• Title/Summary/Keyword: thermal cationic latent catalyst

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A Comparative Study on Electron-Beam and Thermal Curing Properties of Epoxy Resins (에폭시 수지의 전자선 및 열경화 특성에 관한 연구)

  • 이재락;허건영;박수진
    • Polymer(Korea)
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    • v.26 no.1
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    • pp.80-87
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    • 2002
  • A comparative study using electron-beam(EB) and thermal curing techniques was carried out to determine the effect of cure behavior and thermal stability of epoxy resins. In this work, benzylquinoxalinium hexafluoroantimonate(BQH) was used as a latent cationic catalyst for an epoxy resin. According to the thermogravimetric analysis(TGA), the decomposed activation energy based on Coats-Redfern method was higher in the case of thermal curing technique. This could be interpreted in terms of slow thermal diffusion rate resulted from high crosslink density of the thermally cured epoxy resin. However, the increase of hydroxyl group in the epoxy resin cured by EB technique was observed in near-infrared spectroscopy(NIRS) measurements, resulting in improving the stable short aromatic chain structure, integral procedural decomposition temperature, and finally ductile properties for high impact strengths.

Cure Behaviors of Epoxy Resin Initiated by Methylanilinium Salts as Latent Cationic Curing Agent (잠재성 양이온 경화제인 Methylanilinium염에 의해 개시된 에폭시 수지의 경화 거동)

  • 박수진;김택진;이창진;이재락;박정규
    • Polymer(Korea)
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    • v.25 no.2
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    • pp.168-176
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    • 2001
  • The effect of novel N-crotyl-N,N-dimethyl-4-methylanilinium hexafluoroantimonate (CMH) curing agent as a thermal latent initiator on thermal behaviors, rheological properties, and thermal stability of diglycidylether of bisphenol A (DGEBA) epoxy cationic system was investigated. From DSC measurements of DGEBA/CMH system, it was shown that this system exhibits an excellent thermal latent characteristic at a given temperature. The conversion and conversion rate of DGEBA/CMH system increased with increasing the concentration of initiator, due to high activity of CMH. Rheological properties of the system were investigated under isothermal condition using a rheometer The gelation time was obtained from the analysis of storage modulus (G'), loss modulus (G"), and damping factor (tan $\delta$). As a result, the reduction of gelation time was affected by high curing temperature and concentration of CMH, resulting in high degree of network formation in cationic polymerization, due to difference of activity. The thermal stability of the cured epoxy resin was discussed in terms of the activation energy for decomposition and thermal factors determined from TGA measurements.ents.

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Thermal Properties and fracture Toughness of Difunctional Epoxy Resins Cured by Catalytic Initiators (촉매형 개시제로 경화된 이관능성 에폭시 수지의 열적 특성 및 파괴인성)

  • 박수진;허건영;이재락
    • Polymer(Korea)
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    • v.26 no.3
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    • pp.344-352
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    • 2002
  • In this work, two thermal cationic latent catalysts, i.e., triphenyl benzyl phosphonium hexafluoroantimonate (TBPH) and benzyl 2-methylpyrazinium hexafluoroantimonate (BMPH) were newly synthesized. And the thermal and mechanical properties of difunctional epoxy (diglycidylether of bisphenol h, DGEBA) resins initiated by 1 phr of either TBPH or BMPH catalyst were investigated. As experimental results, the epoxy/TBPH system showed higher curing temperature and critical stress intensity factor ($K_{IC}$) than those of epoxy/BMPH. This could be interpreted in terms of slow thermal diffusion rate and bulk structure of four phenyl groups in TBPH. However, the decomposed activation energy determined from Coats-Redfern method was lower in the case of epoxy/TBPH. This result was probably due to the fact that broken short chain structure was developed by steric hindrance of TBPH.

Synthesis and Latent Characteristics of Thermal Cationic Latent Catalysts by Change of Substituent (치환기 변화에 따른 열잠재성 양이온 촉매의 합성과 잠재특성 연구)

  • Park, Soo-Jin;Heo, Gun-Young;Lee, Jae-Rock;Shim, Sang-Yeon;Suh, Dong-Hack
    • Polymer(Korea)
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    • v.25 no.4
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    • pp.558-567
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    • 2001
  • The syntheses of thermal latent catalysts have been carried out by modifying the substituent of pyrazinium salts. The thermal latent properties and cure behaviors of difunctional epoxy resin (diglycidylether of bisphenol-A, DGEBA) with 1 wt% of catalyst as an initiator were investigated by dynamic DSC method. As a result, the synthesized catalysts showed the good latent thermal properties in epoxy system. With increasing the basicity of substituted catalyst, the cure temperature and activation energy of epoxy system were increased, whereas the activity was decreased. This was probably due to the fact that the activity and cure behavior were controlled by ring strain and basicity of substituent. Consequently, the catalyst activity modified by methyl group as an electron donor was decreased in increasing of basicity in an initiation step of epoxy cure system. This is due to a decreasing of stabilities of both leaving group of pyrazinium salts and benzyl cation. However, the catalyst activity modified by cyano group as an electron acceptor was increased in increasing the stability of benzyl cation resulting from organic effects and resonance.

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Cure Kinetics, Thermal Stabilities and Rheological Properties of Epoxy/phenol Resin Blend System Initiated by Cationic Thermal Latent Catalyst (양이온 열잠재성 개시제에 의한 에폭시/페놀 수지 브랜드 시스템의 경화 동력학.열안정성 및 유변학적 특성)

  • 박수진;서민강;이재락
    • The Korean Journal of Rheology
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    • v.11 no.2
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    • pp.135-142
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    • 1999
  • The effects of 1 wt.% N-benzylpyrazinium hexafluoroantimonate (BPH) as a thermal latent initiator and blend compositions composed of 0, 5, 10, 20 and 40 wt.% of phenol-novolac resin to epoxy resin were investigated in terms of cure kinetics, thermal stabilities and rheological properties. Thermal latent properties of BPH were measured from the conversion as a function of reaction temperature on a dynamic DSC. This cationic BPH system turned out to be an effective thermal latent initiator in the epoxy-phenol curing system. And the increase of phenol-novolac resin concentration led to the decrease in the latent temperature and to the increase of cure activation energy ($E_a$) of the blend system. The thermal stability and activation energy ($E_t$) for decomposition, gel-time and activation energy ($E_c$) for cross-linking from rheometer increased within the composition range of 20~40 wt.% of phenol-novolac resin. This implies that the three-dimensional cross-linking may take place among hydroxyl group within phenol resin, epoxide ring within epoxy resin and BPH.

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Thermal Stability and Mechanical Interfacial Properties of DGEBA/PMR-15 Blend System Initiated by Cationic Latent Thermal Catalyst (잠재성 양이온 개시제를 이용한 DGEBA/PMR-15 블렌드계의 열안정성 및 기계적 계면 특성에 관한 연구)

  • Park, Soo-Jin;Lee, Hwa-Young;Han, Mijeong;Hong, Sung-Kwon
    • Journal of Adhesion and Interface
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    • v.5 no.1
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    • pp.3-11
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    • 2004
  • In this work, the cure behaviors of the DGEBA/PMR-15 blends initiated by N-benzylpyrazinium hexafluoroantimonate (BPH) as a cationic latent catalyst were performed in DSC and DMA analyses. And, the thermal stabilities were carried out by TGA analysis and their mechanical interfacial properties of blends were measured in the context of critical stress intensity factor ($K_{IC}$). As a result, the curing activation energy ($E_a$) determined from Ozawa's equation in DSC and the relaxation activation energy ($E_r$) from DMA were increased with increasing PMA-15 content. Also, the thermal stabilities obtained from the integral procedural decomposition temperature (IPDT) and the glass transition temperature ($T_g$) were highly improved with increasing the PMR-15 content, which were probably due to the high heat resistance. And, the $K_{IC}$ showed a similar behavior with $E_a$, which was attributed to the improving of the interfacial adhesion or hydrogen bondings between intermolecular chains.

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Cure Behavior and Thermal Stability of Difunctional/Trifunctional Epoxy Blend System Initiated by Thermal Latent Catalyst (열잠재성 촉매 개시제를 이용한 2관능성/3관능성 에폭시 블렌드계의 경화거동 및 열안정성)

  • Park, Soo-Jin;Kim, Taek-Jin;Lee, Jae-Rock
    • Applied Chemistry for Engineering
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    • v.10 no.7
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    • pp.1046-1051
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    • 1999
  • Cure behavior and thermal stability of the different ratio of diglycidylether of bisphenol A(DGEBA)/trimethylolpropane triglycidylether(TMP) epoxy blends initiated by 1 wt % N-benzylpyrazinium hexafluoroantimonate (BPH) as a cationic latent catalyst were studied using DSC and TGA, respectively. Latent properties were performed by measurement of the conversion as a function of temperature using dynamic DSC. Dynamic DSC thermograms of DGEBA/TMP blends revealed that the weak peak was formed by complex formation between the hydroxyl groups in DGEBA and BPH, and between epoxides and BPH in low temperature ranges. The strong peak was considered as an exothermic reaction by the formation of three-dimensional network in high temperature ranges. Isothermal DSC revealed that the reaction rate of the blends was found to be higher than that of the neat TMP. The thermal stabilities in the cured resins were increased with increasing the DGEBA content. These results could be interpreted in terms of the stable aromatic structure, existence of hydroxyl group and high molecular weight of DGEBA.

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A Study on the Preparation of the Eco-friendly Carbon Fibers-Reinforced Composites

  • Choi, Kyeong-Eun;Seo, Min-Kang
    • Carbon letters
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    • v.14 no.1
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    • pp.58-61
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    • 2013
  • In this work, the effect of catalysts on the mechanical properties of carbon fibers-reinforced epoxy matrix composites cured by cationic latent thermal catalysts, i.e., N-benzylpyrazinium hexafluoroantimonate (BPH) was studied. Differential scanning calorimetry was executed for thermal characterization of the epoxy matrix system. Mechanical interfacial properties of the composites were studied by interlaminar shear strength (ILSS), critical stress intensity factor ($K_{IC}$), and specific fracture energy ($G_{IC}$). As a result, the conversion of neat epoxy matrix cured by BPH was higher than that of one cured by diaminodiphenyl methane (DDM). The ILSS, $K_{IC}$, $G_{IC}$, and impact strength of the composites cured by BPH were also superior to those of the composites cured by DDM. This was probably the consequence of the effect of the substituted benzene group of BPH catalyst, resulting in an increase in the cross-link density and structural stability of the composites studied.