• Title/Summary/Keyword: DMAC

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Dry-jet Wet Spinning of Polyhydroxyamide Fibers

  • Park, Seung-Koo;Cho, Seo-Hyun;Farris, Richard-John
    • Fibers and Polymers
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    • v.1 no.2
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    • pp.92-96
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    • 2000
  • A high molecular weight polyhydroxyamide (PHA) solution in N, N-dimethyl acetamide (DMAc) was prepared from 3, 3'-dihydroxybenzidine and isophthalic chloride (IPC), which was used for spinning PHA fiber. Before spinning, the diffusion property of DMAc into various coagulants was examined. The fiber was well formed in coagulants such as water/ethanol with a composition of 5/5, ethanol, and ethanol/isopropanol with a composition of 7/3 and 5/5. However, the PHA fiber spun in the water/ethanol mixture contained voids. After the fiber spun in ethanol was annealed at over $350^{\circ}C$, the ultimate stress and initial modulus of the fiber increased from 75.5 MPa and 3.22 GPa to 369 MPa and 29.5 GPa, respectively. These properties of the PHA fiber spun by the dry spinning method were also enhanced, attaining 154 MPa and 5.56 Gpa, respectivel.

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Synthesis and Characterization of Fluorinated Polybenzoxazole Copolymers

  • Sohn, Jeong Sun;Park, A Ram;Choi, Jae Kon
    • Elastomers and Composites
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    • v.50 no.3
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    • pp.175-183
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    • 2015
  • A series of fluorinated aromatic poly(hydroxyamide)s (PHAs) were synthesized by direct polycondensation of diacides containing 2,6-dimethylphenoxy group and quinoxaline ring in the main chain with 2,2-bis-(3-amino-4-hydroxyphenyl) hexafluoropropane. The PHAs had relatively low inherent viscosities in the range of 0.35~0.43 dL/g at $35^{\circ}C$ in DMAc solution. All PHAs exhibited excellent solubility in aprotic solvents such as NMP, DMAc, DMF and DMSO as well as in common organic solvents such as pyridine, THF, and m-cresol at room temperature. However, the poly(benzoxazole)s (PBOs) were quite insoluble in all organic solvents except partially soluble in concentrated sulfuric acid. The PBOs showed glass transition temperatures between 233 and $284^{\circ}C$ by DSC and maximum weight loss temperatures in the range of $536-546^{\circ}C$ by TGA.

Synthesis and Properties of Polybenzoxazole Copolymers Having Non Linear Units

  • Han, So Hee;Lee, Eung Jae;Choi, Jae Kon
    • Elastomers and Composites
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    • v.54 no.4
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    • pp.321-329
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    • 2019
  • A series of poly(hyroxyamide)s (PHAs) was prepared by direct polycondensation reaction of 4,4'-(2,3-pyridinedioxy)dibenzoic acid and/or isophthalic acid with 3,3'-dihydroxybenzidine. The yield percentages of the products were high, and the inherent viscosities of the polymer in DMAc solution at 35℃ were 0.31-0.59 dL/g. All PHA polymers were found to be soluble in polar aprotic solvents such as DMAc, DMSO, NMP, and DMF. On the other hand, LiCl was required to dissolve IPHA-1 in aprotic solvents. Poly(benzoxazole)s (PBOs) were partially soluble in conc-H2SO4; IPBO-4, -5, and -6 were partially soluble in NMP only when LiCl was added to the solution, and the solution was heated. The PBO polymers showed a maximum weight loss in the temperature range of 654-680℃, and the char yields at 900℃ under nitrogen atmosphere exceeded 63%.

Preparation and Characterization of Wholly Aromatic Polybenzoxazole Copolymers Bearing Ether and Bulky Units

  • Han, So Hee;Lee, Eung Jae;Choi, Jae Kon
    • Elastomers and Composites
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    • v.55 no.3
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    • pp.205-214
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    • 2020
  • A series of wholly aromatic polyhyroxyamide (PHA) copolymers were prepared by direct polycondensation reaction of isophthalic acid and diacids containing bulky units with 3,3'-dihydroxybenzidine. The inherent viscosities of the PHAs measured at 35℃ in DMAc solution were in the range of 0.31-0.56 dL/g. The solubility study revealed that the PHAs were readily soluble in aprotic solvents such as, dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO), and N-methyl-2-pyrrolidone (NMP) at room temperature and in less polar solvent such as pyridine. However, the polybenzoxazole (PBO) copoymers were quite insoluble in all organic solvents except partially soluble in concentrated sulfuric acid and partially soluble in NMP containing LiCl. The PBO copolymers showed maximum weight loss temperature in the range of 593-632℃ and high char yields in the range of 65.0-71.2% at 900℃ in a nitrogen atmosphere.

DFT 계산을 이용한 카이랄 α,β-불포화 N-Acyloxazolidinone에 의한 비대칭 Diels-Alder 고리첨가 반응의 메커니즘 연구

  • Kim, Guk-Hyeon;Kim, Yeon-Jun;Kim, U-Yeon
    • Proceeding of EDISON Challenge
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    • 2013.04a
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    • pp.153-165
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    • 2013
  • 카이랄 ${\alpha},{\beta}$-불포화 N-Acyloxazolidinone은 Diels-Alder 반응의 친다이엔체로서 dialkylaluminium chloride 촉매하에서 높은 반응성과 부분입체선택성을 가지는 것이 이미 실험적으로 알려져 왔다. 제안된 Diels-Alder 반응의 메커니즘을 토대로 진행한 DFT 계산에서 dimethylaluminium chloride(이하 DMAC)는 $TiCl_4$에 비해 높은 endo 선택성을 띄는 반면, $TiCl_4$는 부분입체선택성에서 우세했다. 특히 DMAC는 현저히 낮은 활성화 에너지를 나타내어 이론적으로 반응속도의 측면에서 상당한 이득이 있음을 예측할 수 있다. 또한 chiral auxiliary로서 phenyl과 isopropyl은 구조적인 차이로 인해 선택성에서 역시 차이를 보였다. 계산화학적인 방법을 통한 입체선택적 Diels-Alder 반응의 분석은 알려진 메커니즘에 대한 명확한 증거를 제시할 뿐만 아니라 다른 유기합성 반응에 있어서 새로운 반응을 개발하는 데 이론적인 근거를 뒷받침 한다.

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Preparation and Properties of Polybenzoxazole Copolymers Bearing Pendants and Imide Ring in the Main Chain

  • Lee, Seul Bi;Lee, Eung Jae;Choi, Jae Kon
    • Elastomers and Composites
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    • v.51 no.3
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    • pp.195-205
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    • 2016
  • A series of aromatic poly(hydroxyamide)s (PHAs) containing varying oligo(oxyethylene) substituents and 1,3-phenylene imide ring unit in the main chain were synthesized by the direct polycondensation reaction. The inherent viscosities of the PHAs exhibited in the range of 0.89~1.12 dL/g in DMAc or DMAc/LiCl solution. The PH-2~5 copolymers were easily soluble in strong aprotic solvents: DMAc, NMP, DMSO etc. and the PH-5 copolymer was soluble in less polar solvents such as m-creasol and pyridine with LiCl salt on heating. However, all PBOs were quite insoluble in other solvents, but only partially soluble in sulfuric acid. All copolymers (PH-2~5) could afford the flexible and tough films by solution casting. We identified that the PHAs were converted to the PBOs by the thermal cyclization reaction in the range of $200{\sim}380^{\circ}C$. The 10% weight loss temperatures and char yields of the PBOs were recorded in the range of $382{\sim}647^{\circ}C$ and 38.7~73.1% values at $900^{\circ}C$. The tensile strength and initial modulus of the PH-5 in the copolmers showed the highest values of 2.46 GPa and 49.55 MPa, respectively. The LOI values of the PHAs were in the range 26.6~29.0%, and increased with increasing 1,3-phenylene imide ring unit.

Preparation and Properties of Poly(vinylidene fluoride) Multilayer Films (Poly(vinylidene fluoride) 다층 필름의 제조 및 특성)

  • Son, Tae-Won;Kim, Jong-Hwan;Choi, Won-Mi;Han, Fei-Fei;Kwon, Oh-Kyeong
    • Polymer(Korea)
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    • v.35 no.2
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    • pp.130-135
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    • 2011
  • Along with the fast development of electronics, the demands of portable electronics and wireless sensors are growing rapidly. The need for self-powering materials capable of powering the electrical devices attached to them is increasing, The piezoelectric effect of polyvinylidene fluoride (PVDF) can be used for this purpose. PVDF has a special crystal structure consisting of a ${\beta}$-phase that can produce piezoelectricity. In this paper, multilayer PVDF films were fabricated to increase the ${\beta}$-phase content. A solution of 10% concentration N;N-dimethylacetamide (DMAc) in PVDF (PVDF/DMAc) was used to fabricate the films via spin coating technique with the following optimum process parameters: a spin rate of 850 rpm, spin time of 60 s, drying temperature of $60^{\circ}C$, and drying time of 30 min, Compared with single-layer PVDF films, the multilayer films exhibited higher ${\beta}$-phase content. The ${\beta}$-phase content of the films increased gradually with increasing number of layers until 4, Maximum ratio of ${\beta}$-phase content was 7.72.

Analysis of Thermal Imidization Kinetics of 6FDA-BAPP Polyimide in Relation with Solvent Evaporation (6FDA-BAPP 폴리이미드 열축합 반응에서의 잔류용매에 따른 이미드화거동 연구)

  • Lee, Eun-Young;Hwang, Tae-Seon;Nam, Jae-Do
    • Polymer(Korea)
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    • v.36 no.4
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    • pp.448-454
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    • 2012
  • A poly(amic acid) (PAA) was prepared by reaction of 4,4'-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluropropane (BAPP) in N,N-dimethylacetamide (DMAc). The cast films of the synthesized PAA were thermally treated at different temperatures to create polyimide (PI) films. The heat treatment temperature varied between 80 and $230^{\circ}C$ to investigate the imidization index in relation with the solvent evaporation rates. The progress of PAA imidization was examined using a thermogravimetric analyzer (TGA) and a Fourier transform infrared spectroscope (FTIR) at various time and temperature. The experimental results showed that the imidization index was fast at the initial stage in the presence of solvent, DMAc, reaching the final imidization. When the imidization temperature is high over $200^{\circ}C$, the imidization index decreased because the solvent was evaporated too fast.

Preparation and Characterization of Organic Solvent-resistant Polybenzimidazole Membranes (용매저항성 폴리벤즈이미다졸 분리막의 제조 및 특성평가)

  • Jeong, Moon Ki;Nam, Sang Yong
    • Applied Chemistry for Engineering
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    • v.28 no.4
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    • pp.420-426
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    • 2017
  • Recently, solvent-resistant nanofiltration membranes have been studied for the separation of solvents or solutes using a molecular weight cut-off system of the polymer which is resistant to a specific solvent. Required conditions for these membranes must have are excellent physical properties and solvent resistance. Polybenzimidazole, which is known to be one of the most heat-resistant commercially available polymers, has an excellent inherent solvent resistance and it is even insoluble in stronger organic solvents when cross-linked. Therefore, in this study, the applicability of polybenzimidazole as a solvent resistant nanofiltration membrane was discussed. The membrane was fabricated using the non-solvent induced phase separation method and showed a suitable morphology as a nanofiltration membrane confirmed by field emission scanning electron microscopy. In addition, the permeance of the solvent in the presence or absence of cross-linking was investigated and the stability was also confirmed through long operation. The permeance test was carried out with five different solvents: water, ethanol, benzene, N, N-dimethylacetamide (DMAc) and n-methyl-2-pyrrolidone (NMP); each of the initial flux was $6500L/m^2h$ (water, 2 bar), $720L/m^2h$ (DMAc, 5 bar), $185L/m^2h$ (benzene, 5 bar), $132L/m^2h$ (NMP, 5 bar), $65L/m^2h$ (ethanol, 5 bar) and the pressure between 2 and 5 bar was applied depending on the type of membrane.