• Bulletin of the Korean Chemical Society
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• v.27 no.11
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• pp.1844-1850
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• 2006

Two types of catalyst samples were prepared, one sulfated zirconia and the other silica doped sulfated zirconia. The acidity tests indicate that sulfated zirconia doped with silica has higher concentration and strength of acidic catalyst sites than undoped sulfated zirconia. The acidic surface sites have been characterized using FTIR, NMR, pyridine adsorption, TPD, XRD and nitrogen adsorption. Doping with silica increased the concentration of surface Lewis and Brfnsted acid sites and resulted in generation of proximate acid sites.The activity test indicates that doping sulfated zirconia with silica increases both the acidity and catalytic activity for liquid phase dehydration of methanol at 413-453 K. Methanol is sequentially dehydrated to dimethyl ether and ethylene over both catalysts. Significant amounts of propylene are also formed over the silica-doped catalyst, but not over the undoped catalyst.

• Korean Journal of Materials Research
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• v.34 no.7
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• pp.341-354
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• 2024

Today, the principles of green chemistry are being fundamentally applied in the chemical industry, such as the nitrobenzene industry, which is an essential intermediate for various commercial products. Research on the application of response surface methodology (RSM) to optimize nitrobenzene synthesis was conducted using a sulfated silica (SO₄/SiO₂) catalyst and batch microwave reactor. The nitrobenzene synthesis process was carried out according to RSM using a central composite design (CCD) design for three independent variables, consisting of sulfuric acid concentration on the silica (%), stirring time (min), and reaction temperature (℃), and the response variable of nitrobenzene yield (%). The results showed that a three-factorial design using the response surface method could determine the optimum conditions for obtaining nitrobenzene products in a batch microwave reactor. The optimum condition for a nitrobenzene yield of 63.38 % can be obtained at a sulfuric acid concentration on the silica of 91.20 %, stirring time of 140.45 min, and reaction temperature of 58.14 ℃. From the 20 experiments conducted, the SO₄/SiO₂ catalyst showed a selectivity of 100 %, which means that this solid acid catalyst can potentially work well in converting benzene to nitrobenzene.

• Korean Journal of Materials Research
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• v.33 no.7
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• pp.265-272
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• 2023

In this study, the synthesis of nitrobenzene was carried out using sulfated silica catalyst. The study delved into H₂SO₄/SiO₂ as a solid acid catalyst and the effect of its weight variation, as well as the use of a microwave batch reactor in the synthesis of nitrobenzene. SiO₂ was prepared using the sol-gel method from TEOS precursor. The formed gel was then refluxed with methanol and calcined at a temperature of 600 ℃. SiO₂ with a 200-mesh size was impregnated with 98 % H₂SO₄ by mixing for 1 h. The resulting 33 % (w/w) H₂SO₄/SiO₂ catalyst was separated by centrifugation, dried, and calcined at 600 ℃. The catalyst was then used as a solid acid catalyst in the synthesis of nitrobenzene. The weights of catalyst used were 0.5; 1; and 1.5 grams. The synthesis of nitrobenzene was carried out with a 1:3 ratio of benzene to nitric acid in a microwave batch reactor at 60 ℃ for 5 h. The resulting nitrobenzene liquid was analyzed using GC-MS to determine the selectivity of the catalyst. Likewise, the use of a microwave batch reactor was found to be appropriate and successful for the synthesis of nitrobenzene. The thermal energy produced by the microwave batch reactor was efficient enough to be used for the nitration reaction. Reactivity and selectivity tests demonstrated that 1 g of H₂SO₄/SiO₂ could generate an average benzene conversion of 40.33 %.

• Analytical Science and Technology
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• v.34 no.4
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• pp.143-152
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• 2021

Capillary electrophoresis (CE) is an effective technique to study chiral recognition because it offers flexibility in adjusting vital factors. Currently, various available cyclodextrins (CDs) can be employed for the chiral separation of numerous analytes. Herein, we investigate the enantioseparation behavior of lipoic acid enantiomers in various types of single and dual CD systems through CE. Additionally, several impacted CE parameters were optimized through the systematic investigation based on the design of experiment (DoE) concept for a single system comprising a heptakis (2,3,6-tri-O-methyl)-β-CD and a dual system containing the combination of the single CD with a sulfated-β-CD. Consequently, absolute enantioresolution was obtained within 15 min on a common standard bare fused-silica capillary (64.5/56 cm in total/effective length, 50/365 ㎛ inner/outer diameter), maintained at 15 ℃ and at an applied voltage of 24 kV. The optimal background electrolyte consisted of 6 mM heptakis (2,3,6-tri-O-methyl)-β-CD dissolved in the solution of 58 mM borate buffer at pH 10. Furthermore, the results of apparent binding constant experiments indicated that the S-enantiomer-heptakis (2,3,6-tri-O-methyl)-β-CD complex exhibited a stronger affinity than its R-enantiomer counterpart. The obtained electrophoretic mobility values could be utilized to interpret the resolution achieved at various CD concentrations and the mobility behavior of the complexes elucidated the migration order of the enantiomers in an electropherogram.