“…The literature also reports that the leaching of heteropolyacids from the support is dependent on the catalyst preparation conditions [9,21]. In order to eliminate the excess HPMo of 25% HPMo (w/w) in the supports (BCM and BLM), which could be responsible for the homogeneous reaction phase, 5 g of sample was used, which was inserted in a Soxhlet extractor with ethanol (500 mL each) under constant stirring for 24 h according to procedure, adapted from [9,51]. At the end of this period the solid was recovered by filtration, washed extensively with water and at room temperature.…”
Section: Methodsmentioning
confidence: 99%
“…The removal of those Keggin units was necessary to avoid their leaching in the liquid medium during the reaction. In this manner, the measurement of the HPMo in the Soxhlet washing solvent made it also possible to indirectly estimate the amount of HPMo efficiently immobilized [20,21,51]. By spectroscopic analysis of ultraviolet-visible spectroscopy (UV-vis) the quantities of HPMo were estimated in the recovered ethanol after extraction and thus, by difference, the quantities of HPMo that were effectively incorporated in the matrices BC and BL [20,21,51].…”
Section: Methodsmentioning
confidence: 99%
“…The calibration curves were constructed at the wavelength 310 nm (λ max ) [54], analyzing the solution of HPMo in ethanol at known concentrations (Figure 1a). Based on literature [20,21,51], the masses of HPMo immobilized in the supports were determined.…”
Two bentonites from Paraíba (Northeastern Brazil) were impregnated with heteropoly phosphomolybdic H3PMo12O40 (HPMo). The materials produced were characterized by various techniques such as N2 adsorption-desorption (specific surface area, SSA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Thermogravimetric analysis (TGA/DTG), Scanning Electron Microscopy (SEM) equipped with Dispersive Energy X-ray spectroscopy (EDS), ultraviolet-visible spectroscopy (UV-vis), acid-base titration analysis. The catalytic activity of these materials was tested in the esterification of a waste from palm oil deodorization and the main results obtained (about 93.3% of conversion) indicated that these materials have potential to act as heterogeneous solid acid catalysts. The prepared materials exhibited satisfactory catalytic performance even after a very simple recycling process in three reuse cycles, without significant loss of their activities.
“…The literature also reports that the leaching of heteropolyacids from the support is dependent on the catalyst preparation conditions [9,21]. In order to eliminate the excess HPMo of 25% HPMo (w/w) in the supports (BCM and BLM), which could be responsible for the homogeneous reaction phase, 5 g of sample was used, which was inserted in a Soxhlet extractor with ethanol (500 mL each) under constant stirring for 24 h according to procedure, adapted from [9,51]. At the end of this period the solid was recovered by filtration, washed extensively with water and at room temperature.…”
Section: Methodsmentioning
confidence: 99%
“…The removal of those Keggin units was necessary to avoid their leaching in the liquid medium during the reaction. In this manner, the measurement of the HPMo in the Soxhlet washing solvent made it also possible to indirectly estimate the amount of HPMo efficiently immobilized [20,21,51]. By spectroscopic analysis of ultraviolet-visible spectroscopy (UV-vis) the quantities of HPMo were estimated in the recovered ethanol after extraction and thus, by difference, the quantities of HPMo that were effectively incorporated in the matrices BC and BL [20,21,51].…”
Section: Methodsmentioning
confidence: 99%
“…The calibration curves were constructed at the wavelength 310 nm (λ max ) [54], analyzing the solution of HPMo in ethanol at known concentrations (Figure 1a). Based on literature [20,21,51], the masses of HPMo immobilized in the supports were determined.…”
Two bentonites from Paraíba (Northeastern Brazil) were impregnated with heteropoly phosphomolybdic H3PMo12O40 (HPMo). The materials produced were characterized by various techniques such as N2 adsorption-desorption (specific surface area, SSA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Thermogravimetric analysis (TGA/DTG), Scanning Electron Microscopy (SEM) equipped with Dispersive Energy X-ray spectroscopy (EDS), ultraviolet-visible spectroscopy (UV-vis), acid-base titration analysis. The catalytic activity of these materials was tested in the esterification of a waste from palm oil deodorization and the main results obtained (about 93.3% of conversion) indicated that these materials have potential to act as heterogeneous solid acid catalysts. The prepared materials exhibited satisfactory catalytic performance even after a very simple recycling process in three reuse cycles, without significant loss of their activities.
“…Acidity measurements of the catalyst surface were done by pyridine adsorption and temperature programmed desorption as follows . The catalysts were pressed to obtain a wafer.…”
Section: Methodsmentioning
confidence: 99%
“…Acidity measurements of the catalyst surface were done by pyridine adsorption and temperature programmed desorption as follows. [65] The catalysts were pressed to obtain a wafer. The wafer was weighted and then placed in a sample holder inside a Pyrexcell especially designed for the controlled heating of the sample under vacuum and equipped with an optical NaCl window.…”
Mesoporous aluminosilicate nanofibers (mASNF) were prepared using hard and soft dual templates approach. The mesoporous material was fully characterized and its acidic nature was confirmed by FTIR spectroscopy of pyridine adsorption and 27Al/29Si solid state NMR. Thanks to the incorporated aluminum atoms, the acidic material showed high hydrothermal stability which is an essential property for biomass conversion applications. The catalytic performance of Pd supported on mASNF for hydrodeoxygenation (HDO) of lignin model compound was also investigated. A complete conversion and a high selectivity towards cyclohexane (up to 95 %) starting from phenol were achieved with this bifunctional catalyst. In comparison, no cyclohexane has been produced with a non‐acidic material which underlines the importance of acidic sites in HDO process selectivity control. Moreover, the catalyst can be recycled without losing its initial structure.
The energetically viable fabrication of stable and highly efficient solid acid catalysts is one of the key steps in large‐scale transformation processes of biomass resources. Herein, the covalent modification of the classical Dawson polyoxometalate (POMs) with sulfonic acids (‐SO3H) is reported by grafting sulfonic acid groups on the POM's surface followed by oxidation of (3‐mercaptopropyl)trimethoxysilane. The acidity of TBA6‐P2W17‐SO3H (TBA=tetrabutyl ammonium) has been demonstrated by using 31P NMR spectroscopy, clearly indicating the presence of strong Brønsted acid sites. The presence of TBA counterions renders the solid acid catalyst as a promising candidate for phase transfer catalytic processes. The TBA6‐P2W17‐SO3H shows remarkable activity and selectivity, excellent stability, and great substrate compatibility for the esterification of free fatty acids (FFA) with methanol and conversion into biodiesel at 70 °C with >98 % conversion of oleic acid in 20 min. The excellent catalytic performance can be attributed to the formation of a catalytically active emulsion, which results in a uniform catalytic behavior during the reaction, leading to efficient interaction between the substrate and the active sites of the catalyst. Most importantly, the catalyst can be easily recovered and reused without any loss of its catalytic activity owing to its excellent phase transfer properties. This work offers an efficient and cost‐effective strategy for large‐scale biomass conversion applications.
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