• Title/Summary/Keyword: dimethylformamide

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Preparations of PAN-based Activated Carbon Nanofiber Web Electrode by Electrostatic Spinning and Their Applications to EDLC (정전방사에 의한 PAN계 활성화 탄소 나노섬유 전극 제조와 EDLC 응용)

  • Kim, Chan;Kim, Jong-Sang;Lee, Wan-Jin;Kim, Hyung-Sup;Edie, Dan D.;Yang, Kap-Seung
    • Journal of the Korean Electrochemical Society
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    • v.5 no.3
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    • pp.117-124
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    • 2002
  • Poly(acrylonitrile)(PAN) solutions in dimethylformamide(DMF) were electrospun to prepare webs consisting of 400nm ultra-fine fibers. The webs were oxidatively stabilized, activated by steam and resulted to be activated carbon fibers(ACFs). The specific surface area was $800\~1230 m^2/g$, which showed a trend of a decrease of the surface area with an increase in activation temperature, showing opposite behavior to the other ACFs. The activation energy of the stabilized fibers for the steam activation was determined as 29.2 kJ/mol to be relatively low indicating the easier activation than that of other carbonized fibers. The ACF webs were characterized by pore size and specific surface uea which would be related to the specific capacitance of the electrical double layer capacitor (EDLC). The specific capacitances measured were 27 F/g, 25 F/g, 22 F/g at the respective activation temperature of $700^{circ}C,\;750^{\circ}C\;800^{\circ}C$, showing similar trend with the specific surface area i.e., the higher activation temperature was, the lower specific capacitance resulted.

Radiation Resistance and Fabrication of Carbon Fiber Reinforced Thermoplastic Composites by Electropolymerization (전기중합법에 의한 열가소성 수지 탄소섬유 강화 복합재료의 제조와 내방사선성)

  • Park, Minho;Kim, Minyoung;Kim, Wonho;Cho, Wonjei
    • Applied Chemistry for Engineering
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    • v.8 no.3
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    • pp.489-501
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    • 1997
  • Electropolymerization of 2-vinylnaphthalene (2-VN) and methylmethacrylate (MMA) with high radiation resistance property was conducted on the surfaces of carbon fibers by using a nonaqueous solution of comonomers dissolved in N,N-dimethylformamide containing sodium nitrate as a supporting electrolyte. The fabrication of carbon fiber/2-VN/MMA prepreg was performed electrochemically in 1:1 comonomer solution. Electropolymerization was conduced by changing the current density, initial comonomer concentration, and reaction time. The weight gain on the surface of the carbon fibers was measured by thermogravimetric analyser (TGA). The highest weight gain of 50 wt% was obtained at 600mA/g~800mA/g current density range, but the weight gain was rapidly decreased above 800mA/g current density. The weight gain was increased with the concentration of comonomer, while the concentration of electrolyte had almost no effect on the weight gain. At 300mA/g current density, weight gain rate was increased abruptly to the initial 30 minutes of reaction time. After that the rate was decreased due to the generation of gas bubbles. In order to check the effect of coated polymers on the radiation resistance, morphology changes before and after $\gamma$-ray irradiation was investigated for the composites.

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Exchange Reaction Mechanism of $Pb(II)-N_2O_m$ Macrocyclic Complexes by $^{207}Pb-NMR$ Spectroscopy ($^{207}Pb-NMR$ 분광법에 의한 $Pb(II)-N_2O_m$계 거대고리 리간드 착물형성 반응의 교환 메카니즘)

  • Kim, Jeong;Yun, Chang Ju;Yu, Han Jun;Kim, Geon;Kim, Si Jung
    • Journal of the Korean Chemical Society
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    • v.38 no.1
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    • pp.41-49
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    • 1994
  • Exchange reaction mechanisms of the Pb(II) ion for the complexes between Pb(II) ion and nitrogen oxygen donor macrocyclic ligands, such as 1,13-diaza-3,4 : $1011-dibenzo-59-dioxacyclohexa-decane(NtnOtnH_4)$, 1,15-diaza-3,4 : $1213-dibenzo-5811-trioxacycloheptadecane(NenOdienH_4)$, and 1,15-diaza-3,4 : $1213-dibenzo-5811-trioxacyclooctadecane(NtnOdienH_4)$, were studied by $^{207}Pb-NMR$ spectroscopy in N,N'-dimethylformamide(DMF) solutions. The associative-dissociative mechanism dominated in $NtnOtnH_4-Pb(II)$ and $NtnOdienH_4-Pb(II)$ system. For $NenOdienH_4-Pb(II)$ system, the bimolecular exchange mechanism prevailed below $-5^{\circ}C$, and both bimolecular exchange and associative-dissociative mechanism dominated above $+5^{\circ}C.$ The order of activation energies for dissociation was $NtnOdienH_4\;<\;NtnOtnH_4\;<\;NenOdienH_4$ which was reverse to the order of stabilities.

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Complexation of Pyridino-Azacrown Ethers with Alkali Metal Ions in N,N-Dimethylformamide (N,N-디메틸포롬아미드 용액에서의 알칼리금속이온과 피리디노-아자크라운에테르와의 착물화 반응)

  • Kim, Dong Won;Shin Young-Kook;Kim Chang Suk;Oh Je Jik;Jeon Young Shin;Kim, Tae Seung
    • Journal of the Korean Chemical Society
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    • v.36 no.5
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    • pp.669-673
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    • 1992
  • The stability constants, K for the complexation of alkali metal cations(Li^+, Na^+, K^+, Rb^+, and Cs^+) with both 4,5: 13,14-dibenzo-6,9,12-triaza-bicyclo [15,3,1] heneicosa-1 (21),7,19-trioxa-2,16-dione (DBPDA) and 6,9,12-trioxa-3,15,21-triaza bicyclo [15,3,1] heneicosa-1 (21),17,19-triene-2,16-dione (PDA) in N,N-Dimethylformamide (DMF) were determined conductomatically at various temperatures. At all the experiment temperatures, the K value sequences of the alkali metal ions with DBPDA and PDA are Cs^+ > K^+ > Rb^+ > Li^+ > Na^+ and Cs^+ > K^+ > Rb^+ > Li^+ > Na+, respectively. The K values for DBPDA are larger those of PDA for alkali metal ions. The widely recounted "hole-size-selectivity" principle is not applicable to these complexation systems. From the K values obtained at different temperatures, {\delta}H and T{\delta}S for these complexation reactions were determined. The enthalpy change plays principal important role in the complex formation by DBPDA. However, in the case of PDA, the entropy change also contributes to its complex formation.

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Effects of Annealing Temperature on Thermal Properties of Glycidyl Azide Polyol-based Energetic Thermoplastic Polyurethane (글리시딜아자이드계 열가소성 폴리우레탄의 열적특성에 대한 열처리 조건의 영향)

  • Kim, Jeong Su;Kim, Du Ki;Kweon, Jeong Ohk;Lee, Jae Myung;Noh, Si Tae;Kim, Sun Young
    • Applied Chemistry for Engineering
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    • v.24 no.3
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    • pp.305-313
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    • 2013
  • In this study, we investigated effects of thermal annealing on the thermal properties and microphase separation behaviors of glycidyl azide-based thermoplastic polyurethane elastomers (ETPE). The GAP-based ETPEs were characterized by attenuated total reflectance-fourier transform infrared spectroscopy (ATR-FTIR), differential scanning calorimeter (DSC), dynamic mechanical analysis (DMA), and gel permeation chromatography (GPC). The effects of annealing temperature conditions ($80{\sim}130^{\circ}C$, 1 h or 24 h) on the properties of the ETPEs were investigated. The intensity of azide group absorption peak of ATR-FTIR spectra and the solubility of ETPE for methylene chloride and dimethylformamide solvent decreased after the annealing at $130^{\circ}C$ for 1 h and at $105^{\circ}C$ for 24 h. With increasing the annealing temperature from $80^{\circ}C$ to $110^{\circ}C$, the high temperature rubbery plateau region of storage modulus curves from DMA thermogram for GAP-based ETPEs was extended to the higher temperature.

Kinetics of the Reaction of Phenacyl Bromide with Anilines in Methanol and Dimethylformamide (Phenacyl Bromide와 置換아닐린類와의 反應에 關한 反應速度論的 硏究)

  • Soo-Dong Yoh;Doo-Jung Kim
    • Journal of the Korean Chemical Society
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    • v.25 no.6
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    • pp.376-382
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    • 1981
  • The rates and the activation parameters for the reaction of phenacyl bromide with substituted anilines in methanol and dimethylformamide were measured. The effects of substituted anilines were discussed. The rate of the reaction was increased with the electron donating power of substituent and showed larger value in DMF than in MeOH. The isokinetic relationship was shown between ${\delta}H^{\neq}$ and ${\delta}S^{\neq}$, isokinetic temperature was 539 and $400^{\circ}C$ in MeOH and DMF respectively, but p-nitro aniline was deviated from linearity in both solvents caused by solvent effects. The excellent linear relationship between log k and p$K_a$ of substituted anilines was observed by following equation. log k = 0.57p$K_a$-1.28 (r = 0.996) in MeOH at $45^{\circ}C$, log k = 0.65p$K_a$-0.88 (r = 0.970) in DMF at $45^{\circ}C$. From the Hammett plot, this reaction was a nucleophilic displacement of aniline to phenacyl bromide and the following equation was obtained at $45^{\circ}C$. log k/$k_0$ = -2.00${\sigma}$ + 0.06 (r = 0.985) in MeOH; log k/$k_0$ = -2.22${\sigma}$ + 0.08 (r = 0.995) in DMF. Large deviation of p-nitro aniline in DMF is resulted from solvent effects too. From above results, the substituent effect of this reaction can be described as $S_N2$ mechanism and bond formation more proceeds in DMF relative to MeOH.

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Synthesis and Characterization of Porous Poly(ε-caprolactone)/Silica Nanocomposites (다공성 폴리(ε-카프로락톤)/실리카 복합체의 제조 및 특성평가)

  • Son, Siwon;Choi, Ji-Eun;Cho, Hun;Kang, DaeJun;Lee, Deuk Yong;Kim, Jin-Tae;Jang, Ju-Woong
    • Polymer(Korea)
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    • v.39 no.2
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    • pp.323-328
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    • 2015
  • Poly(${\varepsilon}$-caprolactone) (PCL) nanofibers and PCL/silica membranes were synthesized by sol-gel derived electrospinning and casting, respectively. Smooth PCL nanofibers were obtained from the precursor containing N,N-dimethylformamide (DMF). PCL/silica membranes were prepared by varying the tetraethyl orthosilicate (TEOS) contents from 0 to 40 vol% to investigate the effect of silica addition on mechanical properties and cytotoxicity of the membranes. Although the strength of the membranes decreased from 12 to 8 MPa with increasing the silica content, the strength remained almost constant 7 weeks after dipping in phosphate buffered saline solution (PBS). The strength reduction was attributed to the presence of a patterned surface pores and micro-pores present in the walls between pores. The crystal structure of the membranes was orthorhombic and the crystallite size decreased from 57 to 18 nm with increasing the silica content. From the agar overlay test, the PCL/silica membranes exhibited neither deformation and discoloration nor lysis of L-929 fibroblast cells.

Studies on the Quaternization of Tertiary Amines (Ⅱ). Kinetics and Mechanism for the Reaction of Substituted Phenacyl Bromides with Substituted Pyridines (3차 아민의 4차화반응에 관한 연구 (제2보). 치환 브롬화페나실류와 치환 피리딘류와의 반응에 관한 반응속도론적 연구)

  • Yoh Soo Dong;Kwang Taik Shim;Lee Kyung A
    • Journal of the Korean Chemical Society
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    • v.25 no.2
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    • pp.110-118
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    • 1981
  • Kinetics and mechanism for the reaction of substituted phenacyl bromides with substituted pyridines have been determined at 25, 35 and $45^{\circ}C$ in methanol and dimethylformamide by the conductivity method. The rate constants for the reaction of various pyridines with phenacyl bromide shown that electron-donating substituents in the pyridine increase the rate, while electron-attracting one decrease in both solvents. The effect of substituents in substrate, the rate being increased by electron-attracting substituents. This is as expected for nucleophilic attack of amines on the carbon atom. Isokinetic and $Br{\psi}nsted$ linear relationship were shown in the reaction of phenacyl bromide with pyridines in both solvent in which isokinetic temperature were obtained 614, $202^{\circ}K$ and ${\beta}$ values were 0.29, 0.36 in methanol and dimethylformamide respectively. In the case of the reaction of substituted phenacyl bromide with pyridines, isokinetic temperature decreases with increasing electron-attracting ability of the substituents in the phenacyl bromide, while the ${\beta}$ values were reverse. From the above results, it can be inferred that N…C bond formation decreases progressively from p-chloro- to p-methoxyphenacyl bromide and the bond formation predominates in DMF than methanol. The ${\rho}$ values of Hammett equation of the reaction of phenacyl bromide with substituted pyridines are negative in both solvent, but its value was larger negative in DMF than methanol and the ${\rho}$ value of that of substitutted substrates with pyridine was 0.3, the low value is ascribed to direct $S_N2$ attack of the nitrogen atom in pyridine ring at the methylene carbon.

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Preparation of Poly(imide-aramid-sulfone)s and their Thermal Properties (폴리(이미드-아라미드-설폰)의 합성과 그들의 열적성질)

  • Park, Hyung-Seok;Gong, Myoung-Seon
    • Polymer(Korea)
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    • v.36 no.4
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    • pp.427-433
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    • 2012
  • A series of poly(imide-aramid-sulfone)s with alternatingly introduced imide/aramid groups were prepared by reacting divinyl sulfone (DVS) and $N^1,N^4$-bis(4-(vinylsulfonyl)phenyl)terephthalamide (2) with pyromellitic diimide. Three model compounds, N-[2-(p-aminophnenylsulfonyl)ethyl]phthalimide (3), 2,2'-(2,2'-sulfonylbis(ethane-2,1-diyl))diisoindoline-1,3-dione (4), and N,N-bis(4-(2-(1,3-dioxoisoindolin-2-yl)ethylsulfonyl)phenyl)terephthalamide (5), resembling polymers were prepared with good yields by reacting p-aminophenyl vinyl sulfone, DVS, and 2 with phthalimide. Condensation polymerization was carried out by Michael-type addition reaction of the difunctional phthalimide group with the DVS group in the presence of tetrabutylammonium hydroxide (TBAH), resulting in poly(imide-aramid-sulfone)s 6-12 with moderate molecular weights and good yields. They were highly soluble in polar solvents such as N,N-dimethylformamide, dimethylsulfoxide, N-methylpyrrolidinone and tetrahydrofuran. The ratios of DVS/2 were 1/0, 3/1, 2/1, 1/1, 1/2, 1/3, and 0/1. Molecular weight and physical properties such as solubility, viscosity, and thermal properties of the polymers were examined.

Optimization of MOF-801 Synthesis Using Sequential Design of Experiments (순차적 실험계획법을 이용한 MOF-801 합성공정 최적화)

  • Lee, Min Hyung;Yoo, Kye Sang
    • Applied Chemistry for Engineering
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    • v.32 no.6
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    • pp.621-626
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    • 2021
  • A sequential design of experiments was used to optimize MOF-801 synthesis process. For the initial screening, a general 2k factorial design was selected followed by the central composition design, one of the response surface methods. A 23 factorial design based on the molar ratio of fumaric acid, dimethylformamide (DMF), and formic acid was performed to select the more suitable response variable for the design of experimental method among the crystallinity and BET specific surface area of MOF-801. After performing 8 synthesis experiments designed by MINITAB 19 software, the characteristic analysis was performed using XRD analysis and nitrogen adsorption method. The crystallinity with R2 = 0.999 was found to be more suitable for the experimental method than that of BET specific surface area. Based on analysis of variance (ANOVA), it was confirmed that the molar ratio of fumaric acid and formic acid was a major factor in determining the crystallinity of MOF-801. Through the response optimization and contour plot of two factors, the optimal molar ratio of ZrOCl2·8H2O : fumaric acid : DMF : formic acid was 1 : 1 : 39 : 35. In order to optimize the synthesis process, the central composition design on synthesis time and temperature was performed under the identical molar ratio of precursors. The results derived through the designed 9 synthesis experiments were calculated using the quadratic model equation. Thus, the maximum crystallinity of MOF-801 predicted under the synthesis time and temperature of 7.8 h and 123 ℃, respectively.