scholarly journals Effect of Calcination Temperature on the Synthesis of ZrO2-Pillared Saponite to Catalytic Activity in Menthol Esterification

2018 ◽  
Vol 16 (1) ◽  
pp. 8 ◽  
Author(s):  
Is Fatimah ◽  
Dwiarso Rubiyanto ◽  
Nanda Candra Kartika

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.

2015 ◽  
Vol 1101 ◽  
pp. 272-275
Author(s):  
Is Fatimah

In this research zirconium pillared saponite clay (Zr-PILS) was prepared for catalysis application. Pillarization was conducted by zirconium isopropoxide via using sol-gel mechanism and the characterization was performed by X-ray diffraction, gas sorption analysis and surface acidity measurement by pyridine adsorption-FTIR measurement techniques. Result showed that pillaring process to saponite produced pillared saponite with increasing specific surface area, pore volume as well as surface acidity that contributed to enhance catalytic activity in menthol esterification. Reusability test was also showed that Zr-PILS activity is relatively stable.


2021 ◽  
Vol 11 (4) ◽  
pp. 3954-3960

The current paper highlighted the physicochemical characteristics of sardine scales (S.pilchardus), which are considered hitherto as solid marine litter despite their richness on biomaterials of high added value. The collected fish scales were washed thoroughly, dried, and grounded into a powder. The prepared samples were characterized using infrared spectroscopy (FT-IR), x-ray diffraction (XRD), scanning electron microscopy coupled with electron dispersive spectroscopy (SEM/EDS). The findings of (FT-IR); (XRD); and (EDS) show that sardine scales contain both organic and inorganic phases. The (SEM) analysis has revealed that sardine scales have a porous and fibrous structure. The physicochemical results confirm that S.pilchardus scales are a pioneering source of marine biomaterials.


1992 ◽  
Vol 57 (4) ◽  
pp. 750-755 ◽  
Author(s):  
Liao Changsheng

Two kinds of crystalline microporous metal aluminophosphate molecular sieves, magnesium cobalt aluminophosphate (MgCoAPO-5) and manganese cobalt aluminophosphate (MnCoAPO-5), were synthesized by hydrothermal crystallization method in order to improve the surface acidity and catalytic activity of AlPO4-5. The results of X-ray diffraction, infrared spectra and chemical compositions of MgCoAPO-5 and MnCoAPO-5 indicate that Mg-Co or Mn-Co enter the framework of AlPO4-5 molecular sieve without disrupting the microporous framework. However, the results of catalytic studies show that MgCoAPO-5 and MnCoAPO-5 possess much higher surface acidity and catalytic activity than the unmodified AlPO4-5.


2014 ◽  
Vol 25 (4) ◽  
pp. 282-288 ◽  
Author(s):  
Fernanda de Paula do Desterro ◽  
Márcia Soares Sader ◽  
Glória Dulce de Almeida Soares ◽  
Guaracilei Maciel Vidigal Jr

The aim of this study was to evaluate the physicochemical characteristics of 3 mineralized bovine inorganic biomaterials and correlate them with the dissolution rate. Bio-Oss(r), GenoxInorgânico(r), and Bonefill(r) were examined using field emission gun scanning electron microscopy (FEG-SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), specific surface area (BET), calcium/phosphorous molar ratio and a dissolution assay. Bio-Oss(r) showed a micro- and nanoporous structure consisting of 15-nm hydroxyapatite (HA) crystallites; Genox(r), a microporous structure composed of 39-nm HA crystallites; and Bonefill(r), micro- and nanoporous structure of indeterminable crystallite size. FTIR analysis showed that Bio-Oss(r) and Genox(r) were composed of calcium phosphate. The absorption bands of phosphate were poorly defined in Bonefill(r). By XRD, Bio-Oss(r) was shown to contain peaks related to the carbonated HA, whereas Genox(r) only contained peaks corresponding to HA. The broad bands in Bonefill(r) indicated low crystallinity. Bio-Oss(r) showed a greater surface area and calcium release rate than that of Genox(r). Although all biomaterials were of bovine origin, the different manufacturing processes result in materials with different physicochemical properties and may influence the biological and clinical response.


2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Is Fatimah ◽  
Dwiarso Rubiyanto ◽  
Thorikul Huda

Preparation of sulfated zirconia-pillared montmorillonite was carried out in two steps; zirconia pillarization and sulfation to zirconia-pillared montmorillonite. The prepared materials were characterized by using X-ray diffraction (XRD), measurement of the specific surface area, total pore volume and pore size distribution by the N2adsorption method, scanning electron microscopy-energy dispersive X-ray (SEM-EDX), and surface acidity determination by using pyridine adsorption-FTIR analysis. The activity of the materials as catalysts was evaluated for a microwave-assisted conversion of citronellal. The results showed that the prepared materials had a physicochemical character that promoted high catalytic activity to convert citronellal. From varied Zr content and study of the effect of sulfation on the activity, it was found that Zr content and sulfation increase the surface acidity of the material as shown by the higher total conversion and tendency to produce menthol as a product of the tandem cyclization-hydrogenation mechanism.


2017 ◽  
Vol 727 ◽  
pp. 657-662 ◽  
Author(s):  
Fu Wei Xiang ◽  
Xiu Hua Chen ◽  
Hui Wen Ma ◽  
Jie Yu ◽  
Hui Zhang ◽  
...  

This study focuses on the development of the pervoskite catalyst for aluminum-air battery. The catalyst powders of porous pervoskite LaMnO3 were prepared by template method with different calcination temperatures. Material characteristics of prepared samples were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermalgravimetry (TG). The half-cell polarization curves and cyclic voltammetry curves were found to be strongly depended on the calcination temperature. The result showed the optimized calcination temperature was 650°C. The full-cell discharge test in NaCl solution (3.5 wt%) with a constant discharge current of 10 mA/cm2 was performed at room temperature, and the discharge voltage of sample synthesized under optimized calcination temperature was 0.73 V.


2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
Xixin Wang ◽  
Jianling Zhao ◽  
Xiaorui Hou ◽  
Qi He ◽  
Chengchun Tang

ZrO2nanotube arrays were prepared by anodization method in aqueous electrolyte containing (NH4)2SO4and NH4F. The morphology and structure of nanotube arrays were characterized through scanning electron microscope, X-ray diffraction, and infrared spectra analysis. The zirconia nanotube arrays were used as catalyst in esterification reaction. The effects of calcination temperature and electrolyte concentration on catalytic esterification activity have been investigated in detail. Experiments indicate that nanotube arrays have highest catalytic activity when the concentration of (NH4)2SO4is 1 mol/L, the concentration of NH4F is 1 wt%, and the calcination temperature is 400°C. Esterification reaction yield of as much as 97% could be obtained under optimal conditions.


2021 ◽  
Vol 10 (2) ◽  
pp. 140-147
Author(s):  
Poedji Loekitowati Hariani ◽  
◽  
Fahma Riyanti ◽  
Desneli Desneli ◽  
Fatma Fatma ◽  
...  

Bagasse is the solid waste derived from the sugar-making process. A large amount of silica in bagasse is a potential source of silica. In this study, extraction of silica from bagasse was carried out in the following steps: pretreatment of bagasse using HCl solution, followed by calcination at varying temperatures (700 oC, 800 oC, and 900 ℃) using a furnace. Furthermore, extraction using NaOH solution and precipitation using HCl. Silica characteristics were obtained using X-Ray Diffraction (XRD), Scanning Electron Microscopy-Electron Dispersive Spectrometry (SEM-EDS), and BET surface area. The results showed that calcination temperature affected the characteristics of the silica produced. The silica extracted at 700℃ produced an amorphous phase with a broad peak at an angle of 2θ = 20-24°. It contained the most considerable silica content and surface area, 42.46% and 796.89 cm2/g, respectively. The extracted silica had an average diameter of 5.67 mm and a pore volume of 1.184 cm3/g.


2015 ◽  
Vol 12 (11) ◽  
pp. 3977-3988
Author(s):  
Mahmoud. N. Abdel-Salam ◽  
M. A. Abdel-Rahim ◽  
A. Gaber ◽  
A. Y. Abdel-Latief

Nanocrystalline tin dioxide synthesized by the homogeneous pre cipitation method using the reaction of tin tetrachloride pentahydrate and urea solutions has been investigated. The nanocrystalline powder has been traced at different calcination temperatures (300ºC-1050ºC), and then characterized by using   Thermogravemetric analysis, differential thermal analysis and x-ray diffraction. The microstructure of the obtained nanoparticles has been examined by scanning and transmission electron microscopy. The average crystallite size, determined by x-ray diffraction, was found to be in the range of 3 –30 nm. The analysis exhibited a tetragonal phase.  Optical properties were investigated by a UV–vis absorption spectrophotometer. The calculated optical band gap lies between 4.47–3.71 eV as a result of increasing the calcination temperatures and crystallite size. Surface area and porosity of SnO2 nanoparticles are measured. Specific surface area which is related to pore volume and decreases from 155 m2/g at 100ºC to 3.3 m2/g at 1050ºC. 


2014 ◽  
Vol 664 ◽  
pp. 75-79
Author(s):  
Beh Hoe Guan ◽  
Muhammad Hanif Zahari ◽  
Lee Kean Chuan

This study investigates the influence of calcination temperatures on the magnetic properties of Ni0.5Zn0.5Fe2O4(Ni-Zn) ferrites.Ni-Zn ferrite with the chemical formula Ni0.5Zn0.5Fe2O4was prepared from their respective nitrate salts through the sol-gel method. The resulting ferrites were characterized using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM) and vibrating sample magnetometer (VSM). Single phased Ni0.5Zn0.5Fe2O4 was obtained at all calcination temperatures.FESEM Micrographs reveals an increase in the grain size with the increase of the calcination temperature. Consequently, the magnetic saturation of the samples were found to increase with each increase in the calcination temperature where the highest value obtained is 70.58 emu/g for the samples calcined at 1000°C.


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