• Korean Chemical Engineering Research
• /
• v.54 no.2
• /
• pp.234-238
• /
• 2016

Solid ash-free coal (AFC) samples recovered from solvent-extracted solution by vacuum drying, dilution precipitation and spray drying methods were compared in terms of physical properties and chemical structure. AFC was prepared by using Kideco coal (Indonesian sub-bituminous coal) and polar N-methyl-2-pyrrolidone (NMP) solvent as raw materials. The physical properties of the AFCs were characterized with proximate, ultimate, and calorific value analysis. In analyzing the chemical structure, FTIR and NMR were used. the proximate analysis showed much reduced ash in the AFCs compared to parent raw coal. The FTIR result showed that the extraction solvent was not fully removed from the AFC prepared by vacuum drying. However, the solvent was not detected in the AFC recovered by using dilution precipitation. Dilution precipitation has advantages over the other two methods, since it can be done at relatively low temperature and separate ash-free coal from extraction solvent more effectively.

• Macromolecular Research
• /
• v.12 no.3
• /
• pp.263-268
• /
• 2004

We have synthesized a water-soluble polyimide precursor, poly(amic acid) amine salt (PAD), from pyromellitic dianhydride (PMDA), 4,4'-oxydianiline, and N,N -dimethylethanolamine (DMEA) and have investigated in detail its properties with respect to the degree of salt formation (D$\_$sf/). The maximum value of D$\_$sf/ we obtained upon precipitation of the precursor solution into acetone was 79%. We synthesized a PAD having a D$\_$sf/ of 100% (PAD100) by the solid state drying of an organic solution. The precursors showed different solubility depending on the D$\_$sf/ to make up to 4 wt% solutions in water containing a small amount of DMEA. PAD100 is completely soluble in pure water. We investigated the imidization behavior of PAD in aqueous solution using various spectroscopic methods, which revealed that PAD 100 has faster imidization kinetics relative to that of the poly(amic acid)-type precursors. The resulting polyimide films prepared from an aqueous precursor solution possess almost similar physical and thermal properties as those prepared from N-methyl-2-pyrrolidone(NMP) solution. Therefore, we have demonstrated that PAD can be used as a water-based precursor of polyimide; this procedure avoids the use of toxic organic solvents, such as NMP.

• Korean Chemical Engineering Research
• /
• v.46 no.5
• /
• pp.965-970
• /
• 2008

The separation of sulfone components using light cycle oil(LCO) after oxidation was carried out by solvent extraction method using various polar solvents such as water, n-methyl-2-pyrrolidone(NMP), dimethyl sulfoxide, ethyl acetate, acetonitrile, dimethyl formamide, and methyl alcohol. It was found that phase separation between LCO layer and solvent occurred under mixed solvent adding a proper amount of water. The mixture solvent of NMP and water was a promising extraction solvent due to the selective removal and high distribution coefficient of sulfone component in LCO. 99.5% over of sulfur contents in LCO can be removed by 4 stages equilibrium extraction.

• Journal of the Korean Electrochemical Society
• /
• v.24 no.4
• /
• pp.106-112
• /
• 2021

Catalyst poisoning by ionomers in membrane electrode assemblies of alkaline membrane fuel cells has been reported recently. We tried to improve the membrane electrode assembly's performance by controlling the solvent's ratio during electrode manufacturing. 4 Different mixing ratios of N-Methyl-2-pyrrolidone (NMP) and ethylene glycol (EG) gave four different cathode electrodes with platinum and Fuma-Tech ionomers. The electrode with higher EG improved polarization performance by about 36% compared to the NMP-based commercial ionomer. The dependence of the ionomer's dispersibility on the solvent seems responsible for the difference, which means that the non-uniform distribution of ionomers improves the performance of the electrode. High-frequency resistance, internal resistance corrected polarization curve, Tafel slope, mass activity, and impedance spectroscopy characterized the electrode. We can find that the existence of poor solvent improves cathode electrode performance. It seems to be the result of reduced poisoning of the catalyst according to the particle size distribution of the ionomer.

• Journal of the Korean Applied Science and Technology
• /
• v.27 no.2
• /
• pp.129-136
• /
• 2010

A series of noble poly(amide-imide)s and copoly(amide-imide)s bearing 1,2-bis(4-phenoxy)benzene units were synthesized by the direct polycondensation of 1,2-bis(4-trimellitimidophenoxy)benzene[1,2-PTPB] with a combination of commercially available aromatic diamines and diacids such as m-phenylene diamine, p-phenylene diamine(PPD), isophthalic acid and terephthalic acid(TA) in N-methyl-2-pyrrolidone(NMP) using triphenyl phosphite and pyridine as a condensing agent in the presence of dehydrating agent ($CaCl_2$). The resulting polymers had inherent viscosities in the range of 0.37~0.78 dL/g and most of them were soluble m common organic solvents including NMP, dimethylacetamide, dimethylsulfoxide, dimethylformamide, and m-cresol. Wide-angle X-ray diffractograms revealed that the copoly(amide-imide) derived from PPD with mixed acids of 1,2-BTPB and TA, showed crystalline nature, whereas all of the other polymers were found to be amorphous. The glass transition temperatures of the polymers occurred over the temperature range of $270{\sim}323^{\circ}C$ in their differential scanning calorimetry curves and their 10% weight loss temperature, determined by thermogravimetric analysis in air and nitrogen atmosphere, were in the range $465{\sim}535^{\circ}C$, $500{\sim}550^{\circ}C$, respectively, indicating their good thermal stability.

• Proceedings of the Membrane Society of Korea Conference
• /
• 2003.07a
• /
• pp.107-114
• /
• 2003

This study investigated the effect of 2-methoxy ethanol (2-Me) non-solvent as additive included in casting solution. Macroporous polymer membranes were prepared by using polyethersufone (PES)/N-methyl-2-pyrrolidone (NMP)/2-Me casting solution and water coagulant. The phase separation co-process of the vapor-induced phase separation (VIPS) and liquid-induced phase separation (LIPS) were used by means of membrane preparation method. The pore size and pore size distribution were controlled with additive (non-solvent), and measured with Automated Perm Porometer. By increasing additive (non-solvent) in the casting solution, the membranes produced changed from finger structure to sponge structure. That is due to the different diffusion rates. At slow diffusion process, sponge-like structure was formed and at fast diffusion process, finger-like structure was formed. Also relative humidity, evaporation time, temperature of casting solution and coagulation bath etc. had effects on the pore size distribution and the porosity of the membrane.

• Carbon letters
• /
• v.16 no.3
• /
• pp.171-182
• /
• 2015

Mesophase pitch is an important starting material for making a wide spectrum of industrial and advanced carbon products. It is produced by pyrolysis of petroleum residues. In this work, mesophase formation behavior in petroleum residues was studied to prepare environmentally-benign mesophase pitches, and the composition of petroleum residues and its influence on the mesophase formation was investigated. Two petroleum residues, i.e., clarified oil s (CLO-1, CLO-2) obtained from fluid catalytic cracking units of different Indian petroleum refineries, were taken as feed stocks. A third petroleum residue, aromatic extract (AE), was produced by extraction of one of the CLO-1 by using N-methyl pyrrolidone solvent. These petroleum residues were thermally treated at 380℃ to examine their mesophase formation behavior. Mesophase pitches produced as a result of thermal treatment were characterized physico-chemically, as well as by instrumental techniques such as Fourier-transform infrared spectroscopy, nuclear magnetic resonance, X-ray diffraction and thermogravimetry/derivative thermogravimetry. Thermal treatment of these petroleum residues led to formation of a liquid-crystalline phase (mesophase). The mesophase formation behavior in the petroleum residues was analyzed by optical microscopy. Mesophase pitch prepared from CLO-2 exhibited the highest mesophase content (53 vol%) as compared to other mesophase pitches prepared from CLO-1 and AE.

• Electrical & Electronic Materials
• /
• v.10 no.1
• /
• pp.54-60
• /
• 1997

The electrical and electromagnetic shielding properties have been investigated in polyaniline free standing films with different degrees of elongation cast from N-methyl 2-pyrrolidone(NMP) solution and camphorsulfonic acid(HCSA) doped polyaniline film. The degree of crystallinity of the crosslinked films increased with increasing the draw ratio. For the case of the oriented films doped with hydrochloric acid, we have the values of conductivities up to 173 S/cm. It is considered that the physical micro-crystalline crosslinking domains act as nucleation sites for the increase of relative crystallinity during stretching. We have obtained the value of conductivity 210 S/cm in the HCSA doped polyaniline film cast from the solvent of m-cresol, which is higher than that of the crosslinking oriented films. The electromagnetic shielding efficiency of HCSA doped polyaniline film obtained 37-41 dB in the frequency range of 10MHz-1GHlz, which is higher than that of the crosslinking oriented films. The higher value of electromagnetic shielding efficiency of HCSA doped polyaniline film suggests strong possibility of electromagnetic shielding material.

• Korean Membrane Journal
• /
• v.3 no.1
• /
• pp.9-16
• /
• 2001

The diamide-diamine having carboxylic acid was prepared by direct condensation of 1,2,4-benzenetricarboxylic acid with bits[4- (3-aminophenoxy ) phenyl] sulfone and bits(4-aminouhenyl)-1,4- diisopropylbenzene in medium consisting of triphenylphosphite, LiCl, and N-methyl-2-pyrrolidone. Copoly (amide-imide) derivatives with high molecular weight could be synthesized by one-step polycondensation of prepared diamide-diamine having carboxylic acid and various dianhydride compounds. Depending on the chemical structure and composition of polymer backbones, the viscosities of polymers were found to range between 0.87∼ 1.57 dL/B. All the polymers showed good thermal stability up to 320$\^{C}$ and the 10% weight loss temperature was observed in the range of 450∼540$\^{C}$ in a thermogravimetric traces. The glass transition was recorded in the temperature range of 200 ∼ 270$\^{C}$. All the polymers showed an amorphous nature on a differential scanning calorimetric thermograms. These polymers generally had good mechanical properties and readily soluble in various polar solvents. Further, it was proved that their properties could be determined from the composition.

• Carbon letters
• /
• v.14 no.4
• /
• pp.251-254
• /
• 2013

In this study, poly(amic acid) was prepared via a polycondensation reaction of 3,3'-dihydroxybenzidine and pyromellitic dianhydride in an N-methyl-2-pyrrolidone solution; reduced graphene oxide/polybenzoxazole (r-GO/PBO) composite films, which significantly increased the electrical conductivity, were successfully fabricated. GO was prepared from graphite using Brodie's method. The GO was used as nanofillers for the preparation of r-GO/PBO composites through an in situ polymerization. The addition of 50 wt% GO led to a significant increase in the electrical conductivity of the composite films by more than sixteen orders of magnitude compared with that of pure PBO films as a result of the electrical percolation networks in the r-GO during the thermal treatment at various temperatures within the films.