• Title/Summary/Keyword: Thermogravimetric analysis (TGA)

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Characterizations of Modified Silica Nanoparticles(I)

  • Min, Seong-Kee;Park, Chan-Young;Lee, Won-Ki;Seul, Soo-Duk
    • Korean Journal of Materials Research
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    • v.22 no.6
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    • pp.275-279
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    • 2012
  • (3-mercaptopropyl)trimethoxysilane (MPTMS) was used as a silylation agent, and modified silica nanoparticles were prepared by solution polymerization. 2.0 g of silica nanoparticles, 150 ml of toluene, and 20 ml of MPTMS were put into a 300 ml flask, and these mixtures were dispersed with ultrasonic vibration for 60 min. 0.2 g of hydroquinone as an inhibitor and 1 to 2 drops of 2,6-dimethylpyridine as a catalyst were added into the mixture. The mixture was then stirred with a magnetic stirrer for 8 hrs. at room temperature. After the reaction, the mixture was centrifuged for 1 hr. at 6000rpm. After precipitation, 150 ml of ethanol was added, and ultrasonic vibration was applied for 30 min. After the ultrasonic vibration, centrifugation was carried out again for 1 hr. at 6000rpm. Organo-modification of silica nanoparticles with a ${\gamma}$-methacryloxypropyl functional group was successfully achieved by solution polymerization in the ethanol solution. The characteristics of the ${\gamma}$-mercaptopropyl modified silica nanoparticles (MPSN) were examined using X-ray photoelectron spectroscopy (XPS, THERMO VG SCIENTIFIC, MultiLab 2000), a laser scattering system (LSS, TOPCON Co., GLS-1000), Fourier transform infrared spectroscopy (FTIR, JASCO INTERNATIONL CO., FT/IR-4200), scanning electron microscopy (SEM, HITACHI, S-2400), an elemental analysis (EA, Elementar, Vario macro/micro) and a thermogravimetric analysis (TGA, Perkin Elmer, TGA 7, Pyris 1). From the analysis results, the content of the methacryloxypropyl group was 0.98 mmol/g and the conversion rate of acrylamide monomer was 93%. SEM analysis results showed that the organo-modification of ultra-fine particles effectively prevented their agglomeration and improved their dispensability.

Investigation on Combustion Characteristics of Sewage Sludge using Pilot-scale Bubbling Fluidized Bed Reactor (파일럿 규모 기포 유동층 반응기를 이용한 하수 슬러지 연소 특성 분석)

  • Kim, Donghee;Huh, Kang Y.;Ahn, Hyungjun;Lee, Youngjae
    • Clean Technology
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    • v.23 no.3
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    • pp.331-342
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    • 2017
  • To estimate the combustion characteristics of sewage sludge and wood pellet, thermogravimetric analysis (TGA) was conducted. As TGA results, combustion characteristics of sewage sludge was worse than wood pellet. In ash fusion temperature (AFT) analysis, slagging tendency of sewage sludge is very high compared to wood pellet. And also, the bubbling fluidized bed reactor with a inner diameter 400 mm and a height of 4300 mm was used for experimental study of combustion characteristics fueled by sewage sludge and wood pellet. The facility consists of a fluidized bed reactor, preheater, screw feeder, cyclone, ash capture equipment and gas analyzer. The thermal input of sewage sludge cases were $54.5{\sim}96.5kW_{th}$, in case of wood pellet experiment, it was $96.1kW_{th}$. As experiment results, the $NO_x$ emission of sewage sludge was averagely about 10 times the $NO_x$ emission of wood pellet. And also CO emission of sewage sludge is about 3.5 times of wood pellet. Lastly as a result of analysis of captured ash in cyclone, the combustion efficiency of all cases were over 99%, but the potential for slagging/fouling was high at all cases by component analysis of ash.

Evaluation of Primary Thermal Degradation Feature of M. sacchariflorus After Removing Inorganic Compounds Using Distilled Water (증류수를 이용한 거대억새 내 무기성분 제거 효과 및 열분해 특성 변화 관찰)

  • Kim, Jae-Young;Oh, Shinyoung;Hwang, Hyewon;Moon, Yoonho;Choi, Joon Weon
    • Journal of the Korean Wood Science and Technology
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    • v.41 no.4
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    • pp.276-286
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    • 2013
  • The goal of this study was to investigate change of thermal decomposition feature of miscanthus (Miscanthus sacchariflorus) after removal of inorganic constituents using distilled water (D.I-w; 30, 60 and $90^{\circ}C$). The carbon content was increased whereas the oxygen content was decreased with the temperature of D.I-w treatment. Moreover, ash content was slightly decreased from 4.6% of control to 3.2% of $90^{\circ}C$ D.I-w treated sample. Results of total monomeric sugar contents and X-ray diffraction (XRD) analysis showed that structural changes of cellulose/hemicellulose regions did not occurr during D.I-w treatment. Results of inductively coupled plasma emission spectrometer (ICP-ES) showed that miscanthus has the largest amount of inorganic constituents such as potassium (5,644 ppm), phosphorus (3,995 ppm), magnesium (1,403 ppm) and calcium (711 ppm). Thermogravimetric analysis (TGA) confirmed that the yield of char slightly decreased whereas the yield of volatiles increased with increasing D.I-w treatment temperature. In addition, differential thermogravimetric analysis (DTGA) indicated that the maximum decomposition rate ($V_M$) and temperature ($T_M$) corresponding to VM were varied from $0.82%/^{\circ}C$, $360.60^{\circ}C$ of control to $1.17%/^{\circ}C$, $362.62^{\circ}C$ of $90^{\circ}C$-D.I-w treated sample.

Pyrolysis Characteristics of the Mixture of Waste Fishing Net and Waste Ship Lubricating Oil (폐어망과 선박용 폐윤활유 혼합물의 열분해반응 특성 연구)

  • Kim, Seung-Soo;Kim, Young-Sik
    • Applied Chemistry for Engineering
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    • v.19 no.5
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    • pp.568-573
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    • 2008
  • Kinetic tests on pyrolysis of waste fishing net [WFN; nylon-6], waste ship lubricating oil [WSLO] and their mixture were carried out by thermogravimetric analysis (TGA) with heating rate of 0.5, 1.0, and $2.0^{\circ}C/min$. Pyrolysis of waste fishing net started at $300^{\circ}C$, and the main region of decomposition temperature was between 360 and $440^{\circ}C$ at each heating rate. Decomposition temperature of the mixture of WFN and WSLO was lower than that of WFN and WSLO, and the shape of thermogravimetic graph of mixture was different as well. The corresponding kinetic parameters including activation energy and pre-exponential factor were determined by differential method over the degree of conversions. The values of activation energies for the mixture of WFN and WSLO were between 98 and 427 kJ/mol as the conversion increased from 5% to 95%. Tubing reactor was used to analysis of pyrolyzed oil at $440^{\circ}C$ for 80 min. The selectivity of specific hydrocarbons was not detected and the carbon number distribution of the pyrolyzed oil was below $C_{22}$.

Isothermal Decomposition of Ammonium Molybdate to Molybdenum Trioxide in a Fluidized Bed Reactor

  • Oh, Chang-Sup;Park, Yong-Ok;Hasolli, Naim;Kim, Hang Goo;Won, Yong Sun;Shin, Su-Been;Kim, Yong-Ha
    • Korean Journal of Materials Research
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    • v.25 no.10
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    • pp.547-551
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    • 2015
  • The present study prepared molybdenum trioxide ($MoO_3$), the most important intermediate of molybdenum metal, by using a fluidized bed reactor for the thermal decomposition of ammonium molybdate (AM) in the presence of an air flow. During the process of fluidizing the sample inside the reactor, the reaction time and temperature were optimized with a close analysis of the X-ray diffraction (XRD) data and with thermogravimetric analysis (TGA). In particular, the temperature level, at which the AM decomposition is completed, is very important as a primary operating parameter. The analysis of the XRD and TGA data showed that the AM decomposition is almost completed at ${\sim}350^{\circ}C$ with a reaction time of 30 min. A shorter reaction time of 10 min. required a higher reaction temperature of ${\sim}500^{\circ}C$ with the same air flow rate to complete the AM decomposition. A sharp rise in the decomposition efficiency at a temperature ranging between 320 and $350^{\circ}C$ indicated a threshold for the AM decomposition. The operating conditions determined in this study can be used for future scale-ups of the process.

Effect of Flame Retardants on Flame Retardancy of Flexible Polyurethane Foam (난연제 종류에 따른 연질 폴리우레탄 폼의 난연 특성에 대한 연구)

  • Kwon, Ohdeok;Lee, Ju-Chan;Seo, Ki-Seog;Seo, Chung-Seok;Kim, Sang Bum
    • Applied Chemistry for Engineering
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    • v.24 no.2
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    • pp.208-213
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    • 2013
  • In this study, the effect of phosphorus flame retardants on the flame retardancy of the flexible polyurethane foam (PUF) was investigated. Tetramethylene bis(orthophosphorylurea) [TBPU] and phosphinyl alkylphosphate ester [CR-530], resorcinol bis diphenylphosphate [RDP], triethyl phosphate [TEP] were used as flame retardants. The results of thermogravimetric analysis (TGA) indicate that TBPU added PUF produces more charred residues than the other flame retardant added PUF. It was found that TBPU added PUF exhibits low mean heat release rate (HRR), peak HRR, effective heat of combusion (EHC), mass loss rate (MLR), CO yield and $CO_2$ compared to those other flame retardants.

Enhanced Flame Resistant Properties of Aluminum Hydroxide Addition on Electrospun Polyurethane Nanofibers (전기방사법에 의해 제조된 폴리우레탄 나노섬유의 수산화알루미늄 내첨에 의한 내염화 특성 향상)

  • Kim, Hyeong Gi
    • Fire Science and Engineering
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    • v.30 no.6
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    • pp.9-13
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    • 2016
  • Anti-oxidation and flame resistant polyurethane nanofibers were prepared by electrospinning and aluminum hydroxide addition. Electrospinning was carried out under the following procedure conditions; applied voltage, 20 kV; polymer solution feeding rate, 1.2 ml/h; collector rolling speed, 120 rpm; and tip to collector distance, 15 cm. Aluminum hydroxide was added to the prepared polymer solution for electrospinning to enhance the oxidation and flame resistant properties. The thermal properties were investigated by thermogravimetric analysis to determine the polymer decomposition temperature, integral procedure decomposition temperature, final decomposition temperature, and remaining amount after thermal decomposition. The activated energy for polymer degradation was also investigated using the Horowitz-Metzger equation. The activation energy increased to more than 50%. The thermal properties of the polyurethane nanofibers were improved by a hydration reaction during the thermal decomposition of aluminum hydroxide around $300{\sim}500^{\circ}C$.

Experimental and Numerical Study of the Thermal Decomposition of an Epoxy-based Intumescent Coating (실험과 계산을 통한 에폭시 계열 내화도료의 열분해에 관한 연구)

  • Kim, Yangkyun
    • Fire Science and Engineering
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    • v.30 no.1
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    • pp.31-36
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    • 2016
  • This study investigates the characteristics of thermal decomposition of an epoxy-based intumescent paint using thermogravimetric analysis (TGA) and numerical simulation. A mathematical and numerical model is introduced to describe mass loss profiles of the epoxy-based intumescent coating induced by the thermal decomposition process. The decomposition scheme covers a range of complexity by employing simplified 4-step sequential reactions to describe the simultaneous thermal decomposition processes. The reaction rates are expressed by the Arrhenius law, and reaction parameters are optimized to fit the degradation behavior seen during thermogravimetric (TG) experiments. The experimental results show a major 2-step degradation under nitrogen and a 3-step degradation in an air environment. The experiment also shows that oxygen takes part in the stabilization of the intumescent coating between 200 and $500^{\circ}C$. The simulation results show that the proposed model effectively predicts the experimental mass loss as a function of time except for temperatures above $800^{\circ}C$, which were intentionally not included in the model. The maximum error in the simulation was less than 3%.

Influence of Alkali and Silane Treatment on the Physico-Mechanical Properties of Grewia serrulata Fibres

  • JAIN, Bhupesh;MALLYA, Ravindra;NAYAK, Suhas Yeshwant;HECKADKA, Srinivas Shenoy;PRABHU, Shrinivasa;MAHESHA, G.T.;SANCHETI, Gaurav
    • Journal of the Korean Wood Science and Technology
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    • v.50 no.5
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    • pp.325-337
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    • 2022
  • Grewia serrulata fibres were chemically treated with 3%, 6%, and 9% NaOH for the duration of 4 h. Additionally, the NaOH-treated fibres were also treated with 3 - (trimethoxysilyl) propyl methacrylate (silane). Properties such as density and tensile strength of the treated fibres were compared against the untreated fibres. The highest density was obtained in the case of 9% NaOH + silane treated fibres, which was 26.47% higher than untreated fibres, implying effective removal of hemicellulose. Likewise, the highest tensile strength was also obtained in the case of 9% NaOH + silane treated fibres. The increment observed in the tensile strength of the natural fibres was related to the removal of impurities, hemicellulose, and stress-raisers as well as deposition over the fibre surface that smoothed it. These observations were further validated by estimating changes in chemical constituents due to chemical treatment along with characterization techniques such as scanning electron microscopy and thermogravimetric analysis.

Study on the Combustion Characteristics of Wood-pellet and Korean Anthracite Using TGA (열중량 분석기를 이용한 목재펠릿 및 국내무연탄의 연소 특성 조사)

  • Kim, Dong-Won;Lee, Jong-Min;Kim, Jae-Sung;Seon, Pyeong-Ki
    • Korean Chemical Engineering Research
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    • v.48 no.1
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    • pp.58-67
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    • 2010
  • Combustion of the Korean Anthracite and wood-pellet was characterized in air atmosphere with variation of heating rate(5, 10, 20 and $30^{\circ}C/min$) in TGA. The results of TGA have shown that the combustion of the wood-pellet occurred in the temperature range of $200{\sim}620^{\circ}C$ which is much lower than that of Korean anthracite. Activation energies of the wood-pellet and Korean anthracite, determined by using Friedman method were 44.12, 21.45 kcal/mol respectively. Also, their reaction orders(n) and pre-exponential factors(A) were 5.153, 0.7453 and $4.01{\times}10^{16}$, $1.39{\times}10^6(s^{-1})$ respectively. In order to find out the combustion mechanism of the wood-pellet and Korean anthracite, twelve solidstate mechanisms defined by Coats Redfern Method were tested. The solid state combustion mechanisms of the woodpellet and Korean anthracite were found to be sigmoidal curve A3 type and a deceleration curve F1 type respectively. Also, from iso-thermal combustion($300{\sim}900^{\circ}C$) of their char, the combustion characteristics of their char was found. Activation energies of the their char were 27.5, 51.2 kcal/mol respectively. Also, pre-exponential factors(A) were $2.55{\times}10^{12}$, $1.49{\times}10^{10}(s^{-1})$ respectively. Due to the high combustion reactivity of wood-pellet compared with Korean anthracite, combustion atmosphere will be improved by co-combustion with Korean anthracite and wood-pellet.