• Journal of the Korean Ceramic Society
• /
• v.55 no.6
• /
• pp.562-569
• /
• 2018

We propose an economic and facile method for the preparation of silica nanoparticles through a two-step process utilizing chlorosilane residues. Mixed chlorosilane residue was alcoholized with absolute ethanol as a first step to form tetraethoxysilane (TEOS). The TEOS was then utilized as a silicon source to synthesize silica nanoparticles in a sol-gel method. The alcoholysis process was designed and optimized utilizing the Taguchi experimental design method and the yield of TEOS was as high as 82.2% under optimal synthetic conditions. Similarly, the Taguchi method was also utilized to study the effects of synthesis factors on the particle size of silica nanoparticles. The results of statistical analysis indicate that the concentration of ammonia has a greater influence on particle size compared to the mass fractions of TEOS and polyethylene glycol (4.6% and 9.7%). The purity of the silica particles synthesized in our experiments is high, but the specific surface area and pore volume are small.

• Journal of Industrial Technology
• /
• v.5
• /
• pp.73-79
• /
• 1985

Thermodynamic calculation for the CVD of SiC from methyltrichlorosilane(MTS) was done in some range of deposition condition to identify optimum condition. The results show that the most considerable chemical species are chloride and chlorosilane for silicon source and methane and acetylene for carbon source. In order to yield single phase ${\beta}$-SiC it is believed that optimum temperature range is between 1500 and $1700^{\circ}k$. With increasing temperature, stable phase is changed from Si+SiC phase to C+SiC phase. It is believed because equilibrium concentration of silicon source decrease and equilibrium concentration of carbon source increases with increasing temperature.

• Biomolecules & Therapeutics
• /
• v.4 no.3
• /
• pp.251-256
• /
• 1996

The metabolism of carbinoxamine, 2-[(4-chlorophenyl)-2-pyridinyl-methoxy]-N, N-dimethylethaneamine, was studied in adult male volunteers after an oral dose of 15 mg. Solvent extracts of urine obtained with or without enzyme hydrolysis were analyzed by gas chromatography-mass spectrometry after derivatization with MSTFA/TMSCl (N-methyl-N-trimethylsilyltrifluoroacetamide/trimethyl chlorosilane). The structures of metabolites were determined based on the electron impact (EI) and chemical ionization (CI) mass spectra. Nonconjugated metabolites identified in the urine were carbinoxamine, nor-carbinoxamine, and bits-nor-carbinoxamine. Parent drug, nor-carbinoxamine, and bits-nor-carbinoxamine were also detected as conjugated forms. These metabolites observed in human urine were different from those previously reported in the rat. Urinary excretions of carbinoxamine were reached to maxima in 4 hours after drug administration with 4.9%-8.1% and 2.5-4.2% of the dose excreted during 24 h as carbinoxamine and its glucuronide, respectively.

• Bulletin of the Korean Chemical Society
• /
• v.19 no.1
• /
• pp.45-50
• /
• 1998

Most organophosphorus pesticides may be metabolized to yield some common phosphates in human or in animals, and these metabolites may be used as the exposure biomarkers to pesticides. In this study, we developed the extraction method of four phosphate metabolites from the spiked human urine in high recovery by the solid phase extraction with a reverse-phase cartridge (cyclohexyl silica) followed by the elution with methanol. The extracted urinary metabolites were derivatized with hexamethyldisilazane/trimethyl-chlorosilane/pyridine (2 : 1 : 10, v/v/v) and identified by gas chromatography/mass spectrometry. Calibration curve obtained from each metabolite standard using by GC/MS/SIM has shown good linearity and detection limits of metabolites were the range of 0.05-0.1 ㎍/㎖ in urine. Phenthoate, one of the organophosphorus pesticides, was orally administrated to rats. Four metabolites were detected in the rat urine. The results of this study may be applied to development of exposure biomarkers for monitoring of environmental pollutants.

• Bulletin of the Korean Chemical Society
• /
• v.21 no.10
• /
• pp.959-968
• /
• 2000

Direct reaction of elemental silicon with a mixture of (dichloromethyl)silanes 1 $[Cl_3-nMenSiCHCl_2:$ n = 0 (a), n = 1(b), n = 2(c), n = 3(d)] and hydrogen chloride has been studied in the presence of copper catalyst using a stirred bed reactor equ ipped with a spiral band agitator at various temperatures from $240^{\circ}C$ to $340^{\circ}C.$ Tris(si-lyl) methanes with Si-H bonds, 3a-d $[Cl_3-nMenSiCH(SiHCl_2)_2]$, and 4a-d $[Cl_3-nMenSiCH(SiHCl_2)(SiCl_3)]$, were obtained as the major products and tris(silyl)methanes having no Si-H bond, 5a-d $[Cl_3-nMenSiCH(SiCl_3)_2]$, as the minor product along with byproducts of bis(chlorosilyl)methanes, derived from the reaction of silicon with chloromethylsilane formed by the decomposition of 1. In addition to those products, trichlorosilane and tetra-chlorosilane were produced by the reaction of elemental silicon with hydrogen chloride. The decomposition of 1 was suppressed and the production of polymeric carbosilanes reduced by adding hydrogen chloride to 1. Cad-mium was a good promoter for and the optimum temperature for this direct synthesis was $280^{\circ}C$.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.4
• /
• pp.873-881
• /
• 2009

Bis(phenylethynyl)dimethylsilane is branched by the hydrosilation of the phenylethynyl group with dichloromethylsilane, and then the resulting chlorosilane is reacted with lithium phenylacetylide to give the $1^{st}$ generation. The same hydrosilation and alkynylation are repeated to obtain the $7^{th}$ generation. In addition peripheral Si-Cl moiety of the seven kind generation dendrimers are reacted with alcoholic moiety of 9-hydroxymethylanthracene and 2-(2-hydroxyphenyl)benzoxazole group in the presence of TMEDA. Then three kinds of carbosilane dendrimers are prepared from the $1^{st}$ to the $7^{th}$ generations, the $7^{th}$ generation of each dendrimer has 256 phenylethynyl, 256 9-anthracenylmethoxy, or 128 2-(2-phenoxy)benzoxazole groups. Each synthesized dendrimer is unequivocally characterized by $^1H\;and\;^{13}C\;NMR$, elemental analysis, MALDI-MS, GPC, and PL (photoluminescence). Characteristically PDI (Polydisperse Index) values of the dendrimers’ peak in GPC are in the range of $1.00{\sim}1.07$, which indicates that each generation of carbosilane is in unified distribution. PL spectra of phenylethynyl and 9- anthracenemethoxy group substituted dendrimers show no significant change with increasing the generation from the $1^{st}$ to the $7^{th}$. However, the PL spectra of 2-(2-phenoxy)benzoxazole group substituted dendrimers show a blue-shift trend with increasing the generation from the $1^{st}$ to the $7^{th}$.

• Journal of the Korean Applied Science and Technology
• /
• v.34 no.2
• /
• pp.260-270
• /
• 2017

Zirconia has white color and physical, chemical stability, also using in high temperature materials and various industrial structural ceramics such as heat insulating materials and refractories due to their low thermal conductivity, excellent strength, toughness, and corrosion resistance. If hydrophobically modified zirconia is introduced into a hydrophobic acrylate coating solution, the hardness, chemical, electrical, and optical properties will be improved due to the better dispersibility of inorganic particle in organic coating media. Thus, we introduced $-CH_3$ group through silylation reaction using either trimethylchlorosilane(TMCS) or hexamethyldisilazane(HMDZ) on zirconia surface. The $Si-CH_3$ peaks derived from TMCS and HMDZ on hydrophobically modified zirconia surface was confirmed by FT-IR ATR spectroscopy, and introduction of silicon was confirmed by FE-SEM/EDS and ICP-AES. In addition, the sedimentation rate result in acrylate monomer of the modified zirconia showed the improved dispersibility. Comparison of the sizes of a pristine and the modified zirconia particles, which were clearly measured not by the normal microscope but by particle size analysis, provided a pulverizing was occurred by physical force during the silylation process. From the BET analysis data, the specific surface area of zirconia was approximately $18m^2/g$ and did not significantly change during modification process.