• 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 Academia-Industrial cooperation Society
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• v.20 no.5
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• pp.1-6
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• 2019

Organic dye-doped silica nanoparticles are used as a promising nanomaterials for bio-labeling, bio-imaging and bio-sensing. Fluorescent silica nanoparticles(NPs) have been synthesized by the modified $St{\ddot{o}}ber$ method. In this study, dye-free fluorescent silica NPs of various sized were synthesized by Sol-Gel process as the modified $St{\ddot{o}}ber$ method. The functional material of APTES((3-aminopropyl)triethoxysilane) was added as an additive during the Sol-Gel process. The as-synthesized silica NPs were calcined at $400^{\circ}C$ for 2 hours. The surface morphology and particle size of the as-synthesized silica NPs were characterized by field-emission scanning electron microscopy. The fluorescent characteristics of the as-synthesized silica NPs was confirmed by UV lamp irradiation of 365 nm wavelength. The photoluminescence (PL) of the as-synthesized silica NPs with different size was analyzed by fluorometry. As the results, the as-synthesized silica NPs exhibits same blue fluorescent characteristics for different NPs size. Especially, as increased of the silica NPs size, the intensity of PL was decreased. The blue fluorescence of dye-free silica NPs was attributed to linkage of $NH_2$ groups of the APTES layer and oxygen-related defects in the silica matrix skeleton.

• Clean Technology
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• v.17 no.1
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• pp.13-18
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• 2011

Phosphine ligand-grafted mesoporous silica materials with large pores were prepared for the ligand-modified heterogeneous Pd nanocatalysts. New heterogeneous catalytic system was developed using palladium nanoparticles encapsulated in phosphine ligand-grafted mesoporous silica. The catalyst showed good catalytic activities for Suzuki cross-coupling using bromobenzene derivatives due to excellent phosphine ligand effects. Catalytic results showed nanoparticie catalysts can be recycled twice with decreased yields.

• Polymer(Korea)
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• v.28 no.6
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• pp.487-493
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• 2004

The distribution of particles, in the mixture of poly(ethyl acrylate-co-t-butyl acrylate) (PEB) emulsion polymer and silica nanoparticles, was determined mainly depending on the pH of the mixture. The weak interfacial interaction was responsible for the severe coagulation of silica particles and the irregular dispersion for these nanocomposites. Methacryloxypropyltrimethoxysilane (MPS) was used to modify both the polymer and the silica. The nanocomposites which were prepared with these modified components had finer dispersion of silica nanoparticles and core-shell morphology due to the strong interfacial interaction. The strong hydrogen bonds were identified for these nanocomposites with FT-IR. The nanocomposites having strong interfacial interaction showed the increased glass transition temperature, the decreased ΔC$_{p}$ , and the increased decomposition temperature of the polymer chains. polymer chains.

• 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.

• Proceedings of the Korean Society of Precision Engineering Conference
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• 2012.10a
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• pp.475-476
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• 2012

• Bulletin of the Korean Chemical Society
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• v.29 no.10
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• pp.1932-1936
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• 2008

A new analytical method using 1-(2-pyridylazo)-2-naphthol modified $SiO_2$ nanoparticles as solid-phase extractant has been developed for the preconcentration of trace amounts of mercury(II) in different water samples. Conditions of the analysis such as preconcentration time, effect of pH, sample volumes, shaking time, elution conditions and effects of interfering ions for the recovery of analyte were investigated. The adsorption capacity of nanometer $SiO_2$-PAN was found to be 260 ${\mu}molg^{-1}$ at optimum pH and the detection limit (3$\sigma$) was 0.48 ${\mu}gL^{-1}$. The extractant showed rapid kinetic sorption. The adsorption equilibrium of mercury(II) on nanometer $SiO_2$-PAN was achieved just in 5 mins. Adsorbed mercury(II) was easily eluted with 5 mL of 6 M hydrochloric acid. The maximum preconcentration factor was 50. The method was applied for the determination of trace amounts of mercury(II) in various water samples and industrial effluents.

• Polymer(Korea)
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• v.36 no.3
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• pp.372-379
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• 2012

In this study, we treated silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify their surfaces. We investigated the effects of BTMA hydrolysis time, BTMA concentration and BTMA treatment time on the degree of silanization reaction of silica nanoparticles. 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 obtain quantitative data. We found the decrease of isolated Si-OH peak intensity at 3747 $cm^{-1}$ and the increase of $-CH_2 $stretching and bending peaks with increasing hydrolysis time, concentration and treatment time of BTMA. EA analysis results also supported this trend. We found a strong effect of BTMA concentration on the degree of silanization of the silica particles, but weak effects of the hydrolysis time and the treatment time.

• Korean Chemical Engineering Research
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• v.46 no.4
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• pp.722-726
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• 2008

Silica microsphere is a world leading innovative material used in adsorbent packing materials in HPLC technology. The application of microsphere lies in the ability to the surface modification of silica with the special materials such as polymers, metals and bio-active materials. Collagen is a major structural protein of connective tissues and has a good biocompatibility. In this study, we prepared the purified silica porous microsphere, having micro diameters in the range of a pore volume at least 50% by the aggregation procedure of colloidal silica with the polymerization method (PICA). The microspheres were modified by collagen hydrogel to improve the biocompatible properties for biomedical product. The silica/collagen microsphere composite doped with silver nanoparticles was prepared and investigated the capabilities of biomaterial application through the evaluation of the structure characteristics of the microsphere composit.

• Polymer(Korea)
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• v.39 no.2
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• pp.300-310
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• 2015

In this study, we modified silica nanoparticles with N-[3-(trimethoxysilyl)propyl]ethylenediamine (TPED) silane coupling agent, which has one primary and one secondary amino groups in a molecule, to introduce amino groups on the silica surface. After modification of silica, we used 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) to introduce methacrylate groups by Michael addition reaction. We found about 30% of N-H groups on the TPED modified silica surface reacted with acrylate groups of AHM compared to about 85% of reaction between N-H groups of pure TPED with acrylate groups of pure AHM. This lower degree of Michael addition reaction for heterogeneous reaction between N-H groups on the solid TPED modified silica and liquid AHM compared to homogeneous reaction between pure liquid TPED and pure liquid AHM may be caused by lower mobility of grafted amino groups of TPED moiety and higher steric hindrance caused by solid silica particles.