• Title/Summary/Keyword: Thermogravimetric Analysis

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Characterization of Gas Permeation Properties of Polyimide Copolymer Membranes (공중합체 폴리이미드를 이용한 기체분리막의 특성평가)

  • Lee, Jung Moo;Lee, Myeong Geon;Kim, Se Jong;Koh, Hyung Chul;Nam, Sang Yong
    • Membrane Journal
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    • v.25 no.3
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    • pp.223-230
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    • 2015
  • We synthesized novel polyimides with high gas permeability and selectivity for application of gas separation membrane. 2,2-bis(3,4-carboxylphenyl) hexafluoropropane dianhydride (6FDA) and two kinds of amines with high permeability and solubility were used to prepare the novel polymide. 2,4,6-Trimethyl-1,3-phenylenediamine (DAM) was used to improve gas permeability and 4,4-Methylenedianiline was used to improve the gas selectivity respectively. The polyimide copolymers were synthesized by commercial chemical imidization method using Triethylamine and Acetic anhydride and their average molecular weights were over 100,000 g/mol. The glass temperature (Tg) and the thermal degradation temperature were characterized using differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). The synthesized copolymers showed high Tg over $300^{\circ}C$ and high thermal degradation temperature over $500^{\circ}C$. The gas permeation properties were measured by time-lag equipment. Although general polyimides showed very low gas permeability, synthesized polyimide copolymer showed high $O_2$ permeability of 10.1 barrer with high $O_2/N_2$ selectivity around 5.3. From this result, we confirm that these membranes have possibility to apply to gas separation membrane.

Characterization of Gas Permeation Properties of Polyimide Copolymer Membranes for OBIGGS (OBIGGS용 공중합체 폴리이미드를 이용한 기체분리막의 투과 특성평가)

  • Lee, Jung Moo;Lee, Myung Gun;Kim, Deuk Ju;Nam, Sang Yong
    • Membrane Journal
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    • v.24 no.4
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    • pp.325-331
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    • 2014
  • We synthesized novel polyimides with high gas permeability and selectivity for application of on board inert gas generation system (OBIGGS). 2,2-bis(3,4-carboxylphenyl) hexafluoropropane dianhydride (6FDA) and two kinds of amines with high permeability and solubility were used to prepare the novel polymide. 2,3,5,6-Tetramethyl-1,4-phenylenediamine (TMPD) was used to improve gas permeability and various kinds of diamines were used to improve the gas selectivity respectively. The polyimide copolymers were synthesized by commercial chemical imidization method and their average molecular weights were over 100,000g/mol. The glass temperature ($T_g$) and the thermal degradation temperature were characterized using differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). The synthesized copolymers showed high $T_g$ over $300^{\circ}C$ and high thermal degradation temperature over $500^{\circ}C$. The gas permeation properties were measured by time-lag equipment. Although general polyimides showed very low gas permeability, synthesized polyimide copolymer showed high $O_2$ permeability of 36.21 barrer with high $O_2/N_2$ selectivity around 4.1. From this result, we confirm that these membranes have possibility to apply to OBIGGS.

Removal of CO2 in Syngas using Li2ZrO3 (Li2ZrO3를 이용한 합성가스내의 CO2 제거)

  • Park, Joo-Won;Kang, Dong-Hwan;Yoo, Kyung-Seun;Lee, Jae-Goo;Kim, Jae-Ho;Han, Choon
    • Applied Chemistry for Engineering
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    • v.17 no.3
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    • pp.250-254
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    • 2006
  • Reaction of $CO_2$ with $Li_{2}ZrO_{3}$ has been investigated in a TGA and the effects of $H_{2}$ and CO on the removal of $CO_{2}$ using $Li_{2}ZrO_{3}$ were evaluated in a packed bed reactor. The initial rate of $CO_{2}$ removal reaction of $Li_{2}ZrO_{3}$ increased with the increase of gas flow rate up to 100 mL/min and then was maintained, which implied the disappearance of the gas film resistance. The reaction of $CO_{2}$ with $Li_{2}ZrO_{3}$ took place as the first order and the range of optimum temperature was found to be about $500{\sim}600^{\circ}C$. XRD and SEM analysis showed the formation of crystalline $Li_{2}ZrO_{3}$ and porous $Li_{2}ZrO_{3}$/$ZrO_{2}$. The presence of $H_{2}$ did not affect the adsorption of $CO_2$ with $Li_2ZrO_3$. On the other hand, CO inhibited the sorption of $CO_{2}$ into $Li_{2}CO_{3}$(L) on $Li_{2}ZrO_{3}$.

Fabrication and Photocatalytic Properties of SiO2-TiO2 Composite Nanofibers (SiO2-TiO2계 복합 나노섬유의 제조 및 광활성 연구)

  • Hyun, Dong Ho;Lim, Tae-Ho;Lee, Sung Wook
    • Applied Chemistry for Engineering
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    • v.19 no.5
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    • pp.554-558
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    • 2008
  • $(1-x)SiO_2-(x)TiO_2$ composite fibers with various compositions of $TiO_2$ were prepared by electrospinning their sol-gel precursors of titanium (IV) iso-propoxide (TiP), and tetraethyl orthosilicate (TEOS). The surface morphology and structure of sintered composite fibers were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), simultaneous thermogravimetric analysis-differential scanning calorimetry (TGA-DSC) and Fourier transform infrared spectroscopy (FT-IR). As the content of $TiO_2$ in $(1-x)SiO_2-(x)TiO_2$ system was increased the average diameter of composite fibers was proportionally increased. Also, the transformation of $TiO_2$ from anatase to rutile form was inhibited by the highly dispersed $TiO_2$ around $SiO_2$ particles up to $0.6SiO_2-0.4TiO_2$ composite fibers even after calcination at $1000^{\circ}C$. The photocatalytic activity of $SiO_2-TiO_2$ composite fibers was examined for the methylene blue (MB) decomposition which was confirmed using UV-vis/DRS spectra. The experiments demonstrated that the MB in aqueous solution was successfully photodegraded using $SiO_2-TiO_2$ composite nanofibers under UV-visible light irradiation.

Pyrolysis Characteristics of Sawdust and Rice Husk (톱밥과 왕겨의 열분해 특성 연구)

  • Park, Dong Kyoo;Seo, Myung Won;Goo, Jeong Hoi;Kim, Sang Done;Lee, See Hoon;Lee, Jae Goo;Song, Byung-Ho
    • Applied Chemistry for Engineering
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    • v.18 no.5
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    • pp.415-423
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    • 2007
  • Pyrolysis characteristics of sawdust and rice husk as biomass resources in a thermogravimetric analysis were determined. Experiments were carried out with a linear heating rate under inert atmosphere of $N_2$ gas. Pyrolysis of the biomass can be classified as a lower temperature reaction zone where the major component of holocellulose is thermally decomposed and a high temperature reaction zone where lignin is thermally decomposed. The obtained data was analyzed by the two-step consecutive reaction model. Activation energies of sawdust and rice husk are found to be respectively 82.5 kJ/mol and 85.1kJ/mol in the low temperature zone according to the first order reaction model and 19.7 kJ/mol, 22.0 kJ/mol in the high temperature zone according to the three-way transport model. The reaction rate constant with variation of heating rate can be well predicted by the kinetic compensation relation of Gaur-Reed.

A Study on Flammability and Mechanical Properties of HDPE/EPDM/Boron Carbide/Triphenyl Phosphate Blends with Compatibilizer (HDPE/EPDM/Boron Carbide/Triphenyl Phosphate 블렌드의 상용화제 첨가에 따른 난연성 및 기계적 물성 연구)

  • Shin, Bum-Sik;Jung, Seung-Tae;Jeun, Joon-Pyo;Kim, Hyun-Bin;Oh, Seung-Hwan;Kang, Phil-Hyun
    • Polymer(Korea)
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    • v.36 no.5
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    • pp.549-554
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    • 2012
  • It was known that triphenyl phosphate wasn't homogeneously dispersed in HDPE/EPDM/boron carbide blends, which caused the decrease in mechanical properties. HDPE, EPDM, boron carbide, and triphenyl phosphate were blended with PE-g-MAH(polyethylene-graft-maleic anhydride) as a compatiblizer for improving the miscibility of triphenyl phosphate. Tensile strength of HDPE/EPDM/boron carbide blends decreased with increasing the contents of triphenyl phosphate for flammability. However, the mechanical properties of HDPE/EPDM/boron carbide/triphenyl phosphate blends increased by the addition of compatiblizer because triphenyl phosphate was homogeneously mixed in the blend system. The homogeneous dispersibility of triphenyl phosphate was confirmed by using scanning electron microscopy (SEM). Increased thermal stability and flammability derived from high miscibility of triphenyl phosphate were confirmed by the results of thermogravimetric analysis (TGA) and limiting oxygen index (LOI). A self-extinguishing HDPE/EPDM/boron carbide/triphenyl phosphate blend was successfully fabricated with more than 21% LOI.

Crystal Structure and Thermal Stability Study on Tetrabutylammonium Hexamolybdate [n-Bu4N]2[Mo6O19](TBAM)

  • Zhao, Pu Su;Zhao, Zhan Ru;Jian, Fang Fang;Lu, Lu De
    • Journal of the Korean Chemical Society
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    • v.47 no.6
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    • pp.553-558
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    • 2003
  • The crystal structure of $[n-Bu_4N]_2[Mo_6O_{19}]$(TBAM) (n-Bu4N=tetrabutylammonium) has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group C2/c, with lattice parameters ${\alpha}$=16.314(5), b=17.288(5), c=17.776(4)${\AA}$ ${\beta}$=101.47(3), and Z=4. In $[Mo_6O{19}]^{2-}$ anion, Mo atoms occupy six vertices of octahedron and each Mo atom is coordinated by six oxygen atoms to adopt distorted octahedral coordination geometry. The average bond distance of Mo-Ot (terminal), Mo-Ob (bridged) and Mo-Oc (central) are 1.680 ${\AA}$, 1.931 ${\AA}$ and 2.325 ${\AA}$ respectively. In $[n-Bu_4N]^+$ cation, the N atom possesses a slightly distorted tetrahedral geometry. There are some potential extensive C-H ${\cdots}$ O hydrogen bonds in the lattice, by which connecte molecules and stabilize the crystal structure. Thermogravimetric analysis suggests that thermal decomposition of the title compound includes two transitions and it loses weight at 356.0 and 803.5 $^{\circ}$, respectively, and the residue presumable be $Mo_2O_2$. Accordingly, the title compound has high thermal stability.

A Study on the Manufacturing and Mechanical Properties of the PA66/EPDM/PP Composites for Enhanced Low Temperature Fracture Resistances (저온 내충격성 향상을 위한 PA66/EPDM/PP 복합체 제조와 기계적 특성 연구)

  • Lee, Tae-Sik;Yoon, Chang-Rok;Bang, Dae-Suk;Ahn, Dae-Young;Kye, Hyoung-San;Shin, Kyung-Chul
    • Elastomers and Composites
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    • v.44 no.2
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    • pp.164-174
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    • 2009
  • PA66/EPDM/PP-g-MA and PA66/EPDM-g-MA/PP-g-MA composites were manufactured by a modular intermeshing twin screw extruder for enhanced low temperature impact resistance with different content of PP-g-MA. The results showed that composite containing 90 wt% of PA66, 8 wt% of EPDM-g-MA, and 2 wt% of PP-g-MA has a optimum value in the thermal and mechanical properties. The characteristics of the composites were analyzed by TGA, DSC, and SEM. From above results, we established that the low interfacial strength and the impact resistance at low temperature shown in a pre-existing PP/EPDM composite were enhanced by grafting with compatibilizer such as maleic anhydride. These results show the possibility of local manufacturing process and cost down with optimum screw configuration for best mixing quality in the twin screw extruder.

A Study on the Preparation of Halogen Free M-P Flame Retardant and Its Application to Composite Material (비할로겐 M-P 난연제 제조 및 복합재료 응용 연구)

  • Lee, Soon-Hong
    • Journal of the Korean Society of Safety
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    • v.24 no.6
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    • pp.63-71
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    • 2009
  • In order to improve flame retardancy, the halogen free organic melamine phosphate(M-P) flame retardant was synthesized from melamine and phosphoric acid by the reaction of precipitation. The ignition test was carried out preparing hybrid flame retardant compound($H_bFRC$) consisting of organic M-P and inorganic Mg$(OH)_2$ as a flame retardant in the polyolefin resins. The flame retardancy and mechanical properties of flame retardant aluminum composite panel($H_bFRC$-ACP) were performed to investigate the possibility of the composite material, which was contained M-P, as a inner core for $H_bFRC$-ACP. For this study, the results of ignition test indicate that a char formation and drip suppressing effect, and combustion time reduced as the content of M-P increased. The limited oxygen index(LOI) values were measured 17.4vol% and 31.5vol% for LDPE only and $H_bFRC$-3(M-P content: 15wt%), respectively. And it was verified that the $H_bFRC$-3 was needed more oxygen quantity with the increase of M-P content when it combustion. Also, the results from thermogravimetric analysis were observed endothermic peak at $350^{\circ}C$ and $550^{\circ}C$, it was confirmed predominant thermal stability though the wide temperature range by the mixture of M-P and Mg$(OH)_2$. The LDPE-ACP (using only LDPE as a inner core), $35.13kW/m^2$ of heat release rate(HRR) and 13.43MJ/m2 of total heat release(THR) were measured while the $H_bFRC$-ACP, $10.44kW/m^2$ of HRR and 1.84MJ/m2 of THR were measured by results of cone calorimeter test. In case of $H_bFRC$-ACP, the average gas emission amount of CO and $CO_2$ could be decreased down to 25% and 20%, respectively, in comparison with LDPE-ACP. The mechanical properties such as tensile strength, bending strength and adhesion strength of $H_bFRC$-ACP were revealed slightly high values $54N/mm^2$, $152N/mm^2$ and 120N/25mm, respectively, compared with LDPE-ACP. It was confirmed that flame retardancy was improved with the synergy effect because of char formation by M-P and hydrolysis by Mg$(OH)_2$. The result of this study suggest that $H_bFRC$ can be applied for an adequate halogen free flame retardant composite material as a inner core for ACP.

Steam Reforming of Ethylene Glycol over Ni/Al2O3 Catalysts: Effect of the Preparation Method and Reduction Temperature (Ni/Al2O3 촉매를 사용한 에틸렌글리콜의 수증기 개질 반응: 촉매 제조 방법과 환원온도의 영향)

  • Choi, Dong Hyuck;Park, Jung Eun;Park, Eun Duck
    • Korean Chemical Engineering Research
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    • v.53 no.3
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    • pp.372-381
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    • 2015
  • The effect of preparation method on the catalytic activities of the $Ni/Al_2O_3$ catalysts on steam reforming of ethylene glycol was investigated. The catalysts were prepared with various preparation methods such as an incipient wetness impregnation, wet impregnation, and coprecipitation method. In the case of coprecipitation method, various precipitants such as KOH, $K_2CO_3$, and $NH_4OH$ were compared. The prepared catalysts were characterized by using $N_2$ physisorption, inductively coupled plasma-atomic emission spectroscopy, X-ray diffraction, temperatureprogrammed reduction, pulsed $H_2$ chemisorption, temperature-programmed oxidation, scanning electron microscopy, and thermogravimetric analysis. Among the catalysts reduced at 773 K, the $Ni/Al_2O_3$ catalyst prepared by a coprecipitation with KOH or $K_2CO_3$ as precipitants showed the best catalytic performance. The preparation method affected the particle size of Ni, reducibility of nickel oxides, catalytic performance (activity and stability), and types of coke formed during the reaction. The $Ni/Al_2O_3$ catalyst prepared by a coprecipitation with KOH showed the increasing catalytic activity with an increase in the reduction temperature from 773 to 1173 K because of an increase in the reduction degree of Ni oxide species even though the particle size of Ni increased with increasing reduction temperature.