4,5-trichloronitrobenzene was effected almost quantitatively utilizing $HNO_3-H_2SO_4$ nitrating agent at low temperature. 6. Yield of 91.4% was observed for the synthesis of 2,4,5-trichloroaniline by reducing 2,4,5-trichloronitrobenzene in the presence of iron turning and hydrochloric acid. 7. Overall yield based on BHC of 3-(2,4,5-trichlorophenyl)-1- methyl urea was 60.8%. 8. Inhibition effects, both germination and growth, 3-(2,4,5-trichlorophenyl)-1-methyl urea on several crops were found comparable to or more potent than those of $linuron{\circledR}\;and\;diuron{\circledR}$. In addition, it was also noted that susceptibility to the prepared compound depended upon the crops as well as specific part (shoots, roots) of the plant exposed to the chemicals.

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A Study on the Adsorption and Desorption Characteristics of Metal-Impregnated Activated Carbons with Metal Precursors for the Regeneration and Concentration of Ammonia (암모니아의 재생 및 농축을 위한 금속 전구체에 따른 금속 첨착 활성탄의 흡착 및 탈착 특성에 관한 연구)

  • Cho, Gwang Hee;Park, Ji Hye;Rasheed, Haroon Ur;Yoon, Hyung Chul;Yi, Kwang Bok
    • Clean Technology
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    • v.26 no.2
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    • pp.137-144
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    • 2020
  • Metal-impregnated activated carbons were prepared via ultrasonic-assisted impregnation method for regeneration and low ammonia concentration. Magnesium and copper were selected as metals, while chloride (Cl-) and nitrate (NO3-) precursors were used to impregnate the surface of activated carbon. The physical and chemical properties of the prepared adsorbents were characterized by TGA, BET, and NH3-TPD. The ammonia breakthrough test was carried out using a fixed bed and flowing ammonia gas (1000 mg L-1 NH3, balanced N2) at 100 mL min-1, under conditions of temperature swing adsorption (TSA) and pressure swing adsorption (PSA, 0.3, 0.5, 0.7, 0.9 Mpa). The adsorption and desorption performance of ammonia were in the order of AC-Mg(Cl) > AC-Cu(Cl) > AC-Mg(N) > AC-Cu(N) > AC through NH3-TPD and TSA and PSA processes. AC-Mg(Cl) using MgCl2 showed the average adsorption amount of 2.138 mmol/g at TSA process. Also, AC-Mg(Cl) showed the highest initial adsorption amount of 3.848 mmol/g at PSA 0.9 Mpa. When metal impregnated the surface of the activated carbon, it was confirmed that not only physical adsorption, but also chemical adsorption increased, making enhancement in adsorption and desorption performances possible. Also, the prepared adsorbents showed stable adsorption and desorption performances despite repeated processes, confirming their applicability in the TSA and PSA processes.