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Journal : Indonesian Journal of Chemistry

CONTROLLING FACTOR IN ALUMINA PILLARED SAPONITE AND ALUMINA PILLARED MONTMORILLONITE SYNTHESIS Fatimah, Is; Narsito, Narsito; Wijaya, Karna
Indonesian Journal of Chemistry Vol 9, No 1 (2009)
Publisher : Universitas Gadjah Mada

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Abstract

The effect of synthesis parameters to the physical properties of pillared saponite and pillared montmorillonite was examined. Mol ratio of Al to clay mass in the range 1.0 - 5.0 and two different calcination methods; conventional calcination and microwave irradiation method are evaluated as controlling factors to evolution of basal spacing d001 , surface acidity, specific surface area, pore distribution and catalytic activity in phenol hydroxylation reaction. XRD, FTIR, and N2-adsorption/desorption analysis were used to characterize the materials. Results showed that pillarization produced higher basal spacing d001 and surface acidity and crystalinity of materials in all Al/clay ratio and in both of the calcination methods. In general, Al to clay mass ratio and calcination method remarkably influence to the basal spacing d001, surface acidity and material crystallinity, but the effect of these factors to catalyst activity in phenol hydroxylation depends on nature of clay. It is concluded that the activity as catalyst is affected by the presence of ionic species and surface acidity in the minerals.     Keywords: Pillared smectite, surface acidity, calcination
TITANIUM OXIDE DISPERSED ON NATURAL ZEOLITE (TiO2/ZEOLITE) AND ITS APPLICATION FOR CONGO RED PHOTODEGRADATION Fatimah, Is; Sugiharto, Eko; Wijaya, Karna; Tahir, Iqmal; Kamalia, Kamalia
Indonesian Journal of Chemistry Vol 6, No 1 (2006)
Publisher : Universitas Gadjah Mada

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Abstract

The utilization of TiO2 dispersed on natural zeolite (TiO2/Zeolite) for degradation of Congo Red photocatlytically has been performed. The TiO2/Zeolite was prepared by mechanically mixing of 100 g of natural zeolite, which it has been heated at 400oC, with TiO2 powder, the final weight ratio of the mixture was 5% (w/w). The mixture was then calcined at 400oC for 6 hours. The calcined product was characterized using x-ray diffractometry, x-ray fluorescence analysis and gas sorption analysis methods to determine its physicochemical properties changes caused by mixing and calcination. Investigation of Congo Red photodegradation using TiO2/Zeolite was carried out by mixing 25 mL 10-4 M solution of Congo Red with 25 mg of TiO2/Zeolite and irradiating the suspention with UV-light of 350 nm for 10, 20, 30, 40, 50 and 60 minutes, respectively. The characterization results showed that dispertion of TiO2 on zeolite resulted in the increasing of titanium concentration on TiO2/Zeolite. The concentration of Ti on natural zeolite was found to be 0.15%(w/w), meanwhile on TiO2/Zeolite was 2.29% (w/w). From X-ray diffractometry analysis result no information was found that TiO2 was dipersed on natural zeolite. It was caused by overlapping of the reflections of zeolite with reflections of TiO2. On the otherhand, the gas sorption analysis result exhibited that the dispersion of TiO2 on zeolite resulted in the decreasing of total pore volume as well as specific surface area of the natural zeolite. The specific surface areas of natural zeolite and TiO2/Zeolite were 21.98 and 16.74 m2/g, respectively, meanwhile the total pore volumes of natural zeolite and TiO2/Zeolite were 20.10x10-3 and 13.47x10-3 mL/g. The simple kinetic of photodegradation of Congo Red exhibited that the rate of degradation followed a first order kinetic and the reaction rate constant was 0.0017 minute-1.   Keywords: natural zeolite, TiO2, photodegradation, Congo Red
PHOTODEGRADATION OF ALIZARIN S DYE USING TiO2-ZEOLITE AND UV RADIATION Wijaya, Karna; Sugiharto, Eko; Fatimah, Is; Tahir, Iqmal; Rudatiningsih, Rudatiningsih
Indonesian Journal of Chemistry Vol 6, No 1 (2006)
Publisher : Universitas Gadjah Mada

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Abstract

An investigation of Alizarin S photodegradation using TiO2-zeolite and UV radiation was performed. TiO2-zeolite was prepared by dispersing oligocations of titanium into suspension of zeolite. The suspension was stirred and then filtered to separate the solid phase from the filtrate. the solid phase was calcined by microwave oven at 800 Watt for 5 minutes to convert the oligocations into its oxide forms. The calcined product and unmodified zeolite were characterized using x-ray diffractometry, FT-IR spectrophotometry, X-ray fluorescence and gas sorption analysis methods to determine their physicochemical properties. Photocatalytic activity of TiO2-zeolite was tested on Alizarin S solution using following method: 50 mg of zeolite was dispersed into 25 mL of 10-4 M Alizarin S. The dispersion was irradiated using 365 nm UV light at room temperature on various irradiation times, i.e. 10, 20, 30, 40 and 60 minutes. At certain irradiation time, the dispersion was filtered and the filtrate was then analyzed its concentration using UV-Vis spectrophotometry method. Characterization results exhibited that the formation of TiO2 on internal as well as external surfaces of zeolite could not be detected  with x-ray diffractometry and FT-IR spectrophotometry, however determination of titanium using x-ray fluorescence analysis on the calcined product showed that the concentration of titanium was much higher than zeolite (0.22% on zeolite and 12.08% on TiO2-zeolite). Gas sorption analysis result indicated that the the calcination  resulted in the increase of specific surface area (16,31 m2/g on zeolite and 100.96 m2/g on TiO2-zeolite) as well as total pore volume of calcined product (13.34 mL/Å/g on zeolite and 57.54 mL/Å/g on TiO2-zeolite). The result of photocatalytic activitiy study showed that ca 99 % of Alizarin S was degraded by TiO2-zeolite after UV irradiation for 60 min.   Keywords: TiO2-zeolite, photocatalytic, Alizarin S.
Effect of Calcination Temperature on the Synthesis of ZrO2-Pillared Saponite to Catalytic Activity in Menthol Esterification Fatimah, Is; Rubiyanto, Dwiarso; Kartika, Nanda Candra
Indonesian Journal of Chemistry Vol 16, No 1 (2016)
Publisher : Universitas Gadjah Mada

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Abstract

The influence of calcination temperature on the synthesis of zirconia-pillared saponite (PILS) and on its catalytic activity in menthol esterification has been studied. Zirconia pillarization was conducted using zirconium tetraisopropoxide as a precursor and with calcination temperatures of 450, 600 and 700 °C. Evaluation of physicochemical characteristics at these varied temperatures was carried out by X-Ray Diffraction (XRD), surface area analysis, Scanning Electron Eicroscope (SEM) analysis, Differential Thermal Analysis (DTA) and total acidity. The obtained results indicate that the structure and surface acidity of saponite were strongly influenced by calcination temperature. The solid acidity and surface parameters such as specific surface area, pore volume, and pore radius play an important role in the total conversion and selectivity in menthol esterification.