• Journal of the Korea Institute of Military Science and Technology
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• v.8 no.1 s.20
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• pp.69-80
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• 2005

A synthesis of azide-terminated glycidyl azide polymer, GAP-A, was carried out by tosylation and azidation of polyepichlorohydrin(PECH) prepared by cationic ring-opening polymerization. Polyepichlorohydrin was prepared by cationic activated monomer polymerization using ethylene glycol and $BF_3{\cdot}OEt_2$ as an initiator and a catalyst at $\~10^{\circ}C$. Tosylation of polyepichlorohydrin was performed using traditional TsCl/pyridine method and was also carried out using TsCl/amine catalysts to reduce the reaction time significantly. Azidation of tosyl-terminated PECH(OTs-PECH) was performed using $NaN_3$ as an azidation reagent in DMF solvent at high temperature and was unexpectedly completed within 2 hours.

• Journal of the Korea Institute of Military Science and Technology
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• v.7 no.2 s.17
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• pp.109-117
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• 2004

We synthesized energetic prepolymer(2-nitrato ethyl oxirane, NEO) for plastic-bonded explosive and measured its thermodynamic parameters. 2-Nitrato ethyl oxirane(NEO) as a monomer was synthesized from 4-butene-ol, the first-step was preparation of 1-nitrate-3-butene and second-step was synthesized 2-nitrate-ethyl oxirane from 1nitrate-3-butene and then polymerized by cationic ring opening polymerization. The unreacted monomer concentration was measured by GC. The thermodynamic parameters were obtained from the ceiling temperature(Tc) values of 1 mole monomer at each reaction temperature. We varied feed rate of monomer, concentration of initiator and monomer to control molecular weight and polydispersity of perpolymer(NEO). Number average molecular weight(Mn), polydispersity(PD), and glass transition temperature(Tg), viscosity of prepolymer(NEO) were 2000, 1.07, $-55^{\circ}C$ and 300 poise respectively.

• Bulletin of the Korean Chemical Society
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• v.19 no.3
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• pp.328-332
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• 1998

Anionic ring-opening polymerization of 3,4-[(dimethylsilyl)isopropyl]benzo-1,1-dimethyl-1-silacyclopentene in the presence of n-butyllithium and HMPA in THF at - 78 ℃ afforded poly[3,4-(dimethylsilylisopropyl)benzo-1,1-dimethyl-1-silapentene]. The characteristic Si-H stretching frequency in the IR is observed at 2100 cm-1. The polycarbosilane has been modified by chloroplatinic acid catalyzed addition of styrene to the polycarbosilane SiH units. Molecular weights and thermal properties of the polymers were compared. The sol-gel polymerization of 3,4-[(dimethoxysilyl)isopropyl]benzo-1,1-dimethoxy-1-silacyclopentene in the presence of aqueous HCl or NaOH in THF resulted in a cross-linked polysiloxane. The xerogel has a low surface area of 13-14 m2/g and is stable up to about 400 ℃ with only 5% weight loss under a nitrogen atmosphere.

• Polymer(Korea)
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• v.28 no.4
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• pp.344-351
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• 2004

Poly(ethylene glycol)-based diblock and triblock polyester copolymers stimulating to temperature were studied as injectable biomaterials in drug delivery system because of their nontoxicity, biocompatibility and biodegradability. We synthesized the diblock copolymers consisting of methoxy poly(ethylene glycol) (MPEG) (M$_{n}$=750 g/mole) and poly($\varepsilon$-caprolactone) (PCL) by ring opening polymerization of $\varepsilon$-CL with MPEG as an initiator in the presence of HCl . Et$_2$O. The aqueous solution of synthesized diblock copolymers represented sol phase at room temperature and a sol to gel phase transition as the temperature increased from room temperature to body temperature. To confirm the in vivo gel formation, we observed the formation of gel in the mice body after injection of 20 wt% aqueous solution of each block copolymer. After 2 months, we observed the maintenance of gel without dispersion in mice. In this study, we synthesized diblock copolymers exhibiting sol-gel phase transition and confirmed the feasibility as biomaterials of injectable implantation.n.

• Polymer(Korea)
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• v.38 no.1
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• pp.9-15
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• 2014

Polyamide4 (PA4)-polyurethane (PU)-PA4 triblock copolymers were synthesized by isocynated (NCO)-terminated PU prepared from 4,4'-diphenyl methane diisocyante (MDI) and polytetramethylene glycol (PTMG) as an initiator and potassium pyrrolidonate (P-py) as a catalyst for anionic ring opening polymerization of 2-pyrrolidone. Subsequently copolymer was controlled to contain different or same molecular weight of PA4 hard block with same or different molecular weight of PU soft block in order to investigate the effects of those differences on various properties of triblock copolymers as a thermoplastic elastomer. As the results shown in typical properties of block copolymeric elastomers, the mechanical strength and melting point ($T_m$) of the copolymers increased with an increase in molecular weight of PA4 block while the elongation at break increased with an increase in that of PU block.

• Proceedings of the Korean Society of Propulsion Engineers Conference
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• 2008.05a
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• pp.221-226
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• 2008

Novel synthetic routes were proposed for hydroxy-terminated Poly(EO-co-THF) by Cationic ring-opening copolymerization of Tetrahydrofuran(THF) and Ethylene oxide(EO). It was carried out using Boron trfluoride tetrahydrofuranate($BF_3$ THF complex) as catalyst in the presence of 1,4-butandiol. The resultant products are well-defined linear polyetherpolyol. Polyurethane(TPU) were prepared using resultant polyetherpolyol with IPDI/N-100 as curing agent and TPB(Triphenylbismuth) /MA(Maleic anhydride) mixture as cure catalyst. Mechanical properties of TPU prepared from poly(EO-co-THF) polyol were investigated and compared with polyurethane using ATK HTPE.

• Bulletin of the Korean Chemical Society
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• v.7 no.5
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• pp.372-376
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• 1986

Substituted 3,4-dihydro-2H-pyrans ($1_{a-e}$) were prepared by (4 + 2) cycloaddition reaction of dimethyl dicyanofumarate with the corresponding electron-rich olefins. The compounds $1_{a-e}$ were ring-open polymerized by cationic initiators to obtain polymers of 1:1 alternating sequence. Polymerizations were carried out with boron trifluoride etherate in methylene chloride at $-78^{\circ}C$. All the polymers obtained were soluble in common solvents and were reprecipitated by pouring its chloroform solution into diethyl ether. All the compounds $1_{a-e}$ were not as reactive as the corresponding pyrans derived from ${\alpha}$ -cyanoacrylate.

• Bulletin of the Korean Chemical Society
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• v.9 no.3
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• pp.176-179
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• 1988

3-Methoxy-4-cyano-2,9-dioxabicyclo[4.3.0]non-3-e ne (1) was prepared by (4 + 2) cycloaddition reaction of methyl ${\alpha}$-cyanoacrylate with 2,3-dihydrofuran. Compound 1 was ring-open polymerized by cationic catalyst such as boron trifluoride etherate to obtain alternating head-to-head (H-H) copolymer (2) of methyl $\alpha$ -cyanoacrylate and 2,3-dihydrofuran. For comparison, head-to-tail (H-T) copolymer (3) was also prepared by free radical copolymerization of the corresponding monomers. The H-H copolymer exhibited minor differences in its $^1H$-NMR and IR spectra, but in the $^{13}C$-NMR spectra significant differences were observed between the H-H and H-T copolymers. All of the H-H and H-T copolymers were soluble in common solvents and the inherent viscosities were in the range 0.2-0.3 dl/g.

• Macromolecular Research
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• v.17 no.5
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• pp.346-351
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• 2009

$TiCl(O-i-Pr)_3/SiO_2$ and $Ti(O-i-Pr)_4/SiO_2$ were prepared by immobilizing chlorotitanium (IV) isopropoxide ($TiCl(O-i-Pr)_3$) and titanium (IV) isopropoxide ($Ti(O-i-Pr)_4$), to pretreated silica. The effect of the polymerization reaction conditions on the catalytic activity and characteristics of the resulting PLA were investigated. The catalytic conversion, molecular weight and polydispersity index (PDI) of the PLA produced on the titanium alkoxide supported catalysts increased proportionally with the reaction temperature. When the PLA was synthesized in bulk polymerization, the PLA produced with the supported catalysts had higher molecular weight than those with homogeneous catalysts. The melting temperature of the polymer produced with silica supported alkoxide catalysts was approximately $170-180^{\circ}C$.

• International Journal of Advanced Culture Technology
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• v.3 no.2
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• pp.100-109
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• 2015

Environmental problems from petroleum-based plastic wastes have been rapidly increasing in recent years. The alternative solution is focus on the development of environmental friendly plastic derived from renewable resource. Poly(lactic acid) (PLA) is a biodegradable polymer synthesized from biomass having potential to replace the petroleum-based non-degradable polymers utilizations. PLA can be synthesized by two methods: (1) ring-opening of lactide intermediate and (2) direct polycondensation of lactic acid processes. The latter process has advantages on high yields and high purity of polymer products, materials handling and ease of process treatments. The polymerization process of PLA synthesis has been widely studied in a laboratory scale. However, the mass scale production using direct polycondensation of lactic acid has not been reported. We have investigated the kinetics and scale-up process of direct polycondensation method to produce PLA in a pilot scale. The order of reaction is 2 and activation energy of lactic acid to lactic acid oligomers is 61.58 kJ/mol. The pre-polymer was further polymerized in a solid state polymerization (SSP) process. The synthesized PLA from both the laboratory and pilot scales show the comparable properties such as melting temperature and molecular weight. The appearance of synthesized PLA is yellow-white solid powder.