• Korean Chemical Engineering Research
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• v.48 no.1
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• pp.45-52
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• 2010

Two different imide oligomers(6FDA-ODA/APA and 6FDA-MDA/MA) having crosslinkable end groups were prepared by using a solution imidization method and their properties were investigated. Also, semi-interpenetrating polymer networks(semi-IPN) were prepared using the blends of imide oligomers with polyetherimide $Ultem^{(R)}$, which is used in dual-ovenable packaging materials. The characteristic properties of semi-IPN films were interpreted by using TGA, Thin Film Diffusion Analyzer, and WAXD. Molecular weights of imide oligomers were successfully controlled utilizing 2-aminophenylacetylene(APA) and maleic anhydride(MA) as an endcapping agent. Exotherm reactions by crosslinking appeared and the amount of exthotherm heat was linearly increased as the content of imide oligomers was increased. For semi-IPNs of $Ultem^{(R)}$ and imide oligomers, 5% and 10% weight loss temperatures increased as the contents of imide oligomers were increased. Diffusion coefficient and water uptake of semi-IPNs decreased as the content of imide oligomers was increased, which might be resulted from hydrophobic fluorine group and high packing density. It was concluded that relatively low thermal stability and hydrolytic stability of polyetherimide $Ultem^{(R)}$ were improved by incorporating new developed imide oligomers.

• Bulletin of the Korean Chemical Society
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• v.31 no.9
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• pp.2603-2606
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• 2010

Novel soluble triazoleimide oligomers terminated with arylacetylene terminated were synthesized by the Cu(I)-catalysed 1,3-dipolar cycloaddition polymerization of diazides and imide-containing dialkyne. Several molecular weight triazoleimide oligomers were prepared from diazide and dialkyne monomers with different stoichiometric combinations. The curing behaviors of the oligomers were tested by differential scanning calorimetry (DSC). The thermal properties of the cured products were evaluated by DSC and thermogravimetric analysis (TGA). These cured oligomers showed the glass transition temperature of about $225-235^{\circ}C$ and the decomposition temperature (at 5% weight loss) of about $385-393^{\circ}C$ in nitrogen.

• Korean Chemical Engineering Research
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• v.54 no.1
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• pp.36-43
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• 2016

Hydrosilylation reactions of 2.4.6.8-tetrahydro-2.4.6.8-tetramethylcyclotetrasiloxane with allyl butyrate catalyzed by Karstedt's, $H_2PtCl_6$ and Pt/C catalyst were studied and 2.4.6.8-tetra (propyl butyrate)-2.4.6.8-tetramethylcyclotetrasiloxane was obtained. The reaction order, activation energies and rate constants were determined. Ringopening polymerization of 2.4.6.8-tetra (propyl butyrate)-2.4.6.8-tetramethylcyclotetrasiloxane in the presence of $CaF_2$, LiF, KF and anhydrous potassium hydroxide in $60-70^{\circ}C$ temperature range was carried out and methylsiloxane oligomers with regular arrangement of propyl butyrate pendant groups were obtained. The synthesized products were studied by FTIR and NMR spectroscopy. The polysiloxanes were characterized by wide-angle X-ray, gel-permeation chromatography and DSC analyses. Via sol-gel processes of oligomers doped with lithium trifluoromethylsulfonate or lithium bis (trifluoromethylsulfonyl)imide, solid polymer electrolyte membranes were obtained. The dependences of ionic conductivity of obtained polyelectrolytes on temperature and salt concentration were investigated, and it was shown that electric conductivity of the polymer electrolyte membranes at room temperature changed in the range $3.5{\times}10^{-4}{\sim}6.4{\times}10^{-7}S/cm$.

• Polymer(Korea)
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• v.38 no.6
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• pp.774-781
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• 2014

Acetylenic or phenylethynyl end-capped polyisoimide oligomers ($M_w$ 2500 g/mol, 5000 g/mol) based upon 4,4'-diamino diphenyl ether (4,4'-ODA)/4,4'-oxydiphthalic anhydride (ODPA) and 4,4'-ODA/3,3',4,4'-benzophenone tetracarboxylic acid dianhydride (BTDA) were synthesized by using 4-ethynylaniline (4-EA) or 4-phenylethynyl phthalic anhydride (4-PEPA) as an end capper. The incorporation of ethynyl groups were confirmed by FTIR spectroscopy. The isomerization temperature was influenced by molecular weight as well as the backbone structure of polyisoimides oligomers. Thus, polyisoimide oligomers with molecular weight of 2500 g/mol was found to be imidized at temperature $10^{\circ}C$ lower than that for the oligomers with molecular weight of 5000 g/mol. The crosslinking reaction of ethynyl groups occurred at a higher temperature than that for the isoimide/imide isomerization reaction. These two reactions were totally or partially overlapped on the DSC thermograms for the polyisoimide oligomer end-capped with 4-EA. Kinetics of thermal imidization and crosslinking reactions for the 4,4'-ODA/ODPA polyisoimide oligomers end-capped with 4-PEPA were investigated by performing dynamic DSC experiments at heating rate of $10^{\circ}C/min$. The activation energy and pre-exponential factors were 141 kJ/mol and $1.45{\times}10^{13}min^{-1}$ for the imidization reaction and 177 kJ/mol and $2.90{\times}10^{13}min^{-1}$ for the crosslinking reaction, respectively.

• Carbon letters
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• v.19
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• pp.1-11
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• 2016

In efforts to characterize and understand the properties and processing of phenylethynyl-terminated imide (LaRC PETI-5, simply referred to as PETI-5) oligomers and polymers as a high-temperature sizing material for carbon fiber-reinforced polymer matrix composites, PETI-5 imidization and thermal curing behaviors have been extensively investigated based on the phenylethynyl end-group reaction. These studies are reviewed here. In addition, the use of PETI-5 to enhance interfacial adhesion between carbon fibers and a bismaleimide (BMI) matrix, as well as the dynamic mechanical properties of carbon/BMI composites, are discussed. Reports on the thermal expansion behavior of intercalated graphite flake, and the effects of exfoliated graphite nanoplatelets (xGnP) on the properties of PETI-5 matrix composites are also reviewed. The dynamic mechanical and thermal properties and the electrical resistivity of xGnP/PETI-5 composites are characterized. The effect of liquid rubber amine-terminated poly(butadiene-co-acrylonitrile) (ATBN)-coated xGnP particles incorporated into epoxy resin on the toughness of xGnP/epoxy composites is examined in terms of its impact on Izod strength. This paper provides an extensive overview from fundamental studies on PETI-5 and xGnP, as well as applied studies on relevant composite materials.