Abstract
Sulfated zirconia mesopore has been successfully prepared from zirconyl oxychloride using structure directing agent cetyl trimethyl ammonium bromide (CTAB) and (NH4)2SO4. The preparation involved calcination at four different temperatures denoted as MZS (400, 500, 600, and 700 °C) and three different zirconyl-to-CTAB ratios (1:1, 3:1, and 9:1). Characterization of resulting zirconia was carried out using XRD method, TEM, gas sorption analyzer, and FTIR. The acidity of zirconia evaluated by ammonia adsorption. Calcination temperatures conducted at 500, 600, and 700 °C lead to crystalline structure and tetragonal phase. MZS-600 prepared at ratio 3:1 showed optimum specific surface area, pore diameter, and pore volume: 147.5 m2/g, 6.6 nm, and 0.396 cc/g, respectively. CTAB assisted larger pore size formation in zirconia along with higher surface area. The catalytic activity of sulfated zirconia mesopore was tested on lauric acid esterification. All sulfated zirconia mesopores prepared were able to give 99–100% conversion. The highest yield of methyl lauric 89.8% was achieved by MZS-600 prepared using CTAB to zirconyl ratio 9:1.
Highlights
Acid catalysts play an important role in many chemical processes to provide feedstock or alternative energy resources
Sulfate group could stabilize surface structure forming of zirconia during calcination made it has high specific surface area by prevent pore from collapse as shown by zyrconil and (NH4)2SO4 (ZS) catalyst
cetyl trimethyl ammonium bromide (CTAB) tends to assist porosity to better develop made it higher in pore diameter which ranges from 6.6 nm for MZS-600 to 12.7 nm for MZS-3:1 and made high pore volume range from 0.382 cc/g for MZS-700 to 0.485 cc/g for MZS-1:1
Summary
Acid catalysts play an important role in many chemical processes to provide feedstock or alternative energy resources. The development of solid acid catalyst based on metal oxides receives attention in as much as other solid materials such as ion-exchange resin, heteropolyacids, zeolite, carbon mesopore and modified clay [1,2,3,4,5,6,7,8]. The activity of sulfated zirconia had been compared with several synthetic zeolites as acid catalyst on n-butane isomerization. The maximum yield of 18% methyl oleic was able to achieve within 4 h using zirconia treated with sulphuric acid 1.0 N. Increase duration of esterification to 12 h rises the yield obtained by 71% This is a relatively low yield of fatty acid methyl ester (FAME) as other obtained methyl oleic
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