• Title/Summary/Keyword: polycondensation

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Synthesis and Properties of Linear and Star-shaped poly(L-lactic acid)s by Direct Solution Polycondensation (직접 용액 축중합에 의한 직쇄형 및 스타형 폴리락트산의 합성과 물성)

  • Kim, Wan Jung;Lee, Sun Young;Kim, Ji-Heung;Kim, Soo Hyun;Kim, Young Ha
    • Applied Chemistry for Engineering
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    • v.10 no.7
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    • pp.1028-1034
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    • 1999
  • Poly(lactic acid) is expected to be one of the most promising biodegradable polymers. However, the high molecular weight polymer could be obtained by ring-opening polymerization process conventionally, which raises the production cost and decreases the final yield. In this study, linear and star-shaped poly(L-lactic acid)s were prepared by direct solution polycondensation method and their physical and thermal properties were examined. Tin compounds were found to be effective catalyst for the preparation of high molecular weight polymers. When 0.2g (0.5 wt % of monomer) of $SnCl_2$ and 100 mL of p-xylene were used, the polymer yield and molecular weight were relatively high. As a means to obtain higher molecular weight polymer easily in the direct polycondensation system, dipentaerythritol(dipet) or pentaerythritol(pet) was introduced as a multifunctional branching monomer to provide a star-shaped poly(lactic acid). Moderately high molecular weight polymers with the inherent viscosity values up to 1.14 dL/g(weight-average molecular weight of about 140000 by GPC) were obtained and could be cast strong and transparent films.

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Synthesis and Characterization of Cationic and Anionic Cyclodextrin Oligomers and Their Use in Layer-by-Layer Film Formation

  • Yang, Sung Yun;Hoonor, Rekha;Jin, Hye-Seung;Kim, Jeongkwon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.7
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    • pp.2016-2022
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    • 2013
  • Ionically modified ${\beta}$-cyclodextrins, which have excellent water-solubility, have been interested in purification technology as well as drug carrier system. The present study summarizes the synthesis and characterization of cationic and anionic ${\beta}$-cyclodextrin (${\beta}$-CyD) products using by polycondensation. The oligo (${\beta}$-CyD)s are synthesized from ${\beta}$-CyD, epichlorohydrin (EP) and choline chloride (CC; for cationic polymer) or chloroacetic acid (CAA; for anionic polymer) through one step polycondenstaion process. Unlike the previous studies, we successfully purified the ionic ${\beta}$-CyD condensation products from the ${\beta}$-CyD reaction mixtures and accomplished a great level of structural analysis. The detailed structural analysis of these ionic ${\beta}$-CyD compounds is done by $^1H$ NMR, MALDI-TOF as well as GPC analysis and confirms the formation of oligomers with a few units of ${\beta}$-CyD. We found that the sequence of reactant addition also could effect on the molecular weight of the resulting product as well as the molar ratio of the reactants. Finally, we used the cationic and anionic ${\beta}$-CyD oligomers for fabricating multilayer films by layer-layer process.

Properties of Poly(benzoxazole) Copolymer Films Containing Quinoxalinedioxy/Pyridinedioxy Unit

  • Park, A Ram;Lee, Eung Jae;Choi, Jae Kon
    • Elastomers and Composites
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    • v.52 no.2
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    • pp.143-153
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    • 2017
  • Herein we studied the characterization of the PBO films formed via solution casting and thermal cyclization of poly(o-hyroxyamide)s(PHAs) that were synthesized by direct polycondensation of 3,3'-dihydroxybenzidine with 4,4'-(2,3-quinoxalinedioxy) dibenzoic acid and/or 4,4'-(2,3-pyridinedioxy) dibenzoic acid. All the PHAs exhibited inherent viscosities in the range of 0.55~0.84 dL/g in DMAc solution. The copolymers, CPH-2-5, were partially soluble in less polar solvents like pyridine and THF. However, all the PBOs were not soluble in polar solvents, but only partially soluble in sulfuric acid. The temperatures corresponding to 10% weight loss of the PBOs with increasing content of quinoxalinedioxy unit were higher than those of the PHAs, and the char yields at $900^{\circ}C$ in $N_2$, tensile strength, and initial modulus of the PBOs were 1.1~1.3 times, 1.2~1.8, and 1.6~3.3 times higher, respectively, than those of the PHAs. The LOI value of CPB-2 was 38.5%, while that of CPB-1 was the highest at 40.0%. The LOI test confirmed that excellent flame retardants were synthesized.

Effect of Curing Temperature on Geopolymeric Polycondensation of Blast Furnace Slag (고로슬래그의 지오폴리머 축중합반응에 미치는 양생온도의 영향)

  • Jeon, Chang-Seob;Song, Tae-Woong
    • Journal of the Korean Ceramic Society
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    • v.48 no.6
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    • pp.610-616
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    • 2011
  • The effect of curing temperature on basic geopolymeric reactivity and hardening behaviour of blast furnace slag were investigated using the mixture of pulverized slag and several alkaline solutions of relatively high concentration. For the pastes prepared at several different temperatures between 20$^{\circ}C$ and 90$^{\circ}C$, setting time and heat of reaction were examined while mineralogical and morphological examinations were performed for the hardened paste after curing period at same temperature. The geopolymeric reaction of slag was revealed to be accelerated strongly according to the curing temperature regardless of the sort and concentration of the alkaline solution. The increase of concentration of the alkaline solution within 9M and the existence of silicic ion in the solution also promoted the reaction severely. The mineral component and their ratio of the hardened paste were revealed to be influenced by the chemical species and silicic ion contained in alkaline solution rather than by the curing temperature. The higher temperature and longer period of curing stage were effective for the sustained formation of geopolymer and succeed improvement of density and uniformity of morphology of the final hardened body.

Synthesis and Thermal Properties of Poly(benzoxazole)s Based on Pendants

  • Jang, Hyewon;Lee, Seulbi;Choi, Jae Kon
    • Elastomers and Composites
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    • v.50 no.2
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    • pp.138-145
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    • 2015
  • A series of wholly aromatic poly(hydroxyamide)s(PHAs), containing varying amounts of 2,6-dimethylphenoxy group and quinoxaline ring in the main chain, were synthesized by a direct polycondensation method. The inherent viscosities of the PHAs in either DMAc or DMAc/LiCl solution at $35^{\circ}C$ were found to be in the range of 1.02~1.90 dL/g. In the solubility study, we observed that PHA 1, PHA 2, and PHA 3 were dissolved in aprotic solvents such as DMAc, NMP, DMF, and DMSO with LiCl on heating; however, PHA 4, PHA 5, and PHA 6 could be dissolved in aprotic solvents on heating without LiCl. For poly(benzoxazole)s(PBOs), the 10% and maximum weight loss temperatures were in the range of $582{\sim}622^{\circ}C$ and $630{\sim}659^{\circ}C$, respectively. Residues of PBOs at $900^{\circ}C$ were found to be relatively high, which were in the range of 65.3~70.8%.

Synthesis and Thermal Properties of Wholly Aromatic Poly(benzoxazole)s

  • Han, So Hee;Lee, Eung Jae;Choi, Jae Kon
    • Elastomers and Composites
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    • v.53 no.3
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    • pp.141-149
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    • 2018
  • A series of aromatic poly(o-hydroxyamide)s (PHAs) were synthesized by the direct polycondensation reaction of 4,4′-(2,3-quinoxalinedioxy) dibenzoic acid and/or 4,4′-(2,3-pyridinedioxy) dibenzoic acid with bis(o-aminophenol) including 2,2-bis-(amino-4-hydroxyphenyl)hexafluoropropane. The PHAs exhibited inherent viscosities in the range of 0.17-0.35 dL/g at $35^{\circ}C$ in a DMAc solution. These polymers showed low inherent viscosities and yielded brittle films. All the PHAs showed excellent solubility in aprotic solvents such as DMAc, DMSO, NMP, and DMF at room temperature and in less polar solvents such as pyridine and THF. However, all the PBOs were only partially soluble in $H_2SO_4$. The PBOs exhibited 10% weight loss at temperatures in the range of $537-551^{\circ}C$. The maximum weight loss temperature increased with an increase in the content of the quinoxaline-containing monomer. The residue of the PBOs showed a weight loss of 45.8-56.7% at $900^{\circ}C$ in a nitrogen atmosphere.