Sonically modified hierarchical FAU-type zeolites as active catalysts for the production of furan from furfural

In this study, the sonochemical-assisted desilication method was applied as a special and innovative way of preparing hierarchical zeolites. The physicochemical properties of the hierarchical zeolites prepared using the sonochemical route were compared with those prepared using the conventional desilication method. Commercial zeolite with FAU-type structure was desilicated with a sodium and tetrabutylammonium hydroxide aqueous solution (NaOH/TBAOH) for 30 min. The ultrasound treatment process was performed using a QSonica Q700 sonicator (Church Hill Rd, Newtown, CT, USA) equipped with a ½″ diameter horn. The average power of sonication was 60 W, and the frequency was 20 kHz. During the sonication procedure, the alkaline solution with the catalyst precursor and sonicator probe were placed in an ice bath to keep them at room temperature. The prepared catalyst samples were examined by ICP-OES, XRD, SEM, NMR, and nitrogen sorption techniques. The acidic properties of the prepared hierarchical zeolite samples were assessed by means of IR spectroscopy with ammonia and carbon monoxide sorption as probe molecules. All catalysts were studied in the decarbonylation of furfural into furan.Independently of the application of ultrasonic irradiation, desilication of zeolites with an NaOH/TBAOH mixture extracts comparable amounts of silicon, resulting in comparable crystallinity and acidity. On the other hand, the samples prepared in the presence of ultrasounds revealed higher both mesoporosity and enhanced catalytic properties in the reaction of decarbonylation of furfural into furan in comparison with their counterparts prepared using the conventional method.     

Ultrasound-assisted rapid hydrothermal design of efficient nanostructured MFI-Type aluminosilicate catalyst for methanol to propylene reaction

The influence of ultrasound-assisted rapid hydrothermal synthesis of aluminosilicate ZSM-5 catalysts was examined in this work. A series of MFI-type nanostructured materials with sonochemical approach and conventional heating were synthesized and evaluated for conversion of methanol to propylene reaction. The prepared samples were tested by characterization analyses such as XRD, FESEM, BET-BJH, FTIR, TPD-NH₃ and TG/DTG. The obtained results confirmed that ultrasound treatment enhanced the nucleation process and crystal growth for ZSM-5 sample synthesized at moderate temperature of 250 °C. Therefore, it was found the formation of pure MFI zeolite with high crystallinity and improved textural, structural and acidic properties for ZSM-5(UH-250) sample compared with the other zeolites. This observation was attributed to the relationship between the perfect crystallization mechanism and catalytic properties, which led to producing an efficient MFI zeolite toward the optimal catalytic performance. In this manner, the methanol conversion and products selectivity of prepared materials were carried out in MTP reaction at 460 °C and atmospheric pressure. The ZSM-5(UH-250) zeolite with slower deactivation regime exhibited the constant level of methanol conversion (84%) and high propylene selectivity (78%) after 2100 min time on stream. Moreover, the synthesis pathway for MFI zeolite at moderate temperature and also deactivation mechanism of improved sample were proposed.     

Electro-oxidation of ethanol using PtSnRh/C electrocatalysts prepared by an alcohol-reduction process

PtRh/C (90:10), PtRh/C (50:50), PtSn/C (50:50), and PtSnRh/C (50:40:10) electrocatalysts were prepared by an alcohol-reduction process using ethylene glycol as solvent and reduction agent and Vulcan Carbon XC72 as supports. The electrocatalysts were characterized by energy-dispersive X-ray analysis, X-ray diffraction, and transmission electron microscopy. The electro-oxidation of ethanol was studied by cyclic voltammetry chronoamperometry at room temperature and on a single cell of a direct ethanol fuel cell at 100 °C. Cyclic voltammetry and chronoamperometry experiments showed that PtSnRh/C and PtSn/C electrocatalysts have similar performance for ethanol oxidation at room temperature, while the activity of PtRh/C electrocatalysts was very low. At 100 °C on a single cell, PtSnRh/C showed superior performance compared to PtSn/C and PtRh/C electrocatalysts.     

Synthesis of star macromolecules for solid polymer electrolytes

The star macromolecules (SM) were synthesized from phloroglucinol, phosphorus oxychloride, and poly(ethylene glycol methyl ether) with different molecular weight. Structures of the products were characterized by Fourier transform infrared and ¹H-nuclear magnetic resonance. Solid polymer electrolyte films were prepared by mixing the products with poly(ethylene oxide) (PEO) and LiClO₄. The polymer blends of PEO and SM have been characterized by differential scanning calorimetry and thermogravimetry, and the polymer electrolytes have been characterized by alternating current impedance. All the SM products could improve the conductivities of the polymer electrolyte obviously at a temperature range from 20 °C to 80 °C.     

Optimization of ultrasonic-assisted extraction of astaxanthin from green tiger (Penaeus semisulcatus) shrimp shell

This study was aimed at optimizing the astaxanthin extraction efficiency from shrimp shell (green tiger, Penaeus semisulcatus). Astaxanthin was extracted using selected nonpolar/polar solvents (petroleum ether, n-hexane, ethanol, acetone) individually and in ternary mixtures of petroleum ether, acetone, and water in ratios of 15:50:35, 50:45:5, and 15:75:10 for different times (2,4 and 6 h). The results showed that solvents with higher polarity were more suitable for the extraction of astaxanthin, and increasing the extraction time from 2 to 6 h improved the extraction yield. The conditions of extraction of astaxanthin with the desirable solvent were then optimized with the ultrasonic method using the Box-Behnken design [variables included: extraction temperature (25 to 45 °C), extraction time (5 to 15 min), and ultrasound amplitude (20 to 100%)]. Optimal extraction conditions were determined as the ultrasonic amplitude of 23.6%, extraction time of 13.9 min, and extraction temperature of 26.3 °C. Under this optimum condition, the amount of astaxanthin, ferric reducing antioxidant power, and free radical scavenging capacity of the extract were obtained as 51.5%, 1705 μmol of Fe²⁺/g, and 73.9%, respectively. Extraction and analysis of the extract at the optimum point were used to validate the results.     

Optimization of ultrasonic-assisted extraction of pomegranate (Punica granatum L.) seed oil

The effectiveness of ultrasonic-assisted extraction (UAE) of pomegranate seed oil (PSO) was evaluated using a variety of solvents. Petroleum ether was the most effective for oil extraction, followed by n-hexane, ethyl acetate, diethyl ether, acetone, and isopropanol. Several variables, such as ultrasonic power, extraction temperature, extraction time, and the ratio of solvent volume and seed weight (S/S ratio) were studied for optimization using response surface methodology (RSM). The highest oil yield, 25.11% (w/w), was obtained using petroleum ether under optimal conditions for ultrasonic power, extraction temperature, extraction time, and S/S ratio at 140 W, 40 °C, 36 min, and 10 ml/g, respectively. The PSO yield extracted by UAE was significantly higher than by using Soxhlet extraction (SE; 20.50%) and supercritical fluid extraction (SFE; 15.72%). The fatty acid compositions were significantly different among the PSO extracted by Soxhlet extraction, SFE, and UAE, with punicic acid (>65%) being the most dominant using UAE.     

Preparation and characterization of PtRu/C-rare earth using an alcohol-reduction process for ethanol electro-oxidation

PtRu/C (100% C) and PtRu/C-CeO₂, PtRu/C-La₂O₃, PtRu/C-Nd₂O₃, and PtRu/C-Er₂O₃ (85% C and 15% rare earth) electrocatalysts were prepared in a single step by an alcohol-reduction process using H₂PtCl₆ 6H₂O and RuCl₃ xH₂O as metal sources, ethylene glycol as solvent and reducing agent, Vulcan XC72 and rare earth (RE) as support. The electrocatalysts were characterized by energy dispersive X-ray, X-ray diffraction, and transmission electron microscopy. The performance for ethanol oxidation was investigated by cyclic voltammetry and chronoamperommetry at room temperature, and studies on the direct ethanol fuel cell were carried at 100 °C. The Pt:Ru atomic ratios were similar to the nominal used in preparation, and the average particle sizes were in the range of 2.0–3.0 nm. All PtRu/C-RE electrocatalysts showed an increase of performance for ethanol oxidation at room temperature and also on a single direct ethanol fuel cell tests in relation to PtRu/C electrocatalyst at 100 °C.     

Performance of lithium-ion cells using 1 M LiPF<Subscript>6</Subscript> in EC/DEC (<Emphasis Type="Italic">v</Emphasis>/<Emphasis Type="Italic">v</Emphasis> = 1/2) electrolyte with ethyl propionate additive

In this work, 1 M LiPF₆:EC:DEC (v/v = 1/2) was used as a baseline electrolyte where EC is ethylene carbonate and DEC is diethyl carbonate. Ethyl propionate (EP) was used as an additive. The conductivity of the liquid electrolyte was obtained at ambient and elevated temperatures. The highest room temperature conductivity was observed at (8.05 ± 0.16) mS cm⁻¹ for the electrolyte containing 28.6 vol.% EP. Viscosity of the baseline and EP added baseline electrolytes have been measured at room and elevated temperatures. The electrolyte was also characterized by linear sweep voltammetry. The highest conducting electrolyte with 28.6 vol.% EP and the baseline electrolyte were used to fabricate several batteries. The batteries were charged and discharged at room temperature and at −20°C.     

Gas sensing properties of single crystalline ZnO nanowires grown by thermal evaporation technique

The ZnO NWs were applied as effective material for the fabrication of ethanol (C₂H₅OH) and carbon monoxide (CO) gas sensor. The ZnO NWs were grown by thermal evaporation techniques on non-catalytic Si (100) substrates. The average width and length of ZnO NWs was 60 nm and 20 μm, respectively and they were single crystalline in nature. The maximum response was 51.64 at 300 °C for 1000 ppm of CO gas, while 104.23 at 400 °C for 250 ppm of ethanol gas. The response of ZnO NWs was very high for ethanol compared to the CO, whereas the recovery time for ethanol was very poor compare to CO gas. The response of ZnO NWs was about 25 times higher for ethanol compare to CO, at 400 °C for 100 ppm of each gas. The high response for ethanol is related to electron donating effect of ethanol (10e^?) which was higher than the CO gas (2e^?). The high response of ZnO NWs was attributed to large contacting surface area for electrons, oxygen, target gas molecule, and abundant channels for gas diffusion.     

Investigation of a Pt–Fe/C catalyst for oxygen reduction reaction in direct ethanol fuel cells

Three cathode catalysts (60% Pt/C, 30% Pt/C and 60% Pt–Fe/C), with a particle size of about 2–3 nm, were prepared to investigate the effect of ethanol cross-over on cathode surfaces. All samples were studied in terms of structure and morphology by using X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses. Their electrocatalytic behavior in terms of oxygen reduction reaction (ORR) was investigated and compared using a rotating disk electrode (RDE). The tolerance of cathode catalysts in the presence of ethanol was evaluated. The Pt–Fe/C catalyst showed both higher ORR activity and tolerance to ethanol cross-over than Pt/C catalysts. Moreover, the more promising catalysts were tested in 5 cm² DEFC single cells at 60 and 80 °C. An improvement in single cell performance was observed in the presence of the Pt–Fe catalyst, due to an enhancement in the oxygen reduction kinetics. The maximum power density was 53 mW cm⁻² at 2 bar rel. cathode pressure and 80 °C.     

Biotemplate fabrication of SnO<Subscript>2</Subscript> nanotubular materials by a sonochemical method for gas sensors

A sonochemical method is developed to fabricate SnO₂ nanotubular materials from biological substances (here, it is cotton). The cotton fibers in SnCl₂ solution were first treated with ultrasonic waves in air, followed by calcinations to give nanotubular materials that faithfully retain the initial cotton morphology. The microstructure and morphology of the obtained SnO₂ nanotubules were characterized by the combination of field-emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR), X-ray diffraction (XRD), and N₂ adsorption/desorption measurements. The thermal behavior and crystalline properties were examined in the temperature range of 450–700 °C. The nanocrystals composing of SnO₂ nanotubules were estimated about 8.5, 13.2, and 14.2 nm corresponding to calcination temperatures of 450, 550, and 700 °C, respectively. The sensor performance of biomorphic SnO₂ nanotubules calcined at 700 °C was investigated in the atmosphere of ethanol, formaldehyde, carbinol, carbon monoxide, hydrogen, ammonia, and acetone, respectively, which exhibited a good selectivity for acetone at a working temperature of 350 °C. The sensitivity to 20 ppm acetone, S, was 6.4 at 350 °C with rapid response and recovery (around 10–9 s). These behaviors were well explained in relation to the morphology of the nanotubules thus produced.     

Ultrasound enhances lipase-catalyzed synthesis of poly (ethylene glutarate)

The present work explores the best conditions for the enzymatic synthesis of poly (ethylene glutarate) for the first time. The start-up materials are the liquids; diethyl glutarate and ethylene glycol diacetate, without the need of addition of extra solvent. The reactions are catalyzed by lipase B from Candida antarctica immobilized on glycidyl methacrylate-ter-divinylbenzene-ter-ethylene glycol dimethacrylate at 40 °C during 18 h in water bath with mechanical stirring or 1 h in ultrasonic bath followed by 6 h in vacuum in both the cases for evaporation of ethyl acetate. The application of ultrasound significantly intensified the polyesterification reaction with reduction of the processing time from 24 h to 7 h. The same degree of polymerization was obtained for the same enzyme loading in less time of reaction when using the ultrasound treatment. The degree of polymerization for long-term polyesterification was improved approximately 8-fold due to the presence of sonication during the reaction. The highest degree of polymerization achieved was 31, with a monomer conversion of 96.77%. The ultrasound treatment demonstrated to be an effective green approach to intensify the polyesterification reaction with enhanced initial kinetics and high degree of polymerization.     

Highly sensitive ethanol sensors based on nanocrystalline SnO2 thin films

This paper reports on a simple and inexpensive ultrasonic spray pyrolysis method to synthesize agglomerate-free nanosized SnO₂ particles with a size smaller than 10 nm. Scanning electron microscopy, transmission electron microscopy and high resolution X-ray diffraction studies were used to characterize the morphology, crystallinity, and structure of the SnO₂ particles. Under the optimized experimental conditions, the prepared SnO₂ sensor shows the high response (S = 491) towards 100 ppm ethanol gas at 300 °C, linearity in the range of 100–500 ppm, quick response time (2 s), recovery time (60 s) and selectivity against other gases. The response of the sensor was monitored in a 250–450 °C temperature range. The seven fold enhancement in gas response and selective detection of C₂H₅OH in the presence of other gases such as CH₃OH and CH₃CHOHCH₃ are the significant points in this investigation. These results demonstrate that pure nanocrystalline SnO₂ thin film can be used as the sensing material for fabricating high performance ethanol sensors.     

Mass fabrication of size-controllable hydrogel microarrays by dip-pen nanolithography with viscosity-tunable ink

A method of mass fabricating poly(ethylene glycol) (PEG) hydrogel microarrays is demonstrated. Microarrays of poly(ethylene glycol) dimethacrylate (PEG-DMA) with photoinitiator were patterned by one-dimensional (1-D) parallel dip-pen nanolithography (DPN), and the microarrays were cross-linked to form PEG hydrogels by UV irradiation in N₂ air. As an ink material for DPN printing, solid and liquid phase of PEG-DMA were mixed and prepared to tune viscosity of the ink material by temperature. Thus, the diameter of the microarrays was able to be averagely controlled from 1.7 to 6.2 μm as temperature during printing was increased from 25 °C to 37 °C, respectively. The overall microarrays showed less than 16% coefficient of variation (C.V.). Moreover, small molecules, such as fluorescence dyes, were able to be embedded in the PEG hydrogel microarrays.     

Preparation of CuO nanoparticles by metal salt-base reaction in aqueous solution and their metallic bonding property

This article describes a method for preparing CuO nanoparticles in aqueous solution, and a demonstration of feasibility of metallic bonding with the use of the CuO particles. Colloid solution of CuO nanoparticles was prepared from Cu(NO₃)₂ aqueous solution (0.01 M) and NaOH aqueous solution (0.019 M) at 5–80 °C. Leaf-like aggregates with an average size of 567 nm composed of CuO nanoparticles were produced at 20 °C. The size of leaf-like aggregates decreased with increasing reaction temperature. Metallic copper discs could be bonded using the CuO nanoparticles under annealing at 400 °C and pressurizing at 1.2 MPa for 5 min in H₂ gas. A shear strength required for separating the bonded discs was 25.4 MPa for the CuO nanoparticles prepared at 20 °C, whose aggregates were the largest among the CuO particles examined. These results indicated that the formation of leaf-like aggregates of CuO nanoparticles led to efficient metallic bonding.     

Elucidating iron doping induced n- to p- characteristics of Strontium titanate based ethanol sensors

A series of pure and iron doped strontium titanate, (SrFe_xTi_1-xO₃; x = 0, 0.1 and 0.2) powders were synthesized, characterized and used to fabricate ethanol sensors for low concentration. X-Ray Diffraction (XRD) technique was used to confirm the single phase formation. Microstructural properties of the powders were investigated using scanning electron microscopy (SEM). Electrical conductivity of all the samples at room temperature (RT) was measured. Sensors were optimized for best responsiveness by varying the operating temperature from 350 °C to 500 °C.The sensor with doping x = 0.2 exhibited best sensing response at 400 °C for ethanol gas. The undoped sensor demonstrated a decrease in resistance on exposure to ethanol gas whereas Fe-doped sensors showed increase in resistance. The doping induced changeover from n to p behavior in the sensing response on doping has been investigated and corroborated with an observed shift in the Fermi level position by X-ray photoelectron spectroscopy (XPS). The disparity in gas sensing response clearly demonstrates inter-connection of multiple influencing factors such as electrical conductivity, morphology, porosity and change in chemical composition on doping. The sensors were exposed to ethanol, nitrogen dioxide, carbon monoxide, butane gases at concentration between 5 ppm and 50 ppm. The sensor exhibited much reduced relative response to all gases other than ethanol which can be utilized for wide range of applications.     

Experimental IR study and ab initio modelling of ethylene adsorption in a MFI-type host zeolite

Different ab initio methods and experimental results are used to investigate the effect of the adsorption of one ethylene molecule on silicalite-1, a MFI-type zeolite. We used simplified models to simulate a portion of a straight or sinusoidal channel of silicalite-1 at a quantum level. The calculated absorption spectra of the models are qualitatively in good agreement with the experimental FTIR spectrum of silicalite-1. Additionally we simulate the FTIR spectrum of the isolated ethylene molecule and that of an ethylene molecule in interaction with the above-mentioned zeolite models. Results are discussed depending on the method and specific basis set and compared with experiments and previous molecular dynamics simulations.     

Preparation of PtSnSb/C by an alcohol reduction process for direct ethanol fuel cell (DEFC)

PtSn/C and PtSnSb/C electrocatalysts (20 wt.% metal loading) were prepared by an alcohol reduction process using H₂PtCl₆.6H₂O, SnCl₂.2H₂O, and Sb(OOCCH3) as metal sources, ethylene glycol as solvent and reducing agent, and Vulcan XC72 as carbon support. The electrocatalysts were characterized by energy dispersive X-ray analysis, X-ray diffraction, and transmission electron microscopy, while that the performance for ethanol oxidation was investigated by cyclic voltammetry and chronoamperommetry (chrono) at room temperature. The diffractograms of the PtSn/C and PtSnSb/C electrocatalysts showed four peaks associated to Pt face-centered cubic structure and two peaks that were related to a SnO₂ phase. For PtSb/C and PtSnSb/C electrocatalysts, no Sb (antimony) peaks corresponding to a metallic antimony or antimony oxide phases were observed. Transmission electron microscopy images showed that the metal particles were homogeneously distributed over the support. The PtSnSb/C (50:45:05) electrocatalyst showed an increase of performance for ethanol oxidation in relation to PtSn/C electrocatalyst at room temperature. In the tests at 100 °C on a single cell of a direct ethanol fuel cell, the maximum power density of PtSnSb/C (50:45:05) electrocatalyst was slightly higher than that of PtSn/C electrocatalyst.     

Nanocrystalline cerium oxide coated fiber optic gas sensor

A clad-modified fiber optic sensor with nanocrystalline CeO₂ is proposed for gas detection. As-prepared and annealed CeO₂ (500 °C) samples have been used as gas sensing media. The spectral characteristics of the fiber optic gas sensor are studied for various concentrations of ammonia, ethanol and methanol gases (0–500 ppm). The sensor exhibits linear variation in the spectral peak intensity with the gas concentration. The characteristics of the sensor are also studied for gas selectivity. The time response characteristics of the sensor are reported.     

Ultrasound and heat treatment effects on Staphylococcus aureus cell viability in orange juice

Ultrasounds are being considered an excellent alternative technology in juice preservation. Yet, when combined with heat treatment, the process seems to be further intensified. This work aimed to evaluate and compare the impact of ultrasounds and heat treatments, when applied alone or in combination, on Staphylococcus aureus survival in orange juice. Inoculated commercial pasteurized orange juice was treated at different times at 20, 30, 40, 50 and 60 °C. SEM analyses were applied to identify morphological changes in S. aureus cells appearance. The microbial inactivation data were fitted using two mathematical models, depending on the behaviour observed.Sonication at 20, 30, and 40 °C induced 4.02 ± 0.52, 3.80 ± 0.49 and 4.30 ± 0.74 log cycles reduction of S. aureus after treatments of 90, 60 and 60 min, respectively. The heat treatments at the same temperatures had no impact on S. aureus survival. When 50 and 60 °C were applied, more than 5-log reductions were attained for both thermosonication and heat treatments alone. A synergistic effect was observed between sonication and high temperatures. At 50 °C, the thermosonication reduced the treatment time from 60 to 35 min and the microbial load from 5.14 ± 0.08 to 10.76 ± 0.28 log cycles reduction, compared to heat treatment alone. Results from SEM images showed that cells undergo membrane damage during sonication exposure. This was observed by collapsed cells, cell disruption, and holes in the cell’s membrane.Thermosonication proved to be a viable alternative to thermal pasteurization of orange juice since milder treatments can be safely applied, improving the final product quality.