• Journal of the Korean Chemical Society
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• v.31 no.3
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• pp.258-270
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• 1987

A series of new thorium nitrate complexes with crown ethers have been synthesized from the reaction of the hydrated thorium nitrate, with the appropriate crown ethers of different cavity sizes in various solvents such as methanol, ethanol, butanol, methylacetate, acetone, tetrahydrofuran and acetylacetone. CHN elemental analysis, ICPAS, thermal analysis and Karl-Fischer method have been used to characterize their compositions, and the spectroscopic methods of IR, UV, $^1H-NMR$, and X-ray diffraction have been employed to determine the structures and solvolysis phenomena of these complexes. and the electrical conductances were measured in DMSO, and water solvent. The solvolysis have been observed only in the complexes synthesized in acetylacetone solvent. In the solvated complexes of 15-crown-5 and 18-crown-6, the mole ratio of $Th^{4+}$: ligand : acetylacetone is found to be 1:1:1, but in the non-solvated complexes of 12-crown-4 and 15-crown-5, the mole ratios of Th:L are 1:2 and 2:3, respectively, and that in the complexes of both 18-crown-6 and dicyclohexano-18-crown-6 is 1:1. All complexes which were not solvated have shown $n{\to}{\sigma}^{\ast}$ electronic transitions of crown ether whereas complexes solvated have exhibited both $n{\to}{\sigma}^{\ast}$ of crown ether and $n{\to}{\pi}^{\ast}$ transitions of acac. The dissociation mole ratio of $Th^{4+}$ and nitrate ion is found to be 1:1 in aprotic solvent, and 1:4 in protic solvent like water.

• Korean Chemical Engineering Research
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• v.49 no.2
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• pp.181-186
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• 2011

In this study, we used 3-(trimethoxysilyl)propylmethacrylate(MPS) silane coupling agent for surface modification of silica nanoparticles. We studied effects of reaction conditions such as solvent pH, MPS hydrolysis time, reaction time, and molar ratio of MPS to Si-OH groups on silica nanoparticle surfaces, on the surface modification reactions of silica nanoparticles. Fourier Transform Infrared Spectroscopy(FTIR), Elemental Analysis(EA) and solid state crosspolarization magic angle spinning(CP/MAS) Nuclear Magnetic Resonance Spectroscopy(NMR) techniques were used to determine the type and the degree of surface modification. We found MPS reacts preferentially with Si-OH groups of the silica nanoparticles as monomeric form at solvent pH = 4.5. But increasing hydrolysis time of MPS from 30 mins to 90 mins, and molar ratio of MPS to Si-OH groups on silica nanoparticle surfaces, we found that MPS reacts preferentially with Si-OH groups of the silica nanoparticles as oligomeric form.

• Polymer(Korea)
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• v.36 no.5
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• pp.668-676
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• 2012

In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to introduce secondary amino groups on the silica surface. After modification of silica, we investigated effects of different types of (meth)acrylate group containing monomers on the Michael addition reaction to introduce reactive (meth)acrylate groups on the BTMA modified silica surface. We used two kinds of (meth)acrylate monomers, trimethylolpropane ethoxylate triacrylate (TMPET) which has three identical acrylate groups, and 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) which has one acrylate and one methacrylate group. We used fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to understand reactions between NH groups on the silica surface with (meth)acrylate groups of TMPET and AHM monomers. We found almost complete Michael addition reaction between all three acrylate groups of TMPET with NH groups on the BTMA modified silica. But, for the AHM treatment of BTMA modified silica, we found Michael addition reaction occurred only between acrylate groups of AHM and NH groups of silica surface, not between methacrylate groups of AHM and NH groups of BTMA modified silica surface.

• Journal of the Korea Institute of Military Science and Technology
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• v.22 no.1
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• pp.35-41
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• 2019

Ferrocene and ferrocene derivatives have been widely used as a burning rate catalyst for composite solid propellants. However, its tendency to migrate through the propellant grain and to crystallize at the surface changes the composition of propellant which results in unpredictable burning rate. To overcome the weakness of ferrocene catalyst, we designed a polymer containing ferrocene, poly(glycidyl azide-co-glycidyl ferrocenyl ether) (GAFP). GAFPs were synthesized from poly(epichlorohydrin-co-glycidyl ferrocenyl ether) (PEGF) which has ferrocenyl ethers in its pendant groups. The structures of GAFPs were confirmed by FT-IR, $^1H$ and $^{13}C$ NMR spectral analyses. Thermal properties of the GAFPs were evaluated using differential scanning calorimeter (DSC). As the contents of ferrocene increased, the glass transition temperature ($T_g$) of the GAFPs shifted to a higher temperature, and the decomposition temperature ($T_d$) decreased because the ferrocene worked as a burning rate catalyst.

• Journal of Energy Engineering
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• v.20 no.1
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• pp.36-43
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• 2011

Plant biomass has been proposed as an alternative source of petroleum-based chemical compounds. Especially, aromatic chemical compounds can be obtained from lignin by depolymerization processes because the lignin consist of complex aromatic materials. In this study, kraft lignin, the largest emitted substance among several kinds of lignin in Korea, was used as a starting material and was characterized by solid-state $^{13}C$-Muclear Magnetic Resonance($^{13}C$-NMR), Fourier Transform Infrared Spectroscopy(FT-IR), Elemental Analysis(EA). The depolymerization of kraft lignin was studied at water-phenol mixture solvent in near critical region and the experiments were conducted using a batch type reactor. The effects of water-to-phenol ratio and reaction temperature($300-400^{\circ}C$) were investigated to determine the optimum operating conditions. Additionally, the effects of formic acid as a hydrogen-donor solvent instead of $H_2$ gas were examined. The chemical species and quantities in the liquid products were analyzed using gas chromatography-mass spectroscopy(GC-MS), and solid residues(char) were analyzed using FT-IR. GC-MS analysis confirmed that the aromatic chemicals such as anisole, o-cresol(2-methylphenol), p-cresol(4-methylphenol), 2-ethylphenol, 4-ethylphenol, dibenzofuran, 3-methyl cabazole and xanthene were produced when phenol was added in the water as a co-solvent.

• Journal of the Korean Chemical Society
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• v.55 no.3
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• pp.436-443
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• 2011

The solid complexes of La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) with 4-hydroxy-3-(1-{2-(2,4-dihydroxy-benzylidene)-amino phenylimino}-ethyl)-6-methyl-pyran-2-one ($H_2$L) derived from o-phenylenediamine, 3-acetyl-6-methyl-(2H)pyran,2,4(3H)-dione (dehydroacetic acid or DHA) and 2, 4-dihydroxy benzaldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, FT-IR, $^1H$-NMR, X-ray diffraction, thermal analysis study, and screened for antimicrobial activity. The FT-IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests distorted octahedral geometry for La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) complexes. The X-ray diffraction data suggests monoclinic crystal system for La(III) and Ce(III) and orthorombic crystal system for Pr(III) and Nd(III) complexes. Thermal behavior (TG/DTA) of the complexes was studied and kinetic parameters were determined by Horowitz-Metzger and Coats-Redfern methods. The ligand and its metal complexes were screened for antibacterial activity against Staphylococcus aureus, Escherichia coli, Bacillus Sp. and fungicidal activity against Aspergillus Niger, Trichoderma and Fusarium oxysporum.

• Journal of the Korean Chemical Society
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• v.53 no.4
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• pp.407-414
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• 2009

The solid complexes of Cu(II), Ni(II), Co(II), Mn(II) and Fe(III) with 4-hydroxy-3-(1-{2-(2-hydroxybenzylidene)- amino phenylimino}-ethyl)-6-methy-pyran-2-one (H2L) derived from o-phenylenediamine, 3-acetyl- 6-methyl-(2H) pyran, 2,4 (3H)-dione (dehydroacetic acid or DHA) and salicylic aldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, IR, $^1H$-NMR spectra, X-ray diffraction, thermal analysis, and screened for antimicrobial activity. The IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests square planar geometry for Cu(II) and Ni(II) complexes and octahedral geometry for Co(II), Mn(II) and Fe(III) complexes. The x-ray differaction data suggests orthorhombic crystal system for Cu(II) complex, monoclinic crystal system for Ni(II), Co(II) and Fe(III) and tetragonal crystal system for Mn(II) complex. Thermal behaviour (TG/DTA) of the complexes was studied and kinetic parameters were determined by Coats-Redfern method. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus Niger and Trichoderma.

• Polymer(Korea)
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• v.37 no.3
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• pp.308-315
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• 2013

In this study, we performed surface modification of silica nanoparticles with bis[3-(triethoxysilylpropyl)]tetrasulfide (TESPT) silane coupling agent to study the effects of treatment temperature, treatment time, and amount of TESPT used on the silanization degree with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), elemental analysis (EA) and solid state $^{13}C$ and $^{29}Si$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR). We found peak area of isolated silanol groups at $3747cm^{-1}$ decreased, but peak area of $-CH_2$ asymmetric stretching of TESPT at $2938cm^{-1}$ increased with the amount of TESPT from FTIR measurements. We also used universal testing machine (UTM) to study mechanical properties of styrene butadiene rubber (SBR) nanocomposites with 20 phr (parts per hundred of rubber) of pristine and TESPT modified silicas, respectively. The tensile strength and 100% modulus of modified silica/SBR nanocomposite were enhanced from 5.65 to 9.38MPa, from 1.62 to 2.73 MPa, respectively, compared to those of pristine silica/SBR nanocomposite.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.18 no.10
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• pp.69-74
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• 2017

In this study, cholesteryl 4-n-alkoxybenzoates (Chol-n), with alkyl groups used for controlling the temperature of transition to the liquid crystal phase, were synthesized, and the effects of the length of the alkyl groups on the physical properties of the liquid crystal compounds were investigated. The chemical structures and thermal and liquid crystalline properties of the synthesized compounds were investigated by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectroscopy ($^1H$-NMR), differential scanning calorimetry (DSC), and polarizing optical microscopy (POM). The synthesized compounds showed melting transition temperatures ($T_m$) in the range of $103^{\circ}C$ to $143^{\circ}C$ and all of the compounds except Chol-6 exhibited a wide liquid crystal phase temperature range of about $60^{\circ}C$ to $100^{\circ}C$. No correlation between the number of carbon atoms in the molecule and the thermal properties of the compounds was found. All of the synthesized compounds showed an enantiotropic cholesteric phase, which was accompanied by a chiral smectic phase in the compounds Chol-6, Chol-8, Chol-9, and Chol-10. All of the compounds exhibited thermochromism in the liquid crystal state, and their color changed from red to blue as the temperature was increased.

• Korean Chemical Engineering Research
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• v.55 no.1
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• pp.60-67
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• 2017

In this study, we performed surface modification of biodegradable microcrystalline cellulose (MCC) to use as a filler in polyethylene (PE) composite in food packaging application. We modified MCC surface with (3-trimethoxysilylpropyl)diethylenetriamine (TPDT) silane coupling agent, which has one primary amino group and two secondary amino groups per molecule, to introduce amino groups with a carbon dioxide adsorption capability in MCC. Effects of each of the reaction conditions such as amount of TPDT introduced, swelling time, reaction temperature, and reaction time on surface modification degree of MCC were investigated by changing a variety of above reaction conditions. The amount of TPDT grafted on MCC surface and formation of chemical bonds were confirmed by Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA) and solid state $^{29}Si$ nuclear magnetic resonance (NMR) spectroscopy. We confirmed increase of grafted amount of TPDT on MCC with increasing reaction time, reaction temperature, and amount of introduced TPDT.