• Title/Summary/Keyword: polycondensation

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Gas Separation Properties of Polyaniline/Polyimide Blend Membranes (Polyaniline/Polyimide 혼합막의 기체 분리 특성)

  • Lee, Ki-Seob;Kim, Jin-Hwan
    • Applied Chemistry for Engineering
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    • v.18 no.5
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    • pp.483-489
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    • 2007
  • Polyaniline (PANI)/Polyimide (PI) membranes were prepared and the effects of PANI contents and doping on the structural properties and gas separation properties were studied. The polyamic acid (PAA) solution was prepared by the polycondensation reaction of 4,4'-(hexafluoroisopropylidene) diphthalic anhydride (6FDA) and 4,4'-oxydianiline (ODA) in 1-methyl-2-pyrrolydinone (NMP) solvent. The PANI/PI blends were obtained by mixing PAA solution and PANI solution, and were doped with 1 M aqueous HCl solution for 24 h. The structural characterizations of the as-cast and doped membranes were examined by FT-IR, XRD, and TGA. The gas permeation experiments with $H_2$, $CO_2$, $O_2$, $N_2$, and $CH_4$ were carried out by variable pressure method at $30^{\circ}C$ and 5 atm. For all gases tested, the permeability coefficients of the blends decreased with increasing PANI content and the magnitude of permeability was in the order of $H_2$ > $CO_2$ > $O_2$ > $N_2$ > $CH_4$. The permeability for PANI/PI membranes decreased after the doping process while the permselectivity increased. For $H_2/CH_4$ separation, the doped PANI/PI (75/25) membrane has a permselectivity of 991.

Synthesis of Polyamine Type Flocculant and Properties in Potable Water Treatment (Polyamine계 고분자 응집제의 합성 및 상수 처리 특성)

  • Park, Lee-Soon;Shin, June-Ho;Choi, Sang-June;Shin, Myung-Chul;Lee, Seok-Hun
    • Applied Chemistry for Engineering
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    • v.9 no.4
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    • pp.542-547
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    • 1998
  • Polyamine type polymer flocculants were synthesized and their characterization, viscosity and flocculation studies were conducted. In order to increase the molecular weight of polyamine flocculant which was prepared by polycondensation reaction from dimethylamine and epichlorohydrin, a small amount of 1,6-hexanediamine was employed. The incorporation of 1,6-hexanediamine up to 5.5 mole % replacing corresponding part of dimethylamine gave a branched type polyamine sample with increased intrinsic viscosity ([${\eta}$]=0.46 in 1 wt % aqueous NaCl solution). The amount of 1,6-hexanediamine above 5.5 mole %, however, resulted in gelation during polymerization. Utilizing raw water from Maegok potable water treatment plant, it was found that the addition of polyamine flocculant at a concentration of 1 mg/L level could reduce the amount of polyaluminum chloride (PAC) inorganic flocculant by half (15 mg/L). It was also observed that the incoporation of polyamine flocculant at 1 mg/L level was effective in the higher pH raw water, while PAC inorganic flocculating agent alone was not effective.

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Synthesis of Functional Copolyester, its Blend with PET, and Properties of Carbon Black Dry Color (기능성 폴리에스테르 공중합체의 합성, PET와의 블렌드 및 카본 블랙 Dry Color의 물성)

  • Park, Lee Soon;Lee, Dong Chan;Kim, Jin Kon;Huh, Wan Soo
    • Applied Chemistry for Engineering
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    • v.7 no.3
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    • pp.496-503
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    • 1996
  • Aromatic and aliphatic copolyesters for the dispersing agent were synthesized by two stage reaction, esterification and polycondensation. Copolyesters were blended with PET in the melt state and their thermal and rheological properties were investigated. From GPC analysis Mn's and Mw's of copolyesters were about 30000 and 65000g/mol, respectively. From DSC experiment copolyesters had melting range of $90{\sim}150^{\circ}C$. Copolymer composition was in good agreement with comonomer feed ratio from $^1H$-NMR analysis. Copolyesters and SPA (standard sample) were blended with PET in the melt state. From DSC experiment, copolyesters and SPA were miscible with PET. From the dynamic melt viscosity experiment, melt viscosity of blended sample was increased as the content of aromatic copolyester was increased, while it was decreased as the content of aliphatic and SPA were increased. As for volume resistivity of dry color containing carbon black and copolyesters with dispersing time, aromatic copolyester showed highest value. It was conferred from this result that aromatic copolyester was the best dispersing agent for carbon black in PET resin.

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Preparation and Properties of Aromatic Polybenzoxazoles with high char yields (높은 char 수득률를 갖는 방향족 polybenzoxazoles의 제조 및 특성)

  • Sohn, Jun-Youn;Moon, Sung-Chul;Yoon, Doo-Soo;Choi, Jae-Kon
    • Elastomers and Composites
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    • v.42 no.4
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    • pp.238-248
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    • 2007
  • A series of polyhydroxyamides(PHAs) having ether linkages in the polymer backbone were prepared via solution polycondensation at low temperature. These polymers were studied by FT-IR, $^1H-NMR$, DSC, TGA and PCFC. The PHAs exhibited inherent viscosities in the range of $0.5{\sim}1.1dL/g\;at\;35^{\circ}C$ in DMAc solution. Most of PHAs except PHA 3 were soluble in polar organic solvents such as N,N-dimethylacetamide(DMAc), N-methyl-2-pyrrolidone(NMP), and N,N-dimethylform-amide(DMF). Subsequent thermal treatment of PHAs afforded polybenzoxazols(PBOs). However, the PBOs were insoluble in a variety of solvents. Most of the PBOs except PBO 3 showed glass-transition temperature($T_g$) in the range of $200{\sim}246^{\circ}C$ by DSC and maximum weight loss temperature in the range of $597{\sim}697^{\circ}C$ in nitrogen by TGA. PBOs showed high char yields in the range of $51{\sim}64%$. PCFC results of the PBOs showed the heat release(HR) capacity, $8{\sim}65J/gK$ and total heat release(total HR), $2.4{\sim}4.7kJ/g$.

Synthesis and Characterization of Epoxy Silane-modified Silica/Polyurethane-urea Nanocomposite Films (에폭시 변성 실리카 나노입자/폴리우레탄-우레아 나노복합체 필름의 제조 및 특성 연구)

  • Joo, Jin;Kim, Hyeon Seok;Kim, Jin Tae;Yoo, Hye Jin;Lee, Jae Ryung;Cheong, In Woo
    • Korean Chemical Engineering Research
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    • v.50 no.2
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    • pp.371-378
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    • 2012
  • Hydrophilic silica nanoparticles (SNPs) were treated by using 3-glycidoxypropyltrimethoxy silane (GPTMS) and then they were blended with polyurethane-urea (PUU) emulsions to obtain SNPs/PUU nanocomposite films. Thermo-mechanical properties of the nanocomposite films were investigated by varying the grafted amount of GPTMS onto SNPs and the contents of SNPs in the PUU matrix. The thermo-mechanical properties of the nanocomposite films were also compared in terms of the dispersibility of SNPs in the PUU matrix and thermal curing of the GPTMS-grafted SNPs. The maximum amount of grafted GPTMS was $1.99{\times}10^{-6}\;mol/m^2$, and which covered ca. 53% of the total SNP surface area. $^{29}Si$ CP/MAS NMR analyses with the deconvolution of peaks revealed the details of polycondensation degree and patterns of GPTMS in the surface modification of SNPs. The surface modification did not significantly affect colloidal stability of the SNPs in aqueous medium; however, the hydrophobic modification of SNPs offered a favorable effect on the dispersibility of SNPs in the PUU matrix as well as better thermal stability. XRD patterns revealed that GPTMS-grafted SNPs broadened the reduced the characteristic peak of polyol in PUU matrix. The composite films became rigid and less flexible as the SNP content increased from 5 wt.% to 20 wt.%. Particularly, Young's modulus and tensile modulus significantly increased after the thermal curing reaction of the epoxy groups in the SNPs.

Preparation and Flame Retardancy of Poly(benzoxazole imide) Having Trifluoromethyl Group in the Main Chain (주사슬에 Trifluoromethyl 그룹을 갖는 Poly(benzoxazole imide)의 제조 및 난연 특성)

  • Yeom, Jin-Seok;Choi, Jae-Kon;Lee, Chang-Hoon
    • Elastomers and Composites
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    • v.47 no.4
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    • pp.355-363
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    • 2012
  • A series of poly(hydroxyamide)s (PHAs) having trifluoromethyl group were prepared by direct polycondensation of aromatic diimide-dicarboxylic acids with 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane by thionyl chloride and triethyl amine in N-methyl-2-pyrrolidinone (NMP). The PHAs exhibited inherent viscosity in the range of 0.54-0.96 dL/g at $35^{\circ}C$ in DMAc solution. All PHAs were readily soluble in a variety of organic solvents, whereas the polybenzoxazoles (PBOs) were quite insoluble except partially soluble in sulfuric acid. PHAs were converted to PBOs by thermal cycling reaction with heat of endotherm. The maximum weight loss temperature of the PHAs occurred in the range of $559-567^{\circ}C$. The PBOs showed relatively high char yields in the range of 47-59%. Pyrolysis Combustion Flow Calorimeter (PCFC) results of the PBOs showed 12-19 W/g heat release rate (HRR), and 2.7-3.6 kJ/g total heat release (total HR). The HRR of PBO 1 showed the lowest value of 12 W/g, which was 37% lower than that of PBO 3 (19 W/g).

Effects of Types of Catalysts and Solvents on the Water Repellency of Coating Films Prepared from MTMS and TMES (MTMS와 TMES로부터 제조된 코팅 도막의 발수성에 미치는 촉매와 용매 종류의 영향)

  • Kim, Dong Gu;Lee, Byung Wha;Song, Ki Chang
    • Korean Chemical Engineering Research
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    • v.57 no.6
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    • pp.749-757
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    • 2019
  • Methyltrimethoxysilane (MTMS) and trimethylethoxysilane (TMES) as starting materials were dissolved in various types of solvents, and hydrolysis with water and polycondensation reaction were carried out using various types of catalysts to prepare non-fluorinated water-repellent coating solutions. The coating solutions were spin-coated on cold-rolled steel sheets, and thermally cured to prepare water-repellent coating films. The effect of types of catalysts and solvents on the water repellency of the resulting coating films was investigated during this process. When hydrochloric acid and nitric acid, which are strong acids, were used as catalysts, the solutions showed a white opaque state due to the aggregation of siloxane polymers. On the other hand, when acetic acid, phosphoric acid, and oxalic acid, which are weak acids, were used, they were in a stable and transparent state without precipitation. As a result, the contact angles of the coated films, prepared from hydrochloric acid and nitric acid, were $58^{\circ}$ and $92^{\circ}$, respectively, showing low water repellency. On the other hand, when acetic acid, phosphoric acid, and oxalic acid were used, the contact angles of the coated films were $101^{\circ}$, $103^{\circ}$ and $116^{\circ}$, respectively, showing high water repellency. In addition, when isopropanol and ethanol were used as solvents, phase separation occurred in the solutions due to the aggregation of siloxane polymers. On the other hand, when methanol, ethyl acetate, and methyl ethyl ketone were used as solvents, the solutions were transparent and showed a stable state without sedimentation.

On the Properties of TLCP/PBT Blends Prepared by In Situ Polymerization in PBT Solution (In situ 중합에 의해서 제조된 TLCP/PBT 블렌드의 특성 연구)

  • Choi, Jae-Kon;Park, Il-Soo;Kim, Sun;Choi, Yoo-Sung;Lee, Eung-Jae;Jo, Byung-Wook
    • Elastomers and Composites
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    • v.39 no.3
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    • pp.217-227
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    • 2004
  • A new thermotropic liquid crystalline polymer(TLCP) containing a triad aromatic ester type mesogenic unit and butylene terephthalate unit(BT) in the main chain was synthesized by polycondensation reaction. The TLCP synthesized showed nematic mesophasic behavior and its transition temperature from solid to mesophase was $260^{\circ}C$. The TLCP/PBT blends were prepared by in-situ polymerization in PBT solution and characterized by differential scanning calorimeter(DSC), thermogavimetric analyzer(TGA), scanning electron microscope(SEM), x-ray diffractometer(XRD), and dynamic mechanical thermal analyze, (DMTA). The blends showed well dispersed TLCP phases with domain sizes $0.05{\sim}0.2{\mu}m$ in the PBT matrix. As the increasing TLCP content from 5 to 20 wt%, ${\Delta}Hm$ values of pure PBT in the blend were increased because TLCP acts as a nucleating agent in the PBT matrix. The mechanical properties of the blends depended on the TLCP contents because the TLCP acted effectively as a reinforcing material in the PBT matrix. The blends showed good interfacial adhesion between the TLCP phase and PBT matrix.The blends prepared by in-situ polymerization showed higher mechanical properties and well dispersed TLCP domains than those of the blends prepared by melt blending.

Properties of Liquid Crystalline Polyester/Poly(ethylene 2,6-naphthalate) Blend Fibers (액정 폴리에스테르/PEN 블렌드 섬유의 성질)

  • Kim, Won;Kim, Young-Yong;Son, Jung-Sun;Yun, Doo-Soo;Han, Chul;Choi, Jae-Kon;Jo, Byung-Wook
    • Elastomers and Composites
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    • v.37 no.4
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    • pp.244-257
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    • 2002
  • A thermotropic liquid crystalline polymer(TLCP) which has flexible butylene/hexylene spacers in the main chain and a triad aromatic ester type mesogenic unit containing a naphthyl group was prepared by solution polycondensation. The in-situ composites based on poly(ethylene 2,6-naphthalate) (PEN) and a thermotropic liquid crystalline polymer(TLCP) were prepared and melt spun at different TLCP contents and different draw ratios to produce monofilaments. Blends of the TLCP with PEN were investigated in terms of thermal, mechanical properties and morphology. The TLCP synthesized showed nematic mesophasic behavior and its transition temperature to isotropic melt from mesophase was 249℃. The blends showed well dispersed TLCP phases in the PEN matrix without macroscopic phase separation. Inclusion of TLCP in the blends decreased the cold crystallization temperature of PEN in the blend, therefore, the TLCP acts as a nucleating agent in the blend and showed good interfacial adhesion between the dispersed LCP phases and PEN matrix with domain sizes 40~50 nm in diameter and well developed fibrillation in the monofilaments. The TLCP acted effectively as a reinforcing material in the PEN matrix at the 10wt% level, it led to an increase of initial modulus up to 270% and tensile strength by 235%, while the elongation rate increasing with higher draw ratios.