• Title/Summary/Keyword: Thermogravimetric Analysis

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Preparation and characterization of boron-nitrogen coordination phenol resin/SiO2 nanocomposites

  • Gao, J.G.;Zhai, D.;Wu, W.H.
    • Advances in materials Research
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    • v.3 no.1
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    • pp.259-269
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    • 2014
  • The boron-nitrogen-containing phenol-formaldehyde resin (BNPFR)/$SiO_2$ nanocomposites (BNPFR/$SiO_2$) were synthesized in-situ, and structure of BNPFR/$SiO_2$ nanocomposites was characterized by FTIR, XRD and TEM. The loss modulus peak temperature $T_p$ of BNPFR/$SiO_2$ nanocomposites cured with different nano-$SiO_2$ content are determined by torsional braid analysis (TBA). The thermal degradation kinetics was investigated by thermogravimetric analysis (TGA). The results show that nano-$SiO_2$ particulate with about 50 nm diameter has a more uniformly distribution in the samples. The loss modulus peak temperature $T_p$ of BNPFR/$SiO_2$ nanocomposite is $214^{\circ}C$ when nano-$SiO_2$ content is 6 wt%. The start thermal degradation temperature $T_{di}$ is higher about $30^{\circ}C$ than pure BNPFR. The residual rate (%) of nanocomposites at $800^{\circ}C$ is above 40 % when nano-$SiO_2$ content is 9 %. The thermal degradation process is multistage decomposition and following first order.

Preparation and Thermal-property Analysis of Heat Storage Concrete with SSPCM for Energy Saving in Buildings (축열 성능 향상 SSPCM 혼합 콘크리트 제조 및 열적특성 분석)

  • Jeong, Su-Gwang;Chang, Seong Jin;Lim, Jae-Han;Kim, Hee-Sun;Ryu, Seong-Ryong;Kim, Sumin
    • Journal of the Korean Solar Energy Society
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    • v.35 no.1
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    • pp.89-96
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    • 2015
  • n-octadecnae based shape stabilized phase change material (SSPCM) was prepared by using vacuum impregnation method. And an exfoliated graphite nanoplate (xGnP) which has high thermal conductivity properties is used as a PCM container. And then we made heat storage concretes which contains SSPCM for reducing heating and cooling load in buildings. In the prepararion process, the SSPCM was mixed to a concrete as 10, 20 and 30wt% of cement weight. The thermal properties and chemical properties of heat storage concrete were analyzed from Scanning electron microscope (SEM), Fourier transformation infrared spectrophotometer (FT-IR), Deferential scanning calorimeter (DSC), Thermogravimetric analysis (TGA) and TCi thermal conductivity analyzer. And we conducted surface temperature analysis of SSPCM and xGnP by using heat plate and insulation mold.

Flame Retardant Properties of Cotton Fiber with Phosphoric/citric Acid Catalysts and TiO2 (인산/구연산 복합 산촉매 및 이산화티타늄을 적용한 면섬유의 난연 특성)

  • Yang, Heejin;Kim, Samsoo;Lee, Sangoh;Lee, Jaewoong
    • Textile Coloration and Finishing
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    • v.33 no.4
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    • pp.238-249
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    • 2021
  • In this study, the effect on flame retardancy and various physical properties when TiO2 was added with a citric acid/phosphate complex acid catalyst together with Pyrovatex CP new (N-methylol dimethylphosphonopropionamide), a phosphorus-based flame retardant, was studied on cotton fibers. SEM-EDS analysis was performed to confirm the surface characteristics and surface element analysis of the flame-retardant treated cotton fibers, and a vertical carbonization test was performed to confirm the char formation capability and flame retardancy according to the phosphoric acid ratio. By comparing the LOI index before and after washing 10 times, the washing durability of the flame retardant solution containing the phosphoric acid catalyst and TiO2 was tested by LOI index after ten washing cycles. In addition, the influence of the flame-retardant processing on the physical properties were compared including thermogravimetric analysis (TGA), tear strength and whiteness.

Addition Polymerization of 5-Norbornene-2-carboxylic Acid Esters Using Palladium Catalyst System: Synthesis of Monomers, Effect of Their Stereochemistry on Polymerization Behavior (Palladium 촉매를 이용한 5-Norbornene-2-carboxylic Acid Esters의 부가 중합: 단량체의 합성, 단량체의 Stereochemistry(Endo-, Exo-이성질체)가 고분자의 중합 거동에 미치는 영향)

  • Chung, Hae-Kang;Shim, Hyoug-Sub;Jeon, Seung-Ho;Kim, Ji-Heung;Nam, Sung Woo;Jeon, Boong Soo;Kim, Young Jun
    • Polymer(Korea)
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    • v.39 no.3
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    • pp.487-492
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    • 2015
  • The effects of chemical structure of alkyl groups of norbornene carboxylic alkyl esters(methyl, octyl, 4-chlorobenzyl) and endo/exo ratios of norbornene monomers on activity of palladium catalyst and polymerization behavior were investigated. Norbornene ester monomers were synthesized from the reaction of 5-norborene-2-carboxylic acid and various alcohols. Polymerization catalyst, di-${\mu}$-chloro-bis(-methoxybicyclo[2,2,1]-hept-2-ene)palladium(II) (DCBMP), was synthesized according to the literature procedure and silver hexafluoroantimonate ($AgSbF_6$) was used as a conjugate anion source. Gel permeation chromatography (GPC), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) were the principal techniques for polymer characterization and $^1H$ NMR spectroscopy was used for chemical structures determination of monomers and polymers. For all of the norbonene alkyl esters GPC data showed that when the amounts of endo isomers exceeded those of exo isomers decreased molecular weight polymers were obtained probably due to the decreased catalyst activity. Polymerizations were conducted by varying the monomer/catalyst mole ratios (100:1, 200:1, 300:1). When 300:1 monomer/catalyst ratio was employed it was possible to synthesize high molecular weight ($M_n=27500g/mol$), film forming polymer from exo-norbornene carboxylic acid octyl ester.

Characterization of Thermal Degradation of Polymide 66 Composite: Relationship between Lifetime Prediction and Activation Energy (폴리아미드 66 복합소재의 열 열화 특성: 수명 예측과 활성화 에너지의 상관관계)

  • Jung, Won-Young;Weon, Jong-Il
    • Polymer(Korea)
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    • v.36 no.6
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    • pp.712-720
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    • 2012
  • Thermal degradation for glass fiber-reinforced polyamide 66 composite (PA 66) with respect of thermal exposure time has been investigated using optical microscopy, scanning electron microscopy and Fourier transform infrared spectroscopy. As the thermal exposure time was prolonged, a slight increase in tensile strength for only initial stage and afterward, a proportional decrease of tensile strength was observed. These results can be explained by the increase of crystallinity, followed by the increase of crosslinking density, chain scission and the decrease in chain mobility, due to thermal oxidation with the exposure time. Fourier transform infrared spectroscopy results showed the increase of ketone peak and silica peak on the surface of thermally exposed PA 66. In addition, the thermal decomposition kinetics of PA 66 was analyzed using thermogravimetric analysis at three different heating rates. The relationship between activation energy and lifetime-prediction of PA 66 was investigated by several methodologies, such as statistical tool, UL 746B, Ozawa and Kissinger. The activation energy determined by thermogravimetric analysis had a relatively large value compared with that from the accelerated test. This may result in over-estimating the lifetime of PA 66. In this study, a master curve of exponential fitting has been developed to extrapolate the activation energy at various service temperatures.

A Study on Analysis of Characteristics Combustion of Floor Covering Materials (바닥내장재의 연소특성 분석에 관한 연구)

  • Park, Young-Ju;Lee, Hae-Pyeong;Kim, Hyun-Ju
    • Journal of the Korean Society of Hazard Mitigation
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    • v.10 no.3
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    • pp.77-83
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    • 2010
  • In this study, we analyzed the combustion characteristics of four different floor covering materials(wood, monorium, laminatedpaper, and varnish-laminated paper) with regard to their ignitibility, thermal characteristics and flame retardancy by using an ignition temperature tester, a dual cone calorimeter, a thermogravimetric analyzer and limited oxygen index, for their fire risk assessment. According to the result, monorium had the lowest ignition temperature of $325^{\circ}C$ and the laminated paper and the varnish-laminated paper promptly ignited before 7s. Further, the wood showed the largest total heat release of $100MJ/m^2$, and the varnish-laminated paper showed the highest peak heat release rate. From the thermogravimetric analysis, it was shown that all specimens underwent rapid weight loss at $300{\sim}400^{\circ}C$. The limit oxygen indices of the laminated paper and the varnish-laminated paper were in the range of 20~21%, while it was 34% for wood. This study enabled us to confirm that wood, laminated paper and varnish-laminated paper have a relatively short ignition time and are easy to burn but they all have low heat release. In contrast, wood showed the lowest fire risk among them and had excellent flame retardancy but with high heat release.

Thermal Characteristics of LaMnO3 Non-isothermal Synthesis Reaction (LaMnO3 비등온 합성반응의 열적특성)

  • Jeon, Jong Seol;Lee, Jung Hun;Yoon, Chang Hyeok;Yoo, Dong Jun;Lim, Dae Ho;Kang, Yong
    • Korean Chemical Engineering Research
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    • v.54 no.3
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    • pp.404-409
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    • 2016
  • Thermal Characteristics and kinetic parameters of $LaMnO_3$ synthesis reaction were investigated by means of TGA (Thermogravimetric analysis) at non-isothermal heating conditions (5.0, 10.0, 15.0 and 20.0 K/min). The reaction was occurred rapidly at 450~600K (X=0.4~0.7) depending on the heating rate. Activation energy for the synthesis of $LaMnO_3$ from the precursor, which was determined by different method such as Friedman, Ozawa-Flynn-Wall and Vyazovkin methods, was in the range of 23~243 kJ/g-mol depending on the fractional conversion level and estimation method. The reaction order decreased with increasing heating rate and fractional conversional level. The average reaction order was 4.50 in case of X=0.1~0.3, while it was 1.87 in case of X=0.7~0.9, respectively. The value of frequency factor of reaction rate increased with inceasing heating rate and fractional conversion level. The aveage value of frequency factor was 205.6 ($min^{-1}$) when X=0.1~0.3, while it was 475.2 ($min^{-1}$) when X=0.7~0.9, respectively.

Study on the Pyrolysis Kinetics of RDF(Refuse Derived Fuel) with Thermogravimetric Analysis (열중량 분석 기법을 통한 RDF의 열분해 특성 조사)

  • Kim, Dong-Won;Lee, Jong-Min;Kim, Jae-Sung
    • Korean Chemical Engineering Research
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    • v.47 no.6
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    • pp.676-682
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    • 2009
  • Devolatilization of the Refuse Derived Fuel(RDF) which is produced at WonJu in Korea was characterized in air atmosphere with variation of heating rate(10, 20 and $30^{\circ}C/min$) in TGA. The results of TG Analysis have shown that the pyrolysis and char combustion of the RDF occurred in the range of $350{\sim}700^{\circ}C$ depending on the heating rate. Activation energy of the RDF which was determined by using Friedman and Ozawa-Flynn-Wall method was in the range of 14.44~18.40 kcal/mol. Also, reaction order(n) and pre-exponential factors(A) were 1.219 and $3.02{\times}10^5$ by using Friedman method, respectively. In order to find out the devolatilization mechanism of the RDF, twelve solid-state mechanisms defined by Coats Redfern Method were tested. The results of the Coats Redfern Method have shown that chemical reaction is the effective mechanism by comparison with the value of the activation energy which was derived from the Friedman and Flynn-Wall-Ozawa method and correlation coefficient from twelve solid-state mechanisms of Coats Redfern Method. The solid state decomposition mechanism of the RDF was found to be a decelerated $F_1$ type, random nucleation with one nucleus on the individual particle.

Kinetic Study on Char-CO2 Catalytic Gasification of an Indonesian lignite (인도네시아 갈탄의 촤-CO2 촉매가스화 반응특성연구)

  • Lee, Do Kyun;Kim, Sang Kyum;Hwang, Soon Choel;Lee, Si Hoon;Rhee, Young Woo
    • Korean Chemical Engineering Research
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    • v.52 no.4
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    • pp.544-552
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    • 2014
  • In this study, We have investigated the kinetics on the char-$CO_2$ gasification reaction. Thermogravimetric analysis (TGA) experiments were carried out for char-$CO_2$ catalytic gasification of an Indonesian Roto lignite. $Na_2CO_3$, $K_2CO_3$, $CaCO_3$ and dolomite were selected as catalyst which was physical mixed with coal. The char-$CO_2$ gasification reaction showed rapid an increase of carbon conversion rate at 60 vol% $CO_2$ and 7 wt% $Na_2CO_3$ mixed with coal. At the isothermal conditions range from $750^{\circ}C$ to $900^{\circ}C$, the carbon conversion rates increased as the temperature increased. Three kinetic models for gas-solid reaction including the shrinking core model (SCM), volumetric reaction model (VRM) and modified volumetric reaction model (MVRM) were applied to the experimental data against the measured kinetic data. The gasification kinetics were suitably described by the MVRM model for the Roto lignite. The activation energies for each char mixed with $Na_2CO_3$ and $K_2CO_3$ were found a 67.03~77.09 kJ/mol and 53.14~67.99 kJ/mol.

Hydrogen Permeation of SrCe0.95Gd0.05O3-α-Ce0.9Gd0.1O2-β Proton-Conducting Ceramic Membranes (프로톤 전도성 SrCe0.95Gd0.05O3-α-Ce0.9Gd0.1O2-β 복합체 멤브레인의 수소투과 특성)

  • Kim, Hwan-Soo;Yu, Ji-Haeng;Shin, Min-Jae
    • Transactions of the Korean hydrogen and new energy society
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    • v.22 no.2
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    • pp.161-167
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    • 2011
  • Proton conductors have attracted considerable attention for solid oxide fuel cell (SOFC), hydrogen pump, gas sensor, and membrane separators. Doped $SrCeO_3$ exhibits appreciable proton conductivity in hydrogen-containing atmosphere at high temperature. However commercial realization has been hampered due to the reactivity of $SrCeO_3$ with $CO_2$. The chemical stability and proton conductivity are dependent on dopant type. The purpose of this work is to investigate chemical stability of $SrCe_{0.95}Gd_{0.05}O_{3-\alpha}-Ce_{0.9}Gd_{0.1}O_{2-\beta}$ composites in $CO_2$ and $H_2$ gases. Thermogravimetric analysis (TGA) was performed in gaseous $CO_2$ and electrical conductivity of the composites were also measured between 500 and $900^{\circ}C$ in air and $H_2$ atmosphere. $SrCe_{0.95}Gd_{0.05}O_{3-\alpha}-Ce_{0.9}Gd_{0.1}O_{2-\beta}$ composite membranes showed good chemical stability of in $CO_2$ atmosphere and high conductivity at hydrogen condition. The hydrogen permeation of $SrCe_{0.95}Gd_{0.05}O_{3-\alpha}-Ce_{0.9}Gd_{0.1}O_{2-\beta}$ composite membranes was investigated as a function of volumetric content of $SrCe_{0.95}Gd_{0.05}O_{3-\alpha}$. The $SrCe_{0.95}Gd_{0.05}O_{3-\alpha}-Ce_{0.9}Gd_{0.1}O_{2-\beta}$(6:4) membrane with a thickness of 1.0 mm showed the highest hydrogen permeability with the flux reaching of 0.12 $ml/min{\cdot}cm^2$ at $800^{\circ}C$ in 100%$H_2/N_2$ as feed gas.