• Title/Summary/Keyword: Thermal cyclization

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Synthesis and Properties of Polybenzoxazole Precursors having Oligo(oxy ethylene) pendant (Oligo(oxy ethylene) pendant를 갖는 PBO 전구체의 합성 및 특성)

  • Lee, Eung-Jae;Yoon, Doo-Soo;Bang, Moon-Soo;Choi, Jae-Kon
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.14 no.5
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    • pp.2550-2558
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    • 2013
  • Poly(o-hydroxyamides)(PHAs) copolymers having oligo(oxy ethylene) pendant in the main chain were synthesized by solution polycondensation reaction at low temperature. Copolymer precursors were studied by fourier transform infrared(FT-IR), differential scanning calorimeter(DSC), thermogravimetric analyzer(TGA), universal testing machine(UTM) and limited oxygen index(LOI). The inherent viscosities of the PHAs measured at $35^{\circ}C$ in DMAc or DMAc/LiCl solution were in the range of 0.74~1.42 dL/g. Solubility of the precursors with higher oligo(oxy ethylene) unit was increased, but the PBOs were nearly insoluble in a variety of solvents. The degradation temperature of the copolymer precursors was recorded in the ranges of $408{\sim}664^{\circ}C$ in nitrogen and char yields showed 13~59% values at $900^{\circ}C$. The mechanical properties and flame retardancy of copolymer precursors decreased with higher oligo(oxy ethylene) unit.

Synthesis and Thermal Properties of Aromatic Poly(o-hydroxyamide)s Containing Phenylene Diimide Unit (Phenylene Diimide 단위를 포함한 방향족 Poly(o-hydroxyamide)s의 합성 및 열적 특성)

  • Lee, Eung-Jae;Yoon, Doo-Soo;Choi, Jae-Kon
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.14 no.11
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    • pp.6029-6038
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    • 2013
  • In this study we attempt to modify the backbone structure and improve processibility of PBO having high melting and glass transition temperature. A series of aromatic poly(o-hydroxyamide)s(PHAs) were synthesized by direct polycondensaton of diacides containing diimide unit with two types of bis(o-aminophenol)s including 3,3'-dihydroxybenzidine and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane. PHAs were studied by FT-IR, $^1H$-NMR, DSC and TGA. PHAs exhibited inherent viscosities in the range of 0.34~0.65 dL/g at $35^{\circ}C$ in DMAc solution. The PHA 1 and 6F-PHA 6, introducing o-phenylene unit in the main chain showed excellent solubilities in aprotic solvents such as NMP etc. However, the PHA 3, having p-phenylene unit was not even dissolved perfectly with LiCl salt. 6F-PHAs were readily soluble at room temperature in aprotic solvents except 6F-PHA 3. But they showed better solubility than that of PHAs. The polybenzoxazoles(PBOs) were quite insoluble in other solvents except partially soluble in sulfuric acid. PBOs exhibited relatively high glass transition temperatures(Tg) in the range of 306~$311^{\circ}C$ by DSC. The maximum weight loss temperature and char yields of PHA3 and 6F-PHA3 showed the highest values of $658^{\circ}C$ and $653^{\circ}C$, 62.6 % and 62.1 %, respectively.

Effects of Pitch Softening Point-based on Soft Carbon Anode for Initial Efficiency and Rate Performance (피치계 소프트 카본 음극재 제조 시 피치의 연화점이 음극재 초기 효율 및 율속 특성에 미치는 영향)

  • Kim, Kyung Soo;Im, Ji Sun;Lee, Jong Dae;Kim, Ji Hong;Hwang, Jin Ung
    • Applied Chemistry for Engineering
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    • v.30 no.3
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    • pp.331-336
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    • 2019
  • In this study, required properties and optimized procedure conditions for the pitch based soft carbon anode of lithium ion battery was investigated for improving the initial efficiency and rate performance. Each petroleum residue was thermally treated at 360, 370, and $410^{\circ}C$ for 3 hours to synthesis a pitch and the corresponding pitch shows the softening point of 86, 98, and $152^{\circ}C$, respectively. The elemental analysis and thermal characteristics of the pitch were investigated by EA analysis and TGA. It was noted that the low H/C and improved thermal stability were obtained with the high softening point. The obtained pitch was carbonized at $1,200^{\circ}C$ for 1 hour to produce a soft carbon based anode. As a result of investigating the crystal structure by XRD analysis, it was found that the crystallinity of soft carbon increased with increasing the softening point. It was considered that relatively higher boiling components and decreases in the evaporation component resulted the components participation for cyclization during the heat treatment process. The soft carbon based anode with an improved crystallinity shows the enhanced initial efficiency and rate performance. The mechanism of both improvements was also discusssed based on the developed crystal structure of soft carbon based anode materials.

Physical Properties and Flame Retardency of Polyhydroxyamides (PHAs) Having Pendant Groups in the Main Chain (주사슬에 곁사슬기를 갖는 폴리히드록시아미드의 물성 및 난연특성)

  • Yoon, Doo-Soo;Choi, Jae-Kon;Jo, Byung-Wook
    • Polymer(Korea)
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    • v.30 no.6
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    • pp.478-485
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    • 2006
  • Physical properties and flammability of polyhydroxyamides (PHAs) haying poly (ethylene-glycol) methyl ether (MPEG) and/or dimethylphenoxy pendants were studied by using DSC, TGA, FTIR, pyrolysis combustion flow calorimeter (PCFC), and X-ray diffractometer. The degradation temperatures of the polymers were recorded in the ranges of $276{\sim}396^{\circ}C$ in air. PCFC results showed that the heat release (HR) capacity and total heat release (total HR) values of the PHAs were increased with in-creasing molecular weight of MPEG. In case of M-PHA 2 annealed at $290^{\circ}C$, the values of HR capacity were siginificantly decreased from 253 to 42 J/gK, and 60% weight loss temperatures increased from 408 to $856^{\circ}C$ with an annealing temperature. The activation energy for the decomposition reaction of the PHAs showed in the range of $129.3{\sim}235.1kJ/mol$, which increased with increasing conversion. Tensile modulus of PHAs were decreased as increasing chain of MPEG, and showed an increase more than initial modulus after converted to PBOs.