Microwave-activated p-TSA dealuminated montmorillonite – a new material with improved catalytic activity

Clay Minerals ◽  
2012 ◽  
Vol 47 (2) ◽  
pp. 231-242 ◽  
Author(s):  
S. Ramesh ◽  
Y. S. Bhat ◽  
B. S. Jai Prakash

AbstractWe report a montmorillonite material with enhanced surface area but with very little alteration in cation exchange capacity (CEC) upon dealumination with para toluene sulphonic acid (p-TSA). The new material shows higher catalytic activity in comparison with mineral-acid-treated clay. Montmorillonite clay was treated with p-TSA for 10 minutes under microwave irradiation. The resulting clay was characterized by CEC, X-ray diffraction (XRD), BET analysis, Fourier transform infrared spectroscopy (FT-IR), temperature programmed desorption (TPD) of ammonia and cyclic voltametry (CV) techniques. XRD patterns show an unchanged structure of pristine matrix after the acid action. BET analysis revealed an increase in the surface area and pore volume on p-TSA treatment, indicating formation of voids in the octahedral layer which suggests dealumination. Nitrogen adsorption-desorption curves showed the creation of new micro porous regions, possibly in the octahedral sheets. In contrast to mineral acid treatment, p-TSA treated clay samples showed similar CEC which shows the absence of dissolution of isomorphously substituted Mg and Fe ions present in the octahedral layer. CV studies confirm the formation of an Al-p-TSA complex, suggesting dissolution of aluminium octahedral sheets. The complex subsequently hydrolyses, replacing interlayer cations with Al3+ ions. Similar treatment with mineral acid resulted in clay with enhanced surface area but with reduced CEC, evidently due to the removal of isomorphously substituted Fe and Mg. Further, the p-TSA treated clays showed relatively higher esterification activity under solvent-free microwave irradiation. The p-TSA treated clay retained its activity even after three subsequent runs and thus can be exploited for practical applications.

Author(s):  
G. Thirumoorthi ◽  
B. Gnanavel ◽  
M. Kalaivani ◽  
Abirami Ragunathan ◽  
Hariharan Venkatesan

Pure and “Fe ([Formula: see text][Formula: see text]wt.%)-doped” WO[Formula: see text] nanoparticles were prepared by facile microwave irradiation method and that was investigated for strong photo catalytic and antibacterial activity applications for the first time. The primary aim of this work is to reveal the great importance of oxygen vacancies ([Formula: see text] due to dopant (Fe[Formula: see text] for photo catalytic and antibacterial activity applications. This work also discusses the contribution of oxygen vacancies and their dependence on surface area and phase formation which are of great research interest for water purification and biological sciences. Herein, pure and “Fe ([Formula: see text][Formula: see text]wt.%)-doped” WO[Formula: see text] nanoparticles were successfully synthesized by facile microwave irradiation (MWI) method (2.45 GHz/240W/10min) in ambient atmosphere. The phase formation and the crystalline nature of the prepared products were evaluated using powder X-ray diffraction (XRD). It confirmed the phase formation of orthorhombic and monoclinic phase formations for the pure (WO[Formula: see text]H2O) and annealed samples (W[Formula: see text]O[Formula: see text] and WO[Formula: see text], respectively. Optical behavior of the samples from UV-Vis diffuse reflectance analysis revealed that W[Formula: see text]O[Formula: see text] has remarkable bandgap values (1.96[Formula: see text]eV) that clearly emphasizes the transfer of oxygen ions which helps in the movement of oxygen vacancies inside the crystalline domain. The morphological nature of the prepared products was observed by FE-SEM analysis and the average dimension was found to be 0.2–3.2[Formula: see text][Formula: see text]m and 2–4[Formula: see text][Formula: see text]m for the pure and annealed products, respectively. The specific surface area from BET analysis explored that W[Formula: see text]O[Formula: see text] having 55.16[Formula: see text]m2g[Formula: see text] was found to be higher than that of commercially available WO3. The photocatalytic behavior of the prepared compounds morphologies was investigated via Rhodamine B (RhB) degradation under visible light irradiation. These results showed “Fe-doped” annealed WO3 nanoparticles have degradation efficiency of 86.9% along with high stable nature. On the other hand, to identify the suitability of the prepared products for antibacterial activity, the microbial strains of Gram-positive Bacillus sp. and Gram-negative strains of Pseudomonas sp. and Salmonella sp. were used for the antimicrobial assay[Formula: see text] The results indicated that W[Formula: see text]O[Formula: see text] showed enhanced antibacterial nature when compared to that of Stoichiometry tungsten oxide (WO[Formula: see text] nanomaterials. From these observations, this work emphasizes the importance of oxygen vacancies for antibacterial activity applications.


2020 ◽  
Vol 21 (1) ◽  
pp. 37
Author(s):  
Febi Yusniyanti ◽  
Wega Trisunaryanti ◽  
Triyono Triyono

Acid-alkaline treatment using acetic acid and sodium hydroxide (NaOH) were applied on mordenite (MOR) to increase the Si/Al ratio and surface area properties. Various time treatment (3, 6, and 9 h) and concentration of acetic acid (6, 9, and 12 M) were used to treat MOR, and followed by the treatment with NaOH (0.1 M) under room temperature. The MOR and treated mordenite were applied as a catalyst for hydrotreatment of cellulose-derived bio-oil. The acetic acid treatment caused the increase of the Si/Al ratio of mordenite up to 27.03. The Si/Al ratio was determined using ICP-AES analysis which was also confirmed using FT-IR analysis. The acidity was determined using NH3 vapors adsorption. The acidity test revealed that as the Si/Al ratio increased the acidity of mordenite decreased. The advantage of using acetic acid for acid treatment was that the XRD patterns of mordenite can be preserved with a little decrease of the intensity. On the other hand, the NaOH treatment under room temperature decreased the crystallinity down to 68%, which was calculated using XRD. The acid-alkaline treatment of mordenite succeeded to increase the surface area 2 times larger than the parent mordenite. The surface area was obtained from BET analysis. The acid-alkaline treated mordenite exhibited better catalytic activity upon hydrotreatment of biomass-derived bio-oil compared to the parent mordenite which corresponded to its highest surface area.


Catalysts ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 1461
Author(s):  
Kieran Aggett ◽  
Thomas E. Davies ◽  
David J. Morgan ◽  
Dan Hewes ◽  
Stuart H. Taylor

CeO2 catalysts were prepared by a precipitation method using either (NH4)2Ce(NO3)6 or Ce(NO3)3, as CeIV or CeIII precursors respectively. The influence of the different precursors on catalytic activity was evaluated for the total oxidation of propane with water present in the feed. The catalyst prepared using the CeIV precursor was more active for propane total oxidation. The choice of precursor influenced catalyst properties such as surface area, reducibility, morphology, and active oxygen species. The predominant factor associated with the catalytic activity was related to the formation of either CeO2.nH2O or Ce2(OH)2(CO3)2.H2O precipitate species, formed prior to calcination. The formation of CeO2.nH2O resulted in enhanced surface area which was an important factor for controlling catalyst activity.


1992 ◽  
Vol 57 (11) ◽  
pp. 2241-2247 ◽  
Author(s):  
Tomáš Hochmann ◽  
Karel Setínek

Solid acid catalysts with acid strength of -14.52 < H0 < -8.2 were prepared by sulfate treatment of the samples of boehmite calcined at 105-800 °C. Two preparation methods were used: impregnation of the calcined boehmite with 3.5 M H2SO4 or mixing of the boehmite samples with anhydrous aluminum sulfate, in both cases followed by calcination in nitrogen at 650 °C. The catalysts were characterized by measurements of surface area, adsorption of pyridine and benzene, acid strength measurements by the indicator method and by catalytic activity tests in the isomerization of cyclohexene, p-xylene and n-hexane. Properties of the catalysts prepared by both methods were comparable.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Yoottapong Klinthongchai ◽  
Seeroong Prichanont ◽  
Piyasan Praserthdam ◽  
Bunjerd Jongsomjit

AbstractMesocellular foam carbon (MCF-C) is one the captivating materials for using in gas phase dehydrogenation of ethanol. Extraordinary, enlarge pore size, high surface area, high acidity, and spherical shape with interconnected pore for high diffusion. In contrary, the occurrence of the coke is a majority causes for inhibiting the active sites on catalyst surface. Thus, this study aims to investigate the occurrence of the coke to optimize the higher catalytic activity, and also to avoid the coke formation. The MCF-C was synthesized and investigated using various techniques. MCF-C was spent in gas-phase dehydrogenation of ethanol under mild conditions. The deactivation of catalyst was investigated toward different conditions. Effects of reaction condition including different reaction temperatures of 300, 350, and 400 °C on the deactivation behaviors were determined. The results indicated that the operating temperature at 400 °C significantly retained the lowest change of ethanol conversion, which favored in the higher temperature. After running reaction, the physical properties as pore size, surface area, and pore volume of spent catalysts were decreased owing to the coke formation, which possibly blocked the pore that directly affected to the difficult diffusion of reactant and caused to be lower in catalytic activity. Furthermore, a slight decrease in either acidity or basicity was observed owing to consumption of reactant at surface of catalyst or chemical change on surface caused by coke formation. Therefore, it can remarkably choose the suitable operating temperature to avoid deactivation of catalyst, and then optimize the ethanol conversion or yield of acetaldehyde.


Catalysts ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 88
Author(s):  
Diana García-Pérez ◽  
Maria Consuelo Alvarez-Galvan ◽  
Jose M. Campos-Martin ◽  
Jose L. G. Fierro

Catalysts based on zirconia- and alumina-supported tungsten oxides (15 wt % W) with a small loading of platinum (0.3 wt % Pt) were selected to study the influence of the reduction temperature and the nature of the support on the hydroisomerization of n-dodecane. The reduction temperature has a major influence on metal dispersion, which impacts the catalytic activity. In addition, alumina and zirconia supports show different catalytic properties (mainly acid site strength and surface area), which play an important role in the conversion. The NH3-TPD profiles indicate that the acidity in alumina-based catalysts is clearly higher than that in their zirconia counterparts; this acidity can be attributed to a stronger interaction of the WOx species with alumina. The PtW/Al catalyst was found to exhibit the best catalytic performance for the hydroisomerization of n-dodecane based on its higher acidity, which was ascribed to its larger surface area relative to that of its zirconia counterparts. The selectivity for different hydrocarbons (C7–10, C11 and i-C12) was very similar for all the catalysts studied, with branched C12 hydrocarbons being the main products obtained (~80%). The temperature of 350 °C was clearly the best reduction temperature for all the catalysts studied in a trickled-bed-mode reactor.


Energies ◽  
2021 ◽  
Vol 14 (7) ◽  
pp. 1875
Author(s):  
Prashanth Reddy Buchireddy ◽  
Devin Peck ◽  
Mark Zappi ◽  
Ray Mark Bricka

Amongst the issues associated with the commercialization of biomass gasification, the presence of tars has been one of the most difficult aspects to address. Tars are an impurity generated from the gasifier and upon their condensation cause problems in downstream equipment including plugging, blockages, corrosion, and major catalyst deactivation. These problems lead to losses of efficiency as well as potential maintenance issues resulting from damaged processing units. Therefore, the removal of tars is necessary in order for the effective operation of a biomass gasification facility for the production of high-value fuel gas. The catalytic activity of montmorillonite and montmorillonite-supported nickel as tar removal catalysts will be investigated in this study. Ni-montmorillonite catalyst was prepared, characterized, and tested in a laboratory-scale reactor for its efficiency in reforming tars using naphthalene as a tar model compound. Efficacy of montmorillonite-supported nickel catalyst was tested as a function of nickel content, reaction temperature, steam-to-carbon ratio, and naphthalene loading. The results demonstrate that montmorillonite is catalytically active in removing naphthalene. Ni-montmorillonite had high activity towards naphthalene removal via steam reforming, with removal efficiencies greater than 99%. The activation energy was calculated for Ni-montmorillonite assuming first-order kinetics and was found to be 84.5 kJ/mole in accordance with the literature. Long-term activity tests were also conducted and showed that the catalyst was active with naphthalene removal efficiencies greater than 95% maintained over a 97-h test period. A little loss of activity was observed with a removal decrease from 97% to 95%. To investigate the decrease in catalytic activity, characterization of fresh and used catalyst samples was performed using thermogravimetric analysis, transmission electron microscopy, X-ray diffraction, and surface area analysis. The loss in activity was attributed to a decrease in catalyst surface area caused by nickel sintering and coke formation.


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