• Title/Summary/Keyword: Grubbs catalyst

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Thermal Stability of Grubbs' Catalyst and Its Reactivity with Self-healing Agents (Grubbs' Catalyst의 열안정성 및 자가치료제와의 반응성 평가)

  • Yoon, Sung Ho;Shi, Ya Long;Feng, Jun;Jang, Se Yong
    • Composites Research
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    • v.28 no.6
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    • pp.395-401
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    • 2015
  • This study investigated the thermal stability of Grubbs' catalyst and its reactivity with self-healing agents for self-healing damage repair. Four types of Grubbs' catalyst supplied by manufacturers were considered and each catalyst was tested in as-received and grinded conditions. Four types of self-healing agents were prepared by varying the mixing ratio of dicyclopentadiene (DCPD) and 5-ethylidene-2-norbonene (ENB). Heat flows as a function of temperature were measured through a differential scanning calorimetry (DSC) to determine the thermal stability of catalysts. Reaction heats of self-healing agents with the catalyst were measured to evaluate the reactivity of the catalyst. For this evaluation, Fluka Chemika Grubbs' catalyst was used based on the maximum temperature and the time to reach the maximum temperature. According to the results, catalysts had different shapes depending on the manufacturer and the results showed that the smaller the size of the catalyst the higher the reactivity with self-healing agents. As the ENB ratio in self-healing agents increased, the maximum temperature increased, and the time to reach the maximum temperature decreased. As the amount of the catalyst increased, the maximum temperature increased, and the time to reach the maximum temperature decreased. Considering the thermal stability of the catalyst and its reactivity with the self-healing agent, combination of 0.5 wt% catalyst and the D3E1 self-healing agent was optimal for self-healing damage repair. Finally, as the thermal decomposition may occur depending on the environmental temperature, the catalyst must not be exposed to temperature higher than that is necessary to maintain the thermal stability of the catalyst.

Synthsis and Antiviral Evaluation of Novel 3'-and 4 -Doubly Branched Carbocyclic Nucleosides as Potential Antiviral Agents

  • Hong, Joon-Hee
    • Archives of Pharmacal Research
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    • v.26 no.12
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    • pp.1109-1116
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    • 2003
  • A series of 3'- and 4'-branched carbocyclic nucleosides 25, 26, 27, 28, 29 and 30 were synthesized starting from simple acyclic ketone derivatives. The construction of the required quaternary carbon was made using a [3,3]-sigmatropic rearrangement. In addition, the installation of a methyl group in the 3'-position was accomplished using a Horner-Wadsworth-Emmons (HWE) reaction with triethyl 2-phosphonopropionate. Bis-vinyl was successfully cyclized using a Grubbs' catalyst (Ⅱ). Natural bases (adenine, cytosine, uracil) were efficiently coupled with the use of a Pd(0) catalyst.

Colorless and Transparent Polyimide Films from Poly(amic acid)s with Cross-linkable Anhydride End (가교 반응이 가능한 말단 무수물을 이용한 무색투명한 폴리이미드 필름)

  • Min, Ung-Ki;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.34 no.6
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    • pp.495-500
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    • 2010
  • Crosslinked PI films were synthesized from 4,4'-(hexafluoro isopropylidene)diphthalic anhydride (6FDA) and bis[4-(3-aminophenoxy) phenyl] sulfone(BAPS) with various ratios of the reactive monomer cis-4-cyclohexene-1,2-dicarboxylic anhydride(CDBA). We prepared crosslinked poly(amic acid) (PAA) using a 0.1 wt% Grubbs catalyst as a crosslinking agent. The crosslinked PAA was heat-treated at different temperatures to give PI films. The thermo-mechanical properties and optical transparency of the PI films were investigated. The thermal properties of the PI films were examined using Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry(DSC), thermogravimetric analysis(TGA), thermo-mechanical analysis(TMA), and universal tensile machine(UTM), and their optical transparencies were investigated using UV-vis. spectrophotometry. The thermomechanical properties of the PI films improved with increasing CDBA content. However, the optical transparency of the PI films decreased slightly with increasing CDBA content.

Evaluation of Bond Performance of Self-Healing Agents Using Single lap Shear Test (Single Lap 전단시험을 적용한 자가치료제의 접착성능 평가)

  • 윤성호;박희원;허광수
    • Composites Research
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    • v.17 no.4
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    • pp.40-46
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    • 2004
  • A single lap shear test was used to investigate the effects of the ratio of a catalyst to a self-healing agent and curing temperature on the bond performance of autonomic polymer composites. DCPD (dicyclopentadiene), ENB (5-ethylidene-2-norbornene), and their mixture were used as self-healing agents and bis(triclohexylphosphine) benzyllidine ruthenium (IV) dichloride Grubbs' catalyst was used as a catalyst. During the experiments, the catalyst ratios of 1.0wt% and 0.5wt% were applied to DCPD, the catalyst ratio of 0.lwt% was applied to ENB, and the catalyst ratio of 0.5wt% was applied to the mixtutes of DPCD and ENB. In addition, the curing temperatures of $25^{\circ}C$, $60{\circ}C$, and $80^{\circ}C$ were considered. According to the results, the higher catalyst ratio and the longer curing time were required to obtain more stabilized bond shear strength of DCPD. ENB with a lower catalyst ratio was cured faster than DCPD. Unlike DCPD, ENB stabilized after a steady fall from its peak as the curing time increased. Moreover, the mixtures of DCPD and ENB revealed similar curing behavior to ENB, but the increase in mixture ratio of ENB to DCPD caused curing process to be faster. Also the increase in curing temperature caused the bond shear strength to be higher and the curing time to be quicker.

Olefin Metathesis Curing Reaction of Essential Oils in Korean Dendropanax Lacquer (Olefin Metathesis를 이용한 황칠 Essential Oil의 경화 반응에 관한 연구)

  • Kim, Mi Ri;Lee, Won Hwi;Yoo, Hye Jin;Kim, Jong Sang;Cheong, In Woo
    • Journal of Adhesion and Interface
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    • v.16 no.4
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    • pp.146-151
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    • 2015
  • Raw sap of essential oil in Korean Dendropanax lacquer was extracted with ethanol, and which was cured by using ROMP (ring opening metathesis polymerization, one of olefin metathesis). Curing behavior with subsequent film properties were studied and compared with conventional curing (under ambient conditions) and UV photo curing. The compositional changes of major ingredients in the lacquer before and after curing were studied by using GC-MS (gas chromatography mass spectrometry). ROMP-cured coating film showed higher gel contents (40%) as compared to those of conventional (8%) and UV curing (25%). ROMP curing with 2 wt% Grubbs' catalyst at $100^{\circ}C$ completed curing reaction within 2 h, which was much faster than that of conventional curing. The quality of coating film prepared with ROMP was more homogeneous and wrinkle-free as compared with that with UV curing. It was found that major ingredients of sesquiterpenes, such as ${\alpha}$-selinene, ${\beta}$-selinene, and ${\delta}$-cadinene were reacted in ROMP, as well as polyacetylenes.

Synthesis of Novel Carbovir Analogue

  • Kim, Ai-hong;Hong, Joon-Hee
    • Bulletin of the Korean Chemical Society
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    • v.27 no.7
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    • pp.976-980
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    • 2006
  • The synthesis of 4'-phenyl and 1'-methyl doubly branched carbocyclic nucleoside was accomplished from 2-hydroxy acetophenone. The 4'-phenyl group was installed via a [3,3]-sigmatropic rearrangement reaction, and the carbonyl addition of methylmagnesium bromide was used to introduce the 1'-methyl group. Cyclization of divinyl 9 was performed using $2^{nd}$ generation Grubbs catalyst. The coupling of cyclopentenol 12$\alpha$ with 6-chloropurine by Mitsunobu reaction and desilylation was used to synthesize the target nucleoside 15.