• Journal of the Korean Chemical Society
• /
• v.39 no.8
• /
• pp.657-665
• /
• 1995

The oxidation of various benzyl ethers and benzyl alkyl ethers to benzoates has been studied in two-phase system of $CH_3CO_2Et$ and aqueous NaOCl (6.6 mol eq.). The oxidant N-oxo-4-methoxy-2,2,6,6-tetramethylpiperidium bromide (N-oxoammonium salt) was prepared in situ and recycled by addition of 4-methoxy-2,2,6,6-tetramethylpiperidine-1-oxyl (0.03 mol eq., 4-methoxy-TEMPO), co-catalyst KBr (0.03mol eq.) and second oxidant NaOCl. Thus the catalytic amount of 4-methoxy-TEMPO was used. An adjustment of the pH value of below 8.0 was also required for this reaction with 2.5 hr of reaction time at 0∼5$^{\circ}C$. Under these conditions benzyl ethers were oxidized to benzoates. The selectivity of oxidation of benzyl alkyl ethers is dependent on the acidity of hydrogen and steric effect of alkyl group.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2016.02a
• /
• pp.402.1-402.1
• /
• 2016

The performance of solid oxide fuel cells (SOFCs) is directly related to the electrocatalytic activity of composite electrodes in which triple phase boundaries (TPBs) of metallic catalyst, oxygen ion conducting support, and gas should be three-dimensionally maximized. The distribution morphology of catalytic nanoparticle dispersed on external surfaces is of key importance for maximized TPBs. Herein in situ grown nickel nanoparticle onto the surface of fluorite oxide is demonstrated employing gadolium-nickel co-doped ceria ($Gd0.2-xNixCe0.8O2-{\delta}$, GNDC) by reductive annealing. GNDC powders were synthesized via a Pechini-type sol-gel process while maximum doping ratio of Ni into the cerium oxide was defined by X-ray diffraction. Subsequently, NiO-GNDC composite were screen printed on the both sides of yttrium-stabilized zirconia (YSZ) pellet to fabricate the symmetrical half cells. Electrochemical impedance spectroscopy (EIS) showed that the polarization resistance was decreased when it was compared to conventional Ni-GDC anode and this effect became greater at lower temperature. Ex situ microstructural analysis using scanning electron microscopy after the reductive annealing exhibited the exsolution of Ni nanoparticles on the fluorite phases. The influence of Ni contents in GNDC on polarization characteristics of anodes were examined by EIS under H2/H2O atmosphere. Finally, the addition of optimized GNDC into the anode functional layer (AFL) dramatically enhanced cell performance of anode-supported coin cells.

• Transactions of the Korean Society of Mechanical Engineers A
• /
• v.39 no.12
• /
• pp.1297-1303
• /
• 2015

The internal chromium plating of a long-axis tube is widely used in military and industrial application, with the thick hard plating formed using a mixed solution of Chromium acid and catalytic $H_2SO_4$. A large-caliber gun can endure a high explosive force as a result of the increased stiffness and wear resistance provided by this internal hard chromium surface. The internal chromium layer of a tube is prone to exfoliation caused by the high kinetic energy of the projectile and high pressure of the explosion. Therefore, we reviewed the plating process. Chromium plating comprises many steps, including the removal of Grease, water cleaning, electrolytic abrasion, etching, plating, water cleaning, and hydrogen brittleness removal. The exfoliated chromium plating layer is affected by the adhesion property of the plating. In particular, the Fe concentration of the electrolyte affects the adhesion property. The optimum Fe concentration for effectively suppressing the exfoliation of the plating layer was established by using a scanning electron microscope to determine the surface roughness, and the effectiveness was proved in an adhesion test, etc.

• Applied Chemistry for Engineering
• /
• v.7 no.2
• /
• pp.269-279
• /
• 1996

The porous armophous catalysts, composed of $SiO_2-TiO_2-V_2O_5$ were prepared through SOL-GEL process by differing the preparation parameters. Selected the optimum SOL-GEL catalyst which has the best NO removal activity through the screening test, and repeated coating it on the cordierite monolith which is the freely through and inert. And examined the NOx, SOx simultaneous removal effect under S. C. R. condition. In addition to its characterization performances by the DTA, TGA, BET, $NH_3$ and NO TPD, ESCA, XRD etc.

• Transactions of the Korean hydrogen and new energy society
• /
• v.25 no.3
• /
• pp.247-254
• /
• 2014

The synthesis of Fischer-Tropsch oil is the catalytic hydrogenation of CO to give a range of products, which can be used for the production of high-quality diesel fuel, gasoline and linear chemicals. Our cobalt based catalyst was prepared Co/alumina, silica and titania by the incipient wet impregnation of the nitrates of cobalt and promoter with supports. Cobalt catalysts was calcined at $350^{\circ}C$ before being loaded into the FT reactors. After the reduction of catalyst has been carried out under $450^{\circ}C$ for 24hrs, FT reaction of the catalyst has been carried out at GHSV of 4,000/hr under $200^{\circ}C$ and 20atm. From these test results, we have obtained the results as following ; in case of 12wt% Co-supported $Al_2O_3$, $SiO_2$ and $TiO_2$ catalysts, maximum activities of the catalysts were appeared at the promoters of Mn, Mo and Ce respectively. The activity of 12wt% $Co/Al_2O_3$ added a Mn promoter was about 3 times as high as that of 12wt% $Co/Al_2O_3$ catalyst without promoters. When it has been the experiment at the range of reaction temperature of $200{\sim}220^{\circ}C$ and GHSV of 1,546~5,000/hr, the results have shown generally increasing the activities with the increase of reaction temperature and GHSV.

• Transactions of the Korean hydrogen and new energy society
• /
• v.28 no.4
• /
• pp.345-351
• /
• 2017

Single stage water-gas shift reaction has been carried out at a gas hourly space velocity of $150,494h^{-1}$ over $Cu-Ce_{0.8}Zr_{0.2}O_2$ catalysts prepared by a co-precipitation method. Cu loading was optimized to obtain highly active co-precipitated $Cu-Ce_{0.8}Zr_{0.2}O_2$ catalysts for single stage water-gas shift reaction. 80 wt.% $Cu-Ce_{0.8}Zr_{0.2}O_2$ exhibited the excellent catalytic performance as well as 100% $CO_2$ selectivity (CO conversion = 27% at $240^{\circ}C$ for 50 h). The high activity and stability of 80 wt.% $Cu-Ce_{0.8}Zr_{0.2}O_2$ are correlated to low activation energy and large amount of surface Cu atoms.

• Applied Chemistry for Engineering
• /
• v.26 no.1
• /
• pp.86-91
• /
• 2015

The MPPO (3-methyl-1-phenyl-2-phospholene-1-oxide) was prepared by using various polymerization inhibitors such as BHT (2,6-di-tert-butyl-4-methylphenol), TBC (4-tert-butylcatechol), and copper stearate. The MPPO was confirmed by the analysis using FTIR, $^1H$-NMR, and GC/MS regardless of the type of inhibitors. The yield of MPPO increased with the increase of reaction time, whereas the purity of MPPO decreased slightly. The yield and purity of MPPO increased with temperature, but the MPPO prepared by using copper stearate as a polymerization inhibitor exhibited no changes in the purity. The amount of inhibitors had no effect on the yield of MPPO. The purity of MPPOs increased with the amount of inhibitors, but the MPPO prepared by using BHT showed no changes of the purity. We found that the MPPO prepared by using copper stearate exhibited the highest catalytic activity for diphenylcarbodiimide synthesis.

• Applied Chemistry for Engineering
• /
• v.20 no.4
• /
• pp.437-442
• /
• 2009

In this work, thermal shock and simultaneous removal reaction for NOx, soot over Pt catalysts using $TiO_2$, $Al_2O_3$ as support were studied. The catalytic reaction test for NOx and soot were also performed independently and simultaneously, as a result, it showed different NOx removal efficiency and soot oxidation rate according to support and phase, and the onset temperature of soot oxidation has correlation to NOx removal efficiency for the catalyst. The onset temperature of soot oxidation shifted to lower temperature by generated $NO_2$ at the simultaneous reaction for NOx and soot. Also Pt/$TiO_2$ catalyst is more affected than Pt/$Al_2O_3$ on NOx removal efficiency caused by thermal shock while Pt sintering effect induced to reduce the performance on soot oxidation rate for all catalysts.

• Korean Journal of Materials Research
• /
• v.21 no.3
• /
• pp.180-185
• /
• 2011

This study is aimed to increase the activity of cathodic catalysts for PEMFCs(Polymer Electrolyte Membrane Fuel Cells). we investigated the temperature effect of 20wt% Pt/C catalysts at five different temperatures. The catalysts were synthesized by using chemical reduction method. Before adding the formaldehyde as reducing agent, process was undergone for 2 hours at the room temperature (RT), $40^{\circ}C$, $60^{\circ}C$, $80^{\circ}C$ and $100^{\circ}C$, respectively. The performances of synthesize catalysts are compared. The electrochemical oxygen reduction reaction (ORR) was studied on 20wt% Pt/C catalysts by using a glassy carbon electrode through cyclic voltammetric curves (CV) in a 1M H2SO4 solution. The ORR specific activities of 20wt% Pt/C catalysts increased to give a relative ORR catalytic activity ordering of $80^{\circ}C$ > $100^{\circ}C$ > $60^{\circ}C$ > $40^{\circ}C$ > RT. Electrochemical active surface area (EAS) was calculated with cyclic voltammetry analysis. Prepared Pt/C (at $80^{\circ}C$, $100^{\circ}C$) catalysts has higher ESA than other catalysts. Physical characterization was made by using X-ray diffraction (XRD) and transmission electron microscope (TEM). The TEM images of the carbon supported platinum electrocatalysts ($80^{\circ}C$, $100^{\circ}C$) showed homogenous particle distribution with particle size of about 2~3.5 nm. We found that a higher reaction temperature resulted in more uniform particle distribution than lower reaction temperature and then the XRD results showed that the crystalline structure of the synthesized catalysts are seen FCC structure.

• Proceedings of the Materials Research Society of Korea Conference
• /
• 2011.10a
• /
• pp.17.2-17.2
• /
• 2011

Double-walled carbon nanotubes (DWCNTs) were grown with vertical alignment on a Si wafer by using catalytic thermal chemical vapor deposition. This study investigated the effect of pre-annealing time of catalyst on the types of CNTs grown on the substrate. The catalyst layer is usually evolved into discretely distributed nanoparticles during the annealing and initial growth of CNTs. The 0.5-nm-thick Fe served as a catalyst, underneath which Al was coated as a catalyst support as well as a diffusion barrier on the Si substrate. Both the catalyst and support layers were coated by using thermal evaporation. CNTs were synthesized for 10 min by flowing 60 sccm of Ar and 60 sccm of H2 as a carrier gas and 20 sccm of C2H2 as a feedstock at 95 torr and $750^{\circ}C$. In this study, the catalyst and support layers were subject to annealing for 0~420 sec. As-grown CNTs were characterized by using field emission scanning electron microscopy, high resolution transmission electron microscopy, Raman spectroscopy, and atomic force microscopy. The annealing for 90~300 sec caused the growth of DWCNTs as high as ~670 ${\mu}m$ for 10 min while below 90 sec and over 420 sec 300~830 ${\mu}m$-thick triple and multiwalled CNTs occurred, respectively. Several radial breathing mode (RBM) peaks in the Raman spectra were observed at the Raman shifts of 112~191 cm-1, implying the presence of DWCNTs, TWCNTs, MWCNTs with the tube diameters 3.4, 4.0, 6.5 nm, respectively. The maximum ratio of DWCNTs was observed to be ~85% at the annealing time of 180 sec. The Raman spectra of the as-grown DWCNTs showed low G/D peak intensity ratios, indicating their low defect concentrations. As increasing the annealing time, the catalyst layer seemed to be granulated, and then grown to particles with larger sizes but fewer numbers by Ostwald ripening.