• Title/Summary/Keyword: DSC measurement

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Characterization of Zirconium Sulfate Supported on Zirconia and Activity for Acid Catalysis

  • Son, Jong Rak;Gwon, Tae Dong;Kim, Sang Bok
    • Bulletin of the Korean Chemical Society
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    • v.22 no.12
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    • pp.1309-1315
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    • 2001
  • Zirconium sulfate supported on zirconia catalysts were prepared by impregnation of powdered $Zr(OH)_4$ with zirconium sulfate aqueous solution followed by calcining in air at high temperature. The characterization of prepared catalysts was performed using Fourier transform infrared (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and by the measurement of surface area. The addition of zirconium sulfate to zirconia increased the phase transition temperature of $ZrO_2$ from amorphous to tetragonal due to the interaction between zirconium sulfate and zirconia, and the specific surface area and acidity of catalysts increased in proportion to the zirconium sulfate content up to 10 wt% of $Zr(SO_4)_2$. Infrared spectra of ammonia adsorbed on $Zr(SO_4)2}ZrO_2$ showed the presence of Bronsted and Lewis acid sites on the surface. $10-Zr(SO_4)_2}ZrO_2$ calcined at $600^{\circ}C$ exhibited maximum catalytic activities for 2-propanol dehydration and cumene dealkylation. The catalytic activities for both reactions were correlated with the acidity of catalysts measured by ammonia chemisorption method.

Evaluation of Hydrate Inhibition Performance of Water-soluble Polymers using Torque Measurement and Differential Scanning Calorimeter (토크 측정과 시차주사열량계를 이용한 수용성 고분자 화합물의 하이드레이트 저해 성능 평가)

  • Shin, Kyuchul;Park, Juwoon;Kim, Jakyung;Kim, Hyunho;Lee, Yohan;Seo, Yongwon;Seo, Yutaek
    • Korean Chemical Engineering Research
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    • v.52 no.6
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    • pp.814-820
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    • 2014
  • In this work, hydrate inhibition performance of water-soluble polymers including pyrrolidone, caprolactam, acrylamide types were evaluated using torque measurement and high pressure differential scanning calorimeter (HP ${\mu}$-DSC). The obtained experimental results suggest that the studied polymers represent the kinetic hydrate inhibition (KHI) performance. 0.5 wt% polyvinylcaprolactam (PVCap) solution shows the hydrate onset time of 34.4 min and subcooling temperature of 15.9 K, which is better KHI performance than that of pure water - hydrate onset time of 12.3 min and subcooling temperature of 6.0 K. 0.5 wt% polyvinylpyrrolidone (PVP) solution shows the hydrate onset time of 27.6 min and the subcooling temperature of 13.2 K while polyacrylamide-co-acrylic acid partial sodium salt (PAM-co-AA) solution shows less KHI performance than PVP solution at both 0.5 and 5.0 wt%. However, PAM-co-AA solution shows slow growth rate and low hydrate amount than PVCap. In addition to hydrate onset and growth condition, torque change with time was investigated as one of KHI evaluation methods. 0.5 wt% PVCap solution shows the lowest average torque of 6.4 N cm and 0.5 wt% PAM-co-AA solution shows the average torque of 7.2 N cm. For 0.5 wt% PVP solution, it increases 11.5 N cm and 5.0 wt% PAM-co-AA solution shows the maximum average torque of 13.4 N cm, which is similar to the average torque of pure water, 15.2 N cm. Judging from the experimental results obtained by both an autoclave and a HP ${\mu}$-DSC, the PVCap solution shows the best performance among the KHIs in terms of delaying hydrate nucleation. From these results, it can be concluded that the torque change with time is useful to identify the flow ability of tested solution, and the further research on the inhibition of hydrate formation can be approached in various aspects using a HP ${\mu}$-DSC.

Cure Behavior and Tensile Properties of Ethylidene Norbornene/endo-Dicyclopentadiene Blends (Ethylidene Norbornene/endo-Dicyclopentadiene 블렌드의 경화 거동 및 인장 특성)

  • Jung, Jong Ki;Choi, Jung Hwa;Yang, Guang;Park, Jongmoon;Kim, Donghak;Kim, Seonggil;Lee, Jong Keun;Oh, Myung-Hoon;Kim, Bongsuk;Bang, Daesuk
    • Polymer(Korea)
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    • v.39 no.3
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    • pp.506-513
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    • 2015
  • Ethylidene norbornene (ENB) and its blends with endo-dicyclopentadiene (endo-DCPD) were prepared and reacted via the ring-opening metathesis polymerization (ROMP) reaction with the $1^{st}$ and $2^{nd}$ generation Grubbs' catalysts. Dynamic exothermic behaviors during ROMP and tensile properties after ROMP were evaluated using a differential scanning calorimeter (DSC) and a universal testing machine (UTM) for the samples, respectively. It revealed that the ROMP rate was accelerated with the less contents of endo-DCPD and under the $2^{nd}$ generation catalyst. Also, the addition of endo-DCPD and the $1^{st}$ generation catalyst resulted in higher tensile modulus and strength but lower toughness. Gel fraction measurement and fracture surface observation were made to understand the tensile properties.

Study on Rheological Properties of HBA/HNA Thermotropic Liquid Crystalline Polymer (HBA/HNA계 열방성 액정고분자의 유변학적 특성에 관한 연구)

  • Son, Young-Gon
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.11 no.12
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    • pp.5216-5220
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    • 2010
  • Rheological measurement of a thermotropic liquid crystalline poymer (TLCP) is not an easy task since their rheological responses are strongly influenced by a thermal history during a processing and thus the reproducibility of the measurement is poor. In order to find out a cause for the strong influence of the thermal history, rheological measurements and DSC observations of the TLCP having various thermal histories were carried out. It was observed that the TLCP used in this study shows liquid-like behavior at a temperature above a crystal-nematic transition temperature ($280^{\circ}C$), but at the same time crystallization can occur at this temperature range and as a consequence the viscosity of the polymer continuously increases. When the samples are heated beyond the $320^{\circ}C$, all crystals thus formed and the thermal histories were observed to disappear. Crystallization rate of the samples annealed above $320^{\circ}C$ was very low at even the lowed temperature ($280^{\circ}C\;{\sim}\;320^{\circ}C$). Therefore, it is concluded that rheological measurements of TLCP used in this study must be performed after annealed above the nematic-isotropic transition temperature for better reproducibility.

Synthesis of (Ni,Mg)Al2O4 Ceramic Nano Pigment by a Polymerized Complex Method (착체중합법을 이용한 (Ni,Mg)Al2O4 Cyan 나노 무기안료 합성)

  • Son, Bo-Ram;Yoon, Dea-Ho;Han, Kyu-Sung;Cho, Woo-Suk;Hwang, Kwang-Taek;Kim, Jin-Ho
    • Journal of the Korean Ceramic Society
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    • v.50 no.3
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    • pp.195-200
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    • 2013
  • Here, we report preparation of cyan ceramic nano-pigment for inkjet printing and the Ni substitutional effects on the cyan color. $MgAl_2O_4$ was selected as the crystalline host network for the synthesis of nickel-based cyan ceramic nano-pigments. Various compositions of $Ni_xMg_{1-x}Al_2O_4$ ($0{\leq}x{\leq}1$) powders were prepared using the polymerized complex method. The powder was then preheated at $400^{\circ}C$ for 5 h and finally calcined at $1000^{\circ}C$ for 5 h. XRD patterns of $Ni_xMg_{1-x}Al_2O_4$ showed a single phase of the spinel structure in all the compositions. The particle sizes ranged from 20 to 50 nm in TEM observations. The characteristics of the color tones of $Ni_xMg_{1-x}Al_2O_4$ were analyzed by UV-Visible spectroscopy and CIE $L^*a^*b^*$ measurement. CIE $L^*a^*b^*$ measurement results indicate that the pigment color changes from light cyan to deep cyan due to the decrease of the $a^*$ and $b^*$ values with an increase of an Ni substitutional amount. In addition, the thermal stability and the binding nature of $Ni_xMg_{1-x}Al_2O_4$ are also discussed using TG-DSC and FT-IR results respectively.

The Variation of Microstructures and Mechanical Properties by Thermomechanical Treatment in Al-Li Based Alloys (AI-Li제 합금의 가공열처리에 따른 조직과 기계적성질의 변화)

  • Kim, Ki Won;Woo, Kee Do;Lee, Kwang Ro;Lee, Min Sang;Lee, Min Ho;Hwang, Ho Eul
    • Journal of the Korean Society for Heat Treatment
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    • v.4 no.3
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    • pp.13-20
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    • 1991
  • The present work was aimed to examine the variation of precipitations and mechanical properties by thermomechanical treatments (TMT) in Al-2.19 wt%Li and Al-2.0 wt%Li-0.11 wt%Zr alloys. This study was performed by TEM, SEM observation, DSC, electrical resistance measurement, hardness and tensile strength measurement. First peak of resistivity aged at $90^{\circ}C$ was caused by precipitation of ${\delta}^{\prime}$-precursor phase, and second peak was caused by precipitation of ${\delta}^{\prime}$ phase. According to this result, the precipitation process of Al-2.19 wt%Li alloy was as follow : $SSSS{\rightarrow}{\delta}^{\prime}$-precursor phase ${\rightarrow}{\delta}^{\prime}$ (Coherent ${\rightarrow}$ Semi-coherent) ${\rightarrow}{\delta}$. In a Al-2.0 wt%Li-0.11 wt%Zr ternary alloy, the first peak of resistivity was appeared at initial aging heat-treatment. It is result from exsistant of ${\delta}^{\prime}$-precursor phase. The effect acceleration in a binary alloy was not appeared and the over-aging ternary alloy was accelerated with increase of the reduction rate. It is caused by combination effect of ${\delta}^{\prime}$ and composite phase.

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Preparation of Poly(vinylidene fluoride)-g-poly(methacrylic acid) Composite Nanofiltration Membrane

  • Kim, Yong-Woo;Choi, Jin-Kyu;Koh, Joo-Hwan;Kim, Jong-Hak
    • Korean Membrane Journal
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    • v.9 no.1
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    • pp.57-63
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    • 2007
  • Amphiphilic graft copolymer from poly(vinylidene fluoride) (PVDF) was synthesized using atom transfer radical polymerization (ATRP) for composite nanofiltration membranes. Direct initiation of the secondary fluorinated site of PVDF facilitates grafting of tert-butyl methacrylate (tBMA). Amphiphilic PVDF-g-PMAA graft copolymer with a 51:49 wt ratio was obtained by hydrolyzing poly(tert-butyl methacrylate) (PtBMA) to poly(methacrylic acid) (PMAA). Wide angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC) confirmed the decrease of crystallinity of PVDF upon graft copolymerization. Composite nanofiltration membranes were prepared from PVDF-g-PMAA as a top layer coated onto PVDF ultrafiltration (UF) support membrane. The morphology and hydrophilicity of membranes were characterized using scanning electron microscopy (SEM) and contact angle measurement. The rejections of composite membranes were 80.2% for $Na_2SO_4$ and 28.4% for NaCl, and the solution flux were 9.5 and $14.5\;L/m^2\;h$ at 1.0 MPa pressure.

P(3HB) Accumulation in Alcaligenes eutrophus H16(ATCC 17699) under Nutrient-Rich Condition and Its Induced Production from Saccharides and Their Derivatives

  • Song, Jae-Jun;Shin, Yong-Chul
    • Journal of Microbiology and Biotechnology
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    • v.3 no.2
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    • pp.115-122
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    • 1993
  • Poly(3-hydroxybutyrate)(P(3HB)) accumulation under nutrient-rich condition with various amounts of $(NH_4)_2 SO_4$ was systematically investigated. The results of the electron-microscopy and the solvent extraction showed that the P(3HB) accumulation is unavoidable even under nutrient-rich condition. This indicates that in a two-step culture of Alcaligenes eutrophus H16, the researches should be careful in interpreting the data of polyhydroxyalkanoates(PHAs) accumulation in terms of the carbon-source fed in the second step because the two-step culture product contains the P(3HB) produced under nutrient-rich condition. The polyester production capability in a two-step batch culture of A. eutrophus H16(ATCC 17699) was also investigated using various saccharides and their derivatives such as glucose, fructose, gluconic acid, glucaric acid, sorbitol, lactose, galactose, and mannose. The polyesters synthesized were characterized by 500 MHz$^{1}H-NMR$ spectroscopy, intrinsic viscosity$[\eta]$ measurement in chloroform and differential scanning calorimetry(DSC). 500 MHz $^{1}H-NMR$ analysis showed that all polyesters synthesized generally contained 1~2 mol% of 3HV. Another finding is that the glucose utilization can be increased by changing the autoclaving procedure of the substrate to enhance the P(3HB) production yield up to 46 wt% of P(3HB) in dry cells.

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Characteristics Analysis of Nano-composites Films Using Extruder (압출성형기를 이용한 나노복합재 필름의 특성 분석)

  • Kwon, Il-Jun;Park, Sung-Min;Yoo, Sung-Hun;Yeum, Jeong-Hyun
    • Textile Coloration and Finishing
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    • v.28 no.2
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    • pp.101-108
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    • 2016
  • Polypropylene(PP)/multiwalled carbon nanotubes(MWCNT) nanocomposites films and PP/poly(vinyl alcohol)/CNT nanocomposites films were prepared through melt mixing method by the extruder. The PP/CNT nanocomposites films, which contain CNT of a variable content, were prepared for the first time and research on a appropriate content of the CNT on the PP/CNT nanocomposites films was conducted. The effects of take-up speed of the extruder on the mechanical and chemical properties of the PP/CNT and PP/PVA/CNT nanocomposites film were studied. Field emission scanning electron microscope(FE-SEM) was used to examine the surface morphology and the DSC measurement and tensile test were conducted. It was found that the properties decreased when take-up speed was increased.

Quality Characteristics of Mokwapyun Containing Various Amount of Tapioca Starch (타피오카 전분을 첨가한 모과편의 품질 특성)

  • Kim, Ga-Hyun;Park, Geum-Soon
    • Journal of the East Asian Society of Dietary Life
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    • v.23 no.4
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    • pp.444-450
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    • 2013
  • The purpose of this study is to evaluate chemical properties, textural characteristics and sensory properties which produces the mokwapyun from the tapioca starch. The mokwapyun-added tapioca starches hold higher moisture contents than mung bean starches. And, the ratios of tapioca starch indicate differences in the study (p<.001). The pH increases with the increasing amounts of tapioca starch and acidity measurement decreases as amount of tapioca starch increases. The 0% addition of tapioca starch is the highest for lightness and 20% addition of tapioca starch is the lowest. Both the redness and yellowness are being increased with increases in the addition of tapioca starch. According to the results of texture, 0% addition of tapioca starch is the highest for hardness, springiness and chewiness of mokwapyun which increases with additional percentages of tapioca starch. Nevertheless, it decreases the cohesiveness and brittleness due to increases in the percentage of tapioca starch. According to the result of DSC analysis, the more tapioca starch added to the mokwapyun, the higher the To, Tp, Tc temperatures become. The result of this study shows that the right contents of tapioca starch with 15% additions make positive acceptability, prepared sensory and machinery characteristics.