• Applied Chemistry for Engineering
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• v.3 no.4
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• pp.595-604
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• 1992

Carbonate-type polyurethane resins containing anionic moieties were systhesized from NCO-terminated prepolymer method. Membranes were manufactured from the polymer solution and the separation of aqueous ethanol solution was investigated. To enhance the property of urethane resin, carbonate-type polyol(PTMCG) was used. ${\alpha}^{\prime},{\alpha}^{{\prime}{\prime}}$-dimethylolpropionic acid was used as a chain extender to increase the hydrophilicily of the urethane membrane. The ionization of the pendent carboxylic groups in urethane resin was carried out using trimthylamine. To confirm the formation of anionic groups in urethane resin, IR spectra of model compounds were compared with those of urethane resins. It was confirmed that the concentration of hard segment and hydrogen bond contributed to the property of the concentration of hard segment and hydrogen bond contributed to the property of urethane resin in which the mole ratio of chain extender and polyol was from 3:1 to urethane resin in which the mole ratio of chain extender and polyol was from 3:1 to 5:1. The carbonate-type polyurethane containing pendent carboxylic grop(PU) had Tg of around-$25^{\circ}C$ and Tm, $45^{\circ}C$ measured by DSC. Transition temperatures of one containing pendent anionic group(APU) prepared from the ionization of PU shifted to $8{\sim}10^{\circ}C$ lower temperature region than those of PU. Pervaporation membrane was prepared through the casting method. N, N-dimethylformamide (DMF) were used as a solvent and hexamethylene diisocyanate(HMDl) as a crosslinking agent. Swelling degree increased with ethanol concentration in mixure and the control of the swelling degree of the membrane could be achieved by crossliking. The results of pervaporation were as follows : separation factor, 2.3~9.8 ; flux, $27{\sim}79.5g/m^2hr$. Pervaporation separation capacity could be enhanced by reducing the molecular weight of polyol from 2,000 to 1,000.

• Nuclear Medicine and Molecular Imaging
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• v.41 no.3
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• pp.241-246
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• 2007

Purpose: $[^{11}C]6-OH-BTA-1$ ([N-methyl-$^{11}C$]2-(4'-methylaminophenyl)-6-hydroxybenzothiazole, 1), a -amyloid imaging agent for the diagnosis of Alzheimer's disease in PET, can be labeled with higher yield by a simple loop method. During the synthesis of $[^{11}C]1$, we found the formation of by-products in various solvents, e.g., methylethylketone (MEK), cyclohexanone (CHO), diethylketone (DEK), and dimethylformamide (DMF). Materials and Methods: In Automated radiosynthesis module, 1 mg of 4-aminophenyl-6-hydroxybenzothiazole (4) in 100 l of each solvent was reacted with $[^{11}C]methyl$ triflate in HPLC loop at room temperature (RT). The reaction mixture was separated by semi-preparative HPLC. Aliquots eluted at 14.4, 16.3 and 17.6 min were collected and analyzed by analytical HPLC and LC/MS spectrometer. Results: The labeling efficiencies of $[^{11}C]1$ were $86.0{\pm}5.5%$, $59.7{\pm}2.4%$, $29.9{\pm}1.8%$, and $7.6{\pm}0.5%$ in MEK, CHO, DEK and DMF, respectively. The LC/MS spectra of three products eluted at 14.4, 16.3 and 17.6 mins showed m/z peaks at 257.3 (M+1), 257.3 (M+1) and 271.3 (M+1), respectively, indicating their structures as 1, 2-(4'-aminophenyl)-6-methoxybenzothiazole (2) and by-product (3), respectively. Ratios of labeling efficiencies for the three products $([^{11}C]1:[^{11}C]2:[^{11}C]3)$ were $86.0{\pm}5.5%:5.0{\pm}3.4%:1.5{\pm}1.3%$ in MEK, $59.7{\pm}2.4%:4.7{\pm}3.2%:1.3{\pm}0.5%$ in CHO, $9.9{\pm}1.8%:2.0{\pm}0.7%:0.3{\pm}0.1%$ in DEK and $7.6{\pm}0.5%:0.0%:0.0%$ in DMF, respectively. Conclusion: The labeling efficiency of $[^{11}C]1$ was the highest when MEK was used as a reaction solvent. As results of mass spectrometry, 1 and 2 were conformed. 3 was presumed.

• Applied Chemistry for Engineering
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• v.24 no.4
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• pp.370-374
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• 2013

The effects of zinc chloride addition on pore development of porous carbon nanofibers prepared by polyacrylonitrile (PAN)/ N,N'-dimethylformamide (DMF) (10 wt%) electrospinning were investigated. The change of morphological and structural modification by zinc chloride activation was investigated by a scanning electron microscopy (SEM) analysis. $N_2$ adsorption isotherm characteristics at 77 K were confirmed by Brunauer-Emmett-Teller (BET) and Horvath-Kawazoe (H-K) equations, and the curves showed the Type I mode in the International Union of Pore and Applied Chemistry (IUPAC) classification, indicating that lots of micropores exist in the sample. In addition, specific surface areas and total pore volumes of porous carbons prepared by the zinc chloride activation were determined as 600~980 $m^2/g$ and 0.24~0.40 $cm^3/g$, respectively. As experimental results, many holes or demolished structures were found on the fiber surfaces after the zinc chloride activation as confirmed by a SEM analysis. It was also observed that various pore sizes were found to be depended on the adding content of zinc chloride in PAN/DMF solution in this system.

• Applied Chemistry for Engineering
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• v.5 no.4
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• pp.616-623
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• 1994

Conductive Polypyrrole films have been synthesized by electrochemical method in nucleophilic solvent such as N, N-dimetylformamide(DMF), dimethylsulfoxide(DMSO). The effect of protic acid as supporting electrolyte to decrease the nucleophilicity of the solvent was studied. Cyclic voltammetry, I-t transients were carried out to investigate the electrodeposition of conductive polypyrrole film on platinum electrode. Three peaks of 0.65V, 0.85V, and 1.2V vs. $Ag/AgNO_3$ indicated oxidation of monomer, oxidation of pyrrole to the platinum electrode and decomposition of polypyrrole film, respectively. With the I-t transients, nucleation process was confirmed and from obtained linear fits of I vs.t2resembles the metal film formation, and 2.15-2.26 of n-value could be calculated. As concentration of pyrrole or prolic acid was increased, the conductivity of polypyrrole film increased linearly. Tensile strength and elongation were investigated for comparing the mechanical properties and also SEM was performed for morphology investigation.

• Membrane Journal
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• v.6 no.3
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• pp.157-165
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• 1996

Polysulfone(PS) membranes were prepared from homogeneous PS solutions by the phase inversion technique. When propionic acid(PA) was added into a casting solution of n-methylpyrrolidone(NMP) and PS, precipitation rate of the solution film was accelerated. This kind of acceleration was consistent, even though a precipitating nonsolvent was changed from water to isopropanol. These phenomena were caused by decrease of nonsolvent tolerance in the casting solution due to addition of PA. PS powder was prepared by precipitation of a 3wt% solution in dimethylformamide(DMF) using ethanol as nonsolvent. Gas adsorption analysis of the powder showed that the capillary condensation sites were found in the powder structure. Membranes prepared from PS solution(15wt%) in NMP had the following characteristics of gas adsorption and water permeation. In gas adsorption analysis, the membrane precipitated using isopropanol showed low uptake of nitrogen gas and the capillary condensation sites were not found. On the contrary, a significant amount of the capillary condensation sites was found in the membrane coagulated by water, which was related to increase of nitrogen uptake. tn the membrane prepared froin the solution including PA, an increase of the Henry's law sites and the Langmuir sites was not found clearly. However, the capillary condensation sites were significantly increased, and the water transport also increased.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.19 no.8
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• pp.378-384
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• 2018

$C_9H_7NHCrO_3Cl$ was synthesized by reacting $C_9H_7NH$ with chromium (VI) trioxide. The structure of the product was characterized by FT-IR (Fourier transform infrared) spectroscopy and elemental analysis. The oxidation of benzyl alcohol by $C_9H_7NHCrO_3Cl$ in various solvents showed that the reactivity increased with increasing dielectric constant(${\varepsilon}$) in the following order: DMF (N,N'-dimethylformamide) > acetone > chloroform > cyclohexane. The oxidation of alcohols was examined by $C_9H_7NHCrO_3Cl$ in DMF. As a result, $C_9H_7NHCrO_3Cl$ was found to be an efficient oxidizing agent that converts benzyl alcohol, allyl alcohol, primary alcohols, and secondary alcohols to the corresponding aldehydes or ketones (75%-95%). The selective oxidation of alcohols was also examined by $C_9H_7NHCrO_3Cl$ in DMF. $C_9H_7NHCrO_3Cl$ was the selective oxidizing agent of benzyl, allyl and primary alcohol in the presence of secondary ones. In the presence of DMF with an acidic catalyst, such as $H_2SO_4$, $C_9H_7NHCrO_3Cl$ oxidized benzyl alcohol (H) and its derivatives ($p-OCH_3$, $m-CH_3$, $m-OCH_3$, m-Cl, and $m-NO_2$). Electron donating substituents accelerated the reaction rate, whereas electron acceptor groups retarded the reaction rate. The Hammett reaction constant (${\rho}$) was -0.69 (308K). The observed experimental data were used to rationalize hydride ion transfer in the rate-determining step.