Search results for: desorption

Authors: Hu-Cheng Weng, Jhen-Ting Huang, Chia-Chia Chang, An-Ya Lo

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In this study, carbon mesoporous material, CMK-3, was adopted as supporting material for electroactive polymerspolyaniline (PANI), polyaniline, for supercapacitor application, where hydroquinone (HQ) was integrated to enhance the redox reaction of PANI. The results show that the addition of PANI improves the capacitance of electrode from 89 F/g (CMK-3) to 337 F/g (PANI/CMK-3), the addition of HQ furtherly improves the capacitance to 463 F/g (PANI/CMK-3/HQ). The PANI provides higher energy density and also acts as binder of the electrode; the CMK-3 provides higher electron double layer capacitance EDLC and stabilize the polyaniline by its highly porosity. With the addition of HQ, the capacitance of PANI/CMK-3 was further enhanced. In-situ analyses including cyclic voltammetry (CV), chronopotentiometry (CP), electron impedance spectrum (EIS) analyses were applied for electrode performance examination. For materials characterization, the crystal structure, morphology, microstructure, and porosity were examined by X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscopy (TEM), and 77K N2 adsorption/desorption analyses, respectively. The effects of electrolyte pH value, PANI polymerization time, HQ concentration, and PANI/CMK-3 ratio on capacitance were discussed. The durability was also studied by long-term operation test. The results show that PANI/CMK-3/HQ with great potential for supercapacitor application. Finally, the potential of all-solid PANI/CMK-3/HQ based supercapacitor was successfully demonstrated.

Keywords: CMK3, PANI, redox electrolyte, solid supercapacitor

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Authors: Yu Zhang, Il Kim

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Polypeptides with defined peptide sequences illustrate the power of remarkable applications in drug delivery, tissue engineering, sensing and catalysis. Especially the cyclic polypeptides, the distinctive topological architecture imparts many characteristic properties comparing to linear polypeptides. Here, a facile and highly efficient strategy for the synthesis of linear and cyclic polypeptides is reported using N-heterocyclic carbenes (NHCs)-mediated ring-opening polymerization (ROP) of α-amino acid N-carboxyanhydrides (NCA) in the presence or absence of primary amine initiator. The polymerization proceeds rapidly in a quasi-living manner, allowing access to linear and cyclic polypeptides of well-defined chain length and narrow polydispersity, as evidenced by nuclear magnetic resonance spectrum (1H NMR and 13C NMR spectra) and size exclusion chromatography (SEC) analysis. The cyclic architecture of the polypeptides was further verified by matrix-assisted laser desorption ionization-time of flight (MALDI-TOF) mass spectra (MALDI-TOF MS) and electrospray ionization (ESI) mass spectra, as well as viscosity studies. This approach can also simplify workup procedures and make bulk scale synthesis possible, which thereby opens avenues for practical uses in diverse areas, opening up the new generation of polypeptide synthesis.

Keywords: α-amino acid N-carboxyanhydrides, living polymerization, polypeptides, N-heterocyclic carbenes, ring-opening polymerization

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Authors: Natapol Pumipuntu

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Staphylococcus argenteus is the emerging species of S. aureus complex. It was generally misidentified as S. aureus by standard techniques and their features. S. argenteus is possibly emerging in both humans and animals, as well as increasing worldwide distribution. The objective of this study was to differentiate and identify S. argenteus from S. aureus, which has been collected and isolated from milk samples of subclinical bovine mastitis cases in Maha Sarakham province, Northeastern of Thailand. Twenty-one isolates of S. aureus, which confirmed by conventional methods and immune-agglutination method were analyzed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) and multilocus sequence typing (MLST). The result from MALDI-TOF MS and MLST showed 6 from 42 isolates were confirmed as S. argenteus, and 36 isolates were S. aureus, respectively. This study indicated that the identification and classification method by using MALDI-TOF MS and MLST could accurately differentiate the emerging species, S. argenteus, from S. aureus complex which usually misdiagnosed. In addition, the identification of S. argenteus seems to be very limited despite the fact that it may be the important causative pathogen in bovine mastitis as well as pathogenic bacteria in food and milk. Therefore, it is very necessary for both bovine medicine and veterinary public health to emphasize and recognize this bacterial pathogen as the emerging disease of Staphylococcal bacteria and need further study about S. argenteus infection.

Keywords: Staphylococcus argenteus, subclinical bovine mastitis, Staphylococcus aureus complex, mass spectrometry, MLST

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Authors: V. Khosravi, F. D. Ardejani, A. Aryafar, M. Sedighi

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Heavy metals have a damaging impact for the environment, animals and humans due to their extreme toxicity and removing them from wastewaters is a very important and interesting task in the field of water pollution control. Biosorption is a relatively new method for treatment of wastewaters and recovery of heavy metals. In this study, a continuous fixed bed study was carried out by using Bacillus thuringiensis as a biosorbent for the removal of Cu and Mn ions from Sarcheshmeh Acid Mine Drainage (AMD). The effect of operating parameters such as flow rate and bed height on the sorption characteristics of B. thuringiensis was investigated at pH 6.0 for each metal ion. The experimental results showed that the breakthrough time decreased with increasing flow rate and decreasing bed height. The data also indicated that the equilibrium uptake of both metals increased with decreasing flow rate and increasing bed height. BDST, Thomas, and Yoon–Nelson models were applied to experimental data to predict the breakthrough curves. All models were found suitable for describing the whole dynamic behavior of the column with respect to flow rate and bed height. In order to regenerate the adsorbent, an elution step was carried out with 1 M HCl and five adsorption-desorption cycles were carried out in continuous manner.

Keywords: acid mine drainage, bacillus thuringiensis, biosorption, cu and mn ions, fixed bed

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Authors: Rezala Houria, Valverde Jose Luis, Romero Amaya, Molinari Alessandra, Maldotti Andrea

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The escalation of oil prices in 1973 confronted the oil industry with the problem of how to maximize the processing of crude oil, especially the heavy fractions, to give gasoline components. Strong impetus was thus given to the development of catalysts with relatively large pore sizes, which were able to deal with larger molecules than the existing molecular sieves, and with good thermal and hydrothermal stability. The oil embargo in 1973 therefore acted as a stimulus for the investigation and development of pillared clays. Iron doped titania-pillared montmorillonite clays was prepared using bentonite from deposits of Maghnia in western-Algeria. The preparation method consists of differents steps (purification of the raw bentonite, preparation of a pillaring agent solution and exchange of the cations located between the clay layers with the previously formed iron/titanium solution). The characterization of this material was carried out by X-ray fluorescence spectrometry, X-ray diffraction, textural measures by BET method, inductively coupled plasma atomic emission spectroscopy, diffuse reflectance UV visible spectroscopy, temperature- programmed desorption of ammonia and atomic absorption.This new material was investigated as photocatalyst for selective oxygenation of the liquid alkylaromatics such as: toluene, paraxylene and orthoxylene and the photocatalytic properties of it were compared with those of the titanium-pillared clays.

Keywords: iron doping, montmorillonite clays, pillared clays, oil industry

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Authors: Martial Pouzet, Marc Dubois, Karine Charlet, Alexis Béakou

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The availability, the ecologic and economic characteristics of wood are advantages which explain the very wide scope of applications of this material, in several domains such as paper industry, furniture, carpentry and building. However, wood is a hygroscopic material highly sensitive to ambient humidity and temperature. The swelling and the shrinking caused by water absorption and desorption cycles lead to crack and deformation in the wood volume, making it incompatible for such applications. In this study, dynamic fluorination using F2 gas was applied to wood samples (douglas and silver fir species) to decrease their hydrophilic character. The covalent grafting of fluorine atoms onto wood surface through a conversion of C-OH group into C-F was validated by Fourier-Transform infrared spectroscopy and 19F solid state Nuclear Magnetic Resonance. It revealed that the wood, which is initially hydrophilic, acquired a hydrophobic character comparable to that of the Teflon, thanks to fluorination. A good durability of this treatment was also determined by aging tests under ambient atmosphere and under UV irradiation. Moreover, this treatment allowed obtaining hydrophobic character without major structural (morphology, density and colour) or mechanical changes. The maintaining of these properties after fluorination, which requires neither toxic solvent nor heating, appears as a remarkable advantage over other more traditional physical and chemical wood treatments.

Keywords: cellulose, spectroscopy, surface treatment, water absorption

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Authors: Lifar M. S., Tereshchenko A. A., Bulgakov A. N., Guda S. A., Guda A. A., Soldatov A. V.

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Metal nanoparticles are widely used as heterogeneous catalysts to activate adsorbed molecules and reduce the energy barrier of the reaction. Reaction product yield depends on the interplay between elementary processes - adsorption, activation, reaction, and desorption. These processes, in turn, depend on the inlet feed concentrations, temperature, and pressure. At stationary conditions, the active surface sites may be poisoned by reaction byproducts or blocked by thermodynamically adsorbed gaseous reagents. Thus, the yield of reaction products can significantly drop. On the contrary, the dynamic control accounts for the changes in the surface properties and adjusts reaction parameters accordingly. Therefore dynamic control may be more efficient than stationary control. In this work, a reinforcement learning algorithm has been applied to control the simulation of CO oxidation on a catalyst. The policy gradient algorithm is learned to maximize the CO₂ production rate based on the CO and O₂ flows at a given time step. Nonstationary solutions were found for the regime with surface deactivation. The maximal product yield was achieved for periodic variations of the gas flows, ensuring a balance between available adsorption sites and the concentration of activated intermediates. This methodology opens a perspective for the optimization of catalytic reactions under nonstationary conditions.

Keywords: artificial intelligence, catalyst, co oxidation, reinforcement learning, dynamic control

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Authors: Zhao Bo

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The TiO2-Na2SO3 and SiO2-Na2SO3 nano-fluids were prepared using ultrasonic dispertion method without any surfactant addition to study the influence of nano-fluids on the mass transfer during forced sulfite oxidation in a thermostatic stirred tank, and the kinetic viscosity of nano-fluids was measured. The influence of temperature (30 ℃ ~ 50 ℃), solid loading of fine particle (0 Kg/m³~1.0 Kg/m³), stirring speed (50 r/min ~ 400 r/min), and particle size (10 nm~100 nm) on the average oxygen absorption rate were investigated in detail. Both TiO2 nano-particles and SiO2 nano-particles could remarkably improve the gas-liquid mass transfer. Oxygen absorption enhancement factor increases with the increase of solid loading of nano-particles to a critical value and then decreases with further increase of solid loading under 30℃. Oxygen absorption rate together with absorption enhancement factor increases with stirring speed. However, oxygen absorption enhancement factor decreases with the increase of temperature due to aggregation of nano-particles. Further inherent relationship between particle size, loading, surface area, viscosity, stirring speed, temperature, adsorption, desorption, and mass transfer was discussed in depth by analyzing the interaction mechanism.

Keywords: fine particles, nano-fluid, mass transfer enhancement, solid loading

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Authors: Komal Verma, V. S. Moholkar

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This paper reports investigations in the mineralization of industrial wastewater (COD = 3246 mg/L, TOC = 2500 mg/L) using a ternary (ultrasound + Fenton + adsorption) hybrid advanced oxidation process. Fe3O4 decorated activated charcoal (Fe3O4@AC) nanocomposites (surface area = 538.88 m2/g; adsorption capacity = 294.31 mg/g) were synthesized using co-precipitation. The wastewater treatment process was optimized using central composite statistical design. At optimum conditions, viz. pH = 4.2, H2O2 loading = 0.71 M, adsorbent dose = 0.34 g/L, reduction in COD and TOC of wastewater were 94.75% and 89%, respectively. This result is essentially a consequence of synergistic interactions among the adsorption of pollutants onto activated charcoal and surface Fenton reactions induced due to the leaching of Fe2+/Fe3+ ions from the Fe3O4 nanoparticles. Microconvection generated due to sonication assisted faster mass transport (adsorption/desorption) of pollutants between Fe₃O₄@AC nanocomposite and the solution. The net result of this synergism was high interactions and reactions among and radicals and pollutants that resulted in the effective mineralization of wastewater The Fe₃O₄@AC showed excellent recovery (> 90 wt%) and reusability (> 90% COD removal) in 5 successive cycles of treatment. LC-MS analysis revealed effective (> 50%) degradation of more than 25 significant contaminants (in the form of herbicides and pesticides) after the treatment with ternary hybrid AOP. Similarly, the toxicity analysis test using the seed germination technique revealed ~ 60% reduction in the toxicity of the wastewater after treatment.

Keywords: Fe₃O₄@AC nanocomposite, RSM, COD;, LC-MS, Toxicity

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Authors: H. C. Woo, F. Bouanis, C. S. Cojocaur

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Graphene, which consists of a single layer of carbon atoms in a honeycomb lattice, is an interesting potential optoelectronic material because of graphene’s high carrier mobility, zero bandgap, and electron–hole symmetry. Graphene can absorb light and convert it into a photocurrent over a wide range of the electromagnetic spectrum, from the ultraviolet to visible and infrared regimes. Over the last several years, a variety of graphene-based photodetectors have been reported, such as graphene transistors, graphene-semiconductor heterojunction photodetectors, graphene based bolometers. It is also reported that there are several physical mechanisms enabling photodetection: photovoltaic effect, photo-thermoelectric effect, bolometric effect, photogating effect, and so on. In this work, we report a simple approach for the realization of graphene based resistive photo-detection devices and the measurements of their photoelectrical response. The graphene were synthesized directly on the glass substrate by novel growth method patented in our lab. Then, the metal electrodes were deposited by thermal evaporation on it, with an electrode length and width of 1.5 mm and 300 μm respectively, using Co to fabricate simple graphene based resistive photosensor. The measurements show that the graphene resistive devices exhibit a photoresponse to the illumination of visible light. The observed re-sistance response was reproducible and similar after many cycles of on and off operations. This photoelectrical response may be attributed not only to the direct photocurrent process but also to the desorption of oxygen. Our work shows that the simple graphene resistive devices have potential in photodetection applications.

Keywords: graphene, resistive sensor, optoelectronics, photoresponse

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Authors: Débora N. Zambrano, Marina O. Gosatti, Leandro M. Dufou, Daniel A. Serrano, M. Mónica Guraya, Soledad Perez-Catán

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Nanoporous g-Al₂O₃ samples were synthesized via a sol-gel technique, introducing changes in the Yoldas´ method. The aim of the work was to achieve an effective control of the nanostructure properties and morphology of the final g-Al₂O₃. The influence of the reagent temperature during the hydrolysis was evaluated in case of water at 5 ºC and 98 ºC, and alkoxide at -18 ºC and room temperature. Sol-gel transitions were performed at 120 ºC and room temperature. All g-Al₂O₃ samples were characterized by X-ray diffraction, nitrogen adsorption and thermal analysis. Our results showed that temperature of both water and alkoxide has not much influence on the nanostructure of the final g-Al₂O₃, thus giving a structure very similar to that of samples obtained by the reference method as long as the reaction temperature above 75 ºC is reached soon enough. XRD characterization showed diffraction patterns corresponding to g-Al₂O₃ for all samples. Also BET specific area values (253-280 m²/g) were similar to those obtained by Yoldas’s original method. The temperature of the sol-gel transition does not affect the resulting sample structure, and crystalline boehmite particles were identified in all dried gels. We analyzed the reproducibility of the samples’ structure by preparing different samples under identical conditions; we found that performing the sol-gel transition at 120 ºC favors the production of more reproducible samples and also reduces significantly the time of the sol-gel reaction.

Keywords: nanostructure alumina, boehmite, sol-gel technique, N2 adsorption/desorption isotherm, pore size distribution, BET area.

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Authors: Magdalena Blachnio, Viktor Bogatyrov, Mariia Galaburda, Anna Derylo-Marczewska

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Agricultural waste materials from traditional oil mill and after extraction of natural raw materials in supercritical conditions were used for the preparation of carbon nanomaterials (activated carbons) by two various methods. Chemical activation using acetic acid and physical activation with a gaseous agent (carbon dioxide) were chosen as mild and environmentally friendly ones. The effect of influential factors: type of raw material, temperature and activation agent on the porous structure characteristics of the materials was discussed by using N₂ adsorption/desorption isotherms at 77 K. Furthermore scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were employed to examine the physicochemical properties of the obtained sorbents. Selection of a raw material and an optimization of the conditions of the synthesis process, allowed to obtain the cheap sorbents with a targeted distribution of pores enabling effective adsorption of the model organic pollutants carried out in the multicomponent systems. Adsorption behavior (capacity and rate) of the chosen activated carbons was estimated by utilizing Crystal violet (CV), 4-chlorophenoxyacetic acid (4-CPA), 2.4-dichlorophenoxyacetic acid (2.4-D) as the adsorbates. Both rate and adsorption capacity of the organics on the sorbents evidenced that the activated carbons could be effectively used in sewage treatment plants. The mechanisms of organics adsorption were studied and correlated with activated carbons properties.

Keywords: activated carbon, adsorption equilibrium, adsorption kinetics, organics adsorption

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Authors: Fredrick O. Okumu, Mangaka C. Matoetoe

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Silver-platinum (Ag-Pt) bimetallic nanoparticles (NPs) with varying mole fractions (1:1, 1:3 and 3:1) were prepared by co-reduction of hexachloroplatinate and silver nitrate with sodium citrate. Upon successful formation of both monometallic and bimetallic (BM) core shell nanoparticles, cyclic voltammetry (CV) was used to characterize the NPs. The drop coated nanofilms on the GC substrate showed characteristic peaks of monometallic Ag NPs; Ag+/Ag0 redox couple as well as the Pt NPs; hydrogen adsorption and desorption peaks. These characteristic peaks were confirmed in the bimetallic NPs voltammograms. The following varying current trends were observed in the BM NPs ratios; GCE/Ag-Pt 1:3 > GCE/Ag-Pt 3:1 > GCE/Ag-Pt 1:1. Fundamental electrochemical properties which directly or indirectly affects the applicability of films such as; diffusion coefficient (D), electroactive surface coverage, electrochemical band gap, electron transfer coefficient (α) and charge (Q) were assessed using Randles - Sevcik plot and Laviron’s equations . High charge and surface coverage was observed in GCE/Ag-Pt 1:3 which supports its enhanced current. GCE/Ag-Pt 3:1 showed high diffusion coefficient while GCE/Ag-Pt 1:1 possessed high electron transfer coefficient that is facilitated by its high apparent heterogeneous rate constant relative to other BM NPs ratios. Surface redox reaction was determined as adsorption controlled in all modified GCEs. Surface coverage is inversely proportional to size; therefore the surface coverage data suggests that Ag-Pt 1:1 NPs have a small particle size. Generally, GCE/Ag-Pt 1:3 depicts the best electrochemical properties.

Keywords: characterization, core-shell, electrochemical, nanoparticles

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Authors: Chaima Zoulikha Tabet Zatla, Nihel Dib, Sumeya Bedrane, Juan Carlos Hernandez Garrido, Redouane Bachir, Miguel Angel Cauqui, Jose Juan Calvino Gamez

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These last year's our planet has witnessed global warming, which is a serious threat to our lives; it has many causes, such as the CO₂ excess in the atmosphere that results from our activity, for the purpose of living in a neater and better environment, working and improving an eco-responsible energy system is a must. Valorization of biomass to produce biofuels is among the most compelling routes to decrease air pollution without considerable modification in current vehicle technology. Effective transformation of lignocellulosic biomass-derived compounds into liquid fuels and value-added chemicals is an economically viable solution. Presently, very competitive technics for the conversion of lignocellulosic biomass into platform chemicals, such as furfural and Hydroxymethylfurfural (HMF), are used. Furfural (C₅H₄O₂) is a major hemi cellulosic biomass-derived platform molecule. In our work, we focus on the valorization of lignocellulosic biomass derivative furfural that is transformed into biofuel through a hydrodeoxygenation reaction in general and involving a catalytic process. In order to get to this point, we are synthesizing and characterizing a series of catalysts with different amounts of Ru (0.5%, 1% and 2%) supported on alumina-silica mixed oxides with various molar ratios (Si/Al = 2.5; 5; 7; 10; 15). These catalysts will be characterized by numerous technics such as N₂ adsorption/desorption, Pyridine adsorption (acidity measure), FTIR, X-rays diffraction, AAS, TEM and SEM.

Keywords: furfural, ruthenium, silica-alumina, biomass, biofuel

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Authors: Lin Huang, Bo Wang, Armando Borgna

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Dehydration of glycerol to acrolein was conducted with solid acid catalysts in liquid phase in a batch reactor and in gas phase in a fix-bed reactor, respectively. In the liquid-phase reaction, ZSM-5, H3PO4-modified ZSM-5 and heteropolyacids including H3PW12O40•xH2O (HPW) and Cs2.5H0.5PW12O40 (CsPW) were studied as catalysts. High temperatures and high boiling point solvents such as sulfolane improved the selectivity to acrolein through suppressing the formation of polyglycerols and coke. Catalytic results and temperature-programmed desorption of ammonia showed that the yield of acrolein increased with increasing catalyst acidity within the range of weak acid strength. Weak acid sites favored the selectivity to acrolein whereas strong acid sites promoted the formation of coke. ZSM-5 possessing only acid sites led to a high acrolein yield, while heteropolyacid catalysts with strong acid sites produced a low acrolein yield. In the gas-phase reaction, HPW and CsPW supported on metal oxides such as SiO2, γ-Al2O3, SiO2-Al2O3, ZrO2 and silicate TUD-1 were studied as catalysts. HPW/TUD-1 was most active for the production of acrolein, followed by HPW/SiO2. An acrolein yield of 61 % was obtained over HPW/TUD-1. X-ray diffraction study suggested that HPW and CsPW were stable and more dispersed on SiO2, silicate TUD-1 and SiO2-Al2O3. It was found that the structures of HPW and CsPW were destroyed by interaction with γ-Al2O3 and ZrO2. Compared to CsPW/TUD-1, the higher acrolein yield with HPW/TUD-1 may be attributed to more Brønsted acid sites on HPW/TUD-1, based on preliminary pyridine adsorption IR study.

Keywords: dehydration, glycerol, acrolein, solid acid catalysts, gas-phase, liquid-phase

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Authors: Houria Rezala, Jose Luis Valverde, Amaya Romero, Alessandra Molinari, Andrea Maldotti

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A pillared montmorillonite containing iron doped titania (Fe/Ti-PILC) has been prepared from a natural clay. This material has been characterized by X-ray diffraction, nitrogen adsorption, temperature programmed desorption of ammonia, inductively coupled plasma atomic emission spectroscopy, atomic absorption, and diffuse reflectance UV-VIS spectroscopy. The layer structure of Fe/Ti-PILC resulted to be ordered with an insertion of pillars, which caused a slight increase in the basal spacing of the clay. Its specific surface area was about three times larger than that of the parent Na-montmorillonite due principally to the creation of a remarkable microporous network. The doped material was a robust photocatalyst able to oxidize liquid alkyl aromatics to the corresponding carbonylic derivatives, using O2 as the oxidizing species, at mild pressure and temperature conditions. Accumulation of valuable carbonylic derivatives was possible since their over-oxidation to carbon dioxide was negligible. Fe/Ti-PILC was able to discriminate between toluene and cyclohexane in favor of the aromatic compound with an efficiency that is about three times higher than that of titanium pillared clays (Ti-PILC). It is likely that the addition of iron favored the formation of new acid sites able to interact with the aromatic substrate. Iron doping caused a significant TiO2 visible light-induced activity (wavelength > 400 nm) with only minor negative effects on its performance under UV-light irradiation (wavelength > 290 nm).

Keywords: alkyl aromatics oxidation, heterogeneous photocatalysis, iron doping, pillared clays

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Authors: S. F. H. Tasfy, N. A. M. Zabidi, M.-S. Shaharun

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Utilization of CO2 as a carbon source to produce valuable chemicals is one of the important ways to reduce the global warming caused by increasing CO2 in the atmosphere. Supported metal catalysts are crucial for the production of clean and renewable fuels and chemicals from the stable CO2 molecules. The catalytic conversion of CO2 into methanol is recently under increased scrutiny as an opportunity to be used as a low-cost carbon source. Therefore, series of the bimetallic Cu/ZnO-based catalyst supported by SBA-15 were synthesized via impregnation technique with different total metal loading and tested in the catalytic hydrogenation of CO2 to methanol. The morphological and textural properties of the synthesized catalysts were determined by transmission electron microscopy (TEM), temperature programmed desorption, reduction, oxidation and pulse chemisorption (TPDRO), and N2-adsorption. The CO2 hydrogenation reaction was performed in microactivity fixed-bed system at 250 °C, 2.25 MPa, and H2/CO2 ratio of 3. Experimental results showed that the catalytic structure and performance was strongly affected by the loading of the active site. Where, the catalytic activity, methanol selectivity as well as the space-time yield increased with increasing the metal loading until it reaches the maximum values at a metal loading of 15 wt% while further addition of metal inhibits the catalytic performance. The higher catalytic activity of 14 % and methanol selectivity of 92 % were obtained over Cu/ZnO-SBA-15 catalyst with total bimetallic loading of 15 wt%. The excellent performance of 15 wt% Cu/ZnO-SBA-15 catalyst is attributed to the presence of well disperses active sites with small particle size, higher Cu surface area, and lower catalytic reducibility.

Keywords: hydrogenation of carbon dioxide, methanol synthesis, metal loading, Cu/ZnO-SBA-15 catalyst

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Authors: Chun-Wei Yeh, Santhanamoorthi Nachimuthu, Jyh-Chiang Jiang

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Reducing greenhouse gases or converting them into fuels and chemicals with added value is vital for the environment. Given the enhanced techniques for hydrocarbon extraction in this context, the catalytic conversion of methane to methanol is particularly intriguing for future applications as vehicle fuels and/or bulk chemicals. Metal-organic frameworks (MOFs) have received much attention recently for the oxidation of methane to methanol. In addition, biomimetic material, particulate methane monooxygenase (pMMO), has been reported to convert methane using copper oxide clusters as active sites. Inspired by these, in this study, we considered the well-known MIL-53(Al) MOF as support for copper oxide clusters (Cu2Ox, Cu3Ox) to investigate their reactivity towards methane oxidation using Density Functional Theory (DFT) calculations. The copper oxide clusters (Cu2O2, Cu3O2) are modeled by oxidizing copper clusters (Cu2, Cu3) with two oxidizers, O2 and N2O. The initial C-H bond activation barriers on Cu2O2/MIL-53(Al) and Cu3O2/MIL-53(Al) catalysts are 0.70 eV and 0.64 eV, respectively, and are the rate-determining steps in the overall methane conversion to methanol reactions. The desorption energy of the methanol over the Cu2O/MIL-53(Al) and Cu3O/MIL-53(Al) is 0.71eV and 0.75 eV, respectively. Furthermore, to explore the prospect of catalyst reusability, we considered the different oxidants and proposed the different reaction pathways for completing the reaction cycle and regenerating the active copper oxide clusters. To know the reason for the difference between bi-copper and tri-cooper systems, we also did an electronic analysis. Finally, we calculate the Microkinetic Simulation. The result shows that the reaction can happen at room temperature.

Keywords: DFT study, copper oxide cluster, MOFs, methane conversion

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Authors: S. Divya, M. Jose

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Over the past years, industrial dyes have emerged as a significant threat to aquatic life, extensively detected in drinking water and groundwater, thus contributing to water pollution due to their improper and excessive use. To address this issue, the utilization of core-shell structures has been prioritized as it demonstrates remarkable efficiency in utilizing light energy for catalytic reactions and exhibiting excellent photocatalytic activity despite the availability of various photocatalysts. This work focuses on the photocatalytic degradation of Nd₂O₃@SiO₂ CSNs under UV light irradiation against MB and RhB dyes. Different characterization techniques, including XRD, FTIR, and TEM analyses, were employed to reveal the material's structure, functional groups, and morphological features. VSM and XPS analyses confirmed the soft, paramagnetic nature and chemical states with respective atomic percentages, respectively. Optical band gaps, determined using the Tauc plot model, indicated 4.24 eV and 4.13 eV for Nd₂O₃ NPs and Nd₂O₃@SiO₂ CSNs, respectively. The reduced bandgap energy of Nd₂O₃@SiO₂ CSNs enhances light absorption in the UV range, potentially leading to improved photocatalytic efficiency. The Nd₂O₃@SiO₂ CSNs exhibited greater degradation efficiency, reaching 95% and 96% against MB and RhB dyes, while Nd₂O₃ NPs showed 90% and 92%, respectively. The enhanced efficiency of Nd₂O₃@SiO₂ CSNs can be attributed to the larger specific surface area provided by the SiO₂ shell, as confirmed by surface area analysis using the BET surface area analyzer through N₂ adsorption-desorption.

Keywords: core shell nanocomposites, rare earth oxides, photocatalysis, advanced oxidation process

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Authors: Issam Lakdhar, Akram Alhussein, Juan Creus

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With the huge increase in world energy consumption, researchers are working to find other alternative sources of energy instead of fossil fuel one causing many environmental problems as the production of greenhouse effect gases. Hydrogen is considered a green energy source, which its combustion does not cause environmental pollution. The transport and the storage of the gas molecules or the other products containing this smallest chemical element in metallic structures (pipelines, tanks) are crucial issues. The dissolve and the permeation of hydrogen into the metal lattice lead to the formation of hydride phases and the embrittlement of structures. To protect the metallic structures, a surface treatment could be a good solution. Among the different techniques, magnetron sputtering is used to elaborate micrometric coatings capable of slowing down or stop hydrogen permeation. In the plasma environment, the deposition parameters of new thin-film metallic glasses Al-Ti-W were optimized and controlled in order to obtain, hydrogen barrier. Many characterizations were carried out (SEM, XRD and Nano-indentation…) to control the composition and understand the influence of film microstructure and chemical composition on the hydrogen permeation through the coatings. The coating performance was evaluated under two hydrogen production methods: chemical and electrochemical (cathodic protection) techniques. The hydrogen quantity absorbed was experimentally determined using the Thermal-Desorption Spectroscopy method (TDS)). An ideal ATW thin film was developed and showed excellent behavior against the diffusion of hydrogen.

Keywords: thin films, hydrogen, PVD, plasma technology, electrochemical properties

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Authors: A. O. Adebayo, G. A. Idowu, F. Odegbemi

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Investigations on the recovery of nickel from aqueous solution using 2-hydroxy-5-nonyl- acetophenone oxime (LIX-84I) impregnated on activated charcoal was carried out. The LIX-84I was impregnated onto the pores of dried activated charcoal by dry method and optimum conditions for different equilibrium parameters (pH, adsorbent dosage, extractant concentration, agitation time and temperature) were determined using a simulated solution of nickel. The kinetics and adsorption isotherm studies were also evaluated. It was observed that the efficiency of recovery with LIX-84I impregnated on charcoal was dependent on the pH of the aqueous solution as there was little or no recovery at pH below 4. However, as the pH was raised, percentage recovery increases and peaked at pH 5.0. The recovery was found to increase with temperature up to 60ºC. Also it was observed that nickel adsorbed onto the loaded charcoal best at a lower concentration (0.1M) of the extractant when compared with higher concentrations. Similarly, a moderately low dosage (1 g) of the adsorbent showed better recovery than larger dosages. These optimum conditions were used to recover nickel from the leachate of Ni-MH batteries dissolved with sulphuric acid, and a 99.6% recovery was attained. Adsorption isotherm studies showed that the equilibrium data fitted best to Temkin model, with a negative value of constant, b (-1.017 J/mol) and a high correlation coefficient, R² of 0.9913. Kinetic studies showed that the adsorption process followed a pseudo-second order model. Thermodynamic parameter values (∆G⁰, ∆H⁰, and ∆S⁰) showed that the adsorption was endothermic and spontaneous. The impregnated charcoal appreciably recovered nickel using a relatively smaller volume of extractant than what is required in solvent extraction. Desorption studies showed that the loaded charcoal is reusable for three times, and so might be economical for nickel recovery from waste battery.

Keywords: charcoal, impregnated, LIX-84I, nickel, recovery

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Authors: Deepanjali Gurav, Kun Qian

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In-vitro metabolic diagnosis relies on designed materials-based analytical platforms for detection of selected metabolites in biological samples, which has a key role in disease detection and therapeutic evaluation in clinics. However, the basic challenge deals with developing a simple approach for metabolic analysis in bio-samples with high sample complexity and low molecular abundance. In this work, we report a designer plasmonic nanoshells based platform for direct detection of small metabolites in clinical samples for in-vitro metabolic diagnostics. We first synthesized a series of plasmonic core-shell particles with tunable nanoshell structures. The optimized plasmonic nanoshells as new matrices allowed fast, multiplex, sensitive, and selective LDI MS (Laser desorption/ionization mass spectrometry) detection of small metabolites in 0.5 μL of bio-fluids without enrichment or purification. Furthermore, coupling with isotopic quantification of selected metabolites, we demonstrated the use of these plasmonic nanoshells for disease detection and therapeutic evaluation in clinics. For disease detection, we identified patients with postoperative brain infection through glucose quantitation and daily monitoring by cerebrospinal fluid (CSF) analysis. For therapeutic evaluation, we investigated drug distribution in blood and CSF systems and validated the function and permeability of blood-brain/CSF-barriers, during therapeutic treatment of patients with cerebral edema for pharmacokinetic study. Our work sheds light on the design of materials for high-performance metabolic analysis and precision diagnostics in real cases.

Keywords: plasmonic nanoparticles, metabolites, fingerprinting, mass spectrometry, in-vitro diagnostics

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Authors: Chia-Chia Chang, Jhen-Ting Huang, Hu-Cheng Weng, An-Ya Lo

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This study developed a simple hierarchical porous carbon (HPC) synthesis process and used for supercapacitor application. In which, mesopore provides huge specific surface area, meanwhile, macropore provides excellent mass transfer. Thus the hierarchical porous electrode improves the charge-discharge performance. On the other hand, cerium oxide (CeO2) have also got a lot research attention owing to its rich in content, low in price, environmentally friendly, good catalytic properties, and easy preparation. Besides, a rapid redox reaction occurs between trivalent cerium and tetravalent cerium releases oxygen atom and increase the conductivity. In order to prevent CeO2 from disintegration under long-term charge-discharge operation, the CeO2 carbon porous materials were was integrated as composite material in this study. For in the ex-situ analysis, scanning electron microscope (SEM), X-ray diffraction (XRD), transmission electron microscope (TEM) analysis were adopted to identify the surface morphology, crystal structure, and microstructure of the composite. 77K Nitrogen adsorption-desorption analysis was used to analyze the porosity of each specimen. For the in-situ test, cyclic voltammetry (CV) and chronopotentiometry (CP) were conducted by potentiostat to understand the charge and discharge properties. Ragone plot was drawn to further analyze the resistance properties. Based on above analyses, the effect of macropores/mespores and the CeO2/HPC ratios on charge-discharge performance were investigated. As a result, the capacitance can be greatly enhanced by 2.6 times higher than pristine mesoporous carbon electrode.

Keywords: hierarchical porous carbon, cerium oxide, supercapacitor

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Authors: Thidarat Imyen, Paisan Kongkachuichay

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Cu-Zn/core-shell Al-MCM-41 catalyst with various copper species, prepared by a combination of three methods—substitution, ion-exchange, and impregnation, was studied for the selective catalytic reduction (SCR) of NO with NH3 at 300 °C for 150 min. In order to investigate the effects of Zn introduction on the nature of the catalyst, Cu/core-shell Al-MCM-41 and Zn/core-shell Al-MCM-41 catalysts were also studied. The roles of Zn promoter in the acidity and the NOx adsorption properties of the catalysts were investigated by in situ Fourier transform infrared spectroscopy (FTIR) of NH3 and NOx adsorption, and temperature-programmed desorption (TPD) of NH3 and NOx. The results demonstrated that the acidity of the catalyst was enhanced by the Zn introduction, as exchanged Zn(II) cations loosely bonded with Al-O-Si framework could create Brønsted acid sites by interacting with OH groups. Moreover, Zn species also provided the additional sites for NO adsorption in the form of nitrite (NO2–) and nitrate (NO3–) species, which are the key intermediates for SCR reaction. In addition, the effect of Zn on the nature of copper was studied by in situ FTIR of CO adsorption and in situ X-ray adsorption near edge structure (XANES). It was found that Zn species hindered the reduction of Cu(II) to Cu(0), resulting in higher Cu(I) species in the Zn promoted catalyst. The Cu-Zn/core-shell Al-MCM-41 exhibited higher catalytic activity compared with that of the Cu/core-shell Al-MCM-41 for the whole reaction time, as it possesses the highest amount of Cu(I) sites, which are responsible for SCR catalytic activity. The Cu-Zn/core-shell Al-MCM-41 catalyst also reached the maximum NO conversion of 100% with the average NO conversion of 76 %. The catalytic performance of the catalyst was further improved by using Zn promoter in the form of ZnO instead of reduced Zn species. The Cu-ZnO/core-shell Al-MCM-41 catalyst showed better catalytic performance with longer working reaction time, and achieved the average NO conversion of 81%.

Keywords: Al-MCM-41, copper, nitrogen oxide, selective catalytic reduction, zinc

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Authors: R. Hosny, Mahmoud F. Mubarak, Heba M. Salem, Asmaa A. Abdelrahman

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Oilfield scaling is a major problem in the oil and gas industry. Scale issues cost the industry millions of dollars in damage and lost production every year. One of the main causes of global production decline is scale. In this study, solid scale inhibitors based on silver tungstate loaded KIT-6 were synthesized and evaluated in both static and scale inhibition modeling. The silver tungstate loaded KIT-6 catalysts were synthesized via a simple impregnated method using 3D mesoporous KIT-6 as support. The synthesized materials were characterized using wide and low XRD, N2 adsorption–desorption analysis, TGA analysis, and FTIR, SEM, and XPS analysis. The scale inhibition efficiency of the synthesized materials was evaluated using a static scale inhibition test. The results of this study demonstrate the potential application of silver tungstate-loaded KIT-6 solid scale inhibitors for the oil and gas industry. The results of this study will contribute to the development of new and innovative solid scale inhibitors based on silver tungstate-loaded KIT-6. The inhibition efficiency of the scale inhibitor increases, and calcite scale inhibitor decreases with increasing pH (2 to8), it proposes that the scale inhibitor was more effective under alkaline conditions. An inhibition efficiency of 99% on calcium carbonate can be achieved at the optimal dosage of 7.5 ppm at 55oC, indicating that the scale inhibitor exhibits a relatively good inhibition performance on calcium carbonate. The use of these materials can potentially lead to more efficient and cost-effective solutions for scaling inhibition in various industrial processes.

Keywords: produced water treatment, solid scale inhibitors, calcite, silver tungestate, 3 D mesoporous KIT-6, oilfield scales, adsorption

Procedia PDF Downloads 140

Authors: K. Mohammed, M. Agarwal, J. Mewman, Y. Ren

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An optimum technic has been developed for extracting volatile organic compounds which contribute to the aroma of lime fruit (Citrus aurantifolia). The volatile organic compounds of healthy and infested lime fruit with California red scale Aonidiella aurantii were characterized using headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) as a very simple, efficient and nondestructive extraction method. A three-phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing and fibre exposure time for volatiles reaching equilibrium from whole lime fruit in the headspace of the chamber was 16 and 4 hours respectively. 5 min was selected as desorption time of the three-phase fibre. Herbivorous activity induces indirect plant defenses, as the emission of herbivorous-induced plant volatiles (HIPVs), which could be used by natural enemies for host location. GC-MS analysis showed qualitative differences among volatiles emitted by infested and healthy lime fruit. The GC-MS analysis allowed the initial identification of 18 compounds, with similarities higher than 85%, in accordance with the NIST mass spectral library. One of these were increased by A. aurantii infestation, D-limonene, and three were decreased, Undecane, α-Farnesene and 7-epi-α-selinene. From an applied point of view, the application of the above-mentioned VOCs may help boost the efficiency of biocontrol programs and natural enemies’ production techniques.

Keywords: lime fruit, Citrus aurantifolia, California red scale, Aonidiella aurantii, VOCs, HS-SPME/GC-FID-MS

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Authors: Sreetama Ghosh, Sundara Ramaprabhu

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Carbon dioxide gas has been a major cause for the worldwide increase in green house effect, which leads to climate change and global warming. So CO₂ capture & sequestration has become an effective way to reduce the concentration of CO₂ in the environment. One such way to capture CO₂ in porous materials is by adsorption process. A potential material in this aspect is porous hexagonal boron nitride or 'white graphene' which is a well-known two-dimensional layered material with very high thermal stability. It had been investigated that the sample with hierarchical pore structure and high specific surface area shows excellent performance in capturing carbon dioxide gas and thereby mitigating the problem of environmental pollution to the certain extent. Besides, the presence of sulfur as well as nitrogen in the sample synergistically helps in the increase in adsorption capacity. In this work, a cost effective single step synthesis of highly porous boron nitride nanosheets doped with sulfur had been demonstrated. Besides, the CO₂ adsorption-desorption studies were carried on using a pressure reduction technique. The studies show that the nanosheets exhibit excellent cyclic stability in storage performance. Thermodynamic studies suggest that the adsorption takes place mainly through physisorption. The studies show that the nanosheets exhibit excellent cyclic stability in storage performance. Further, the surface modification of the highly porous nano sheets carried out by incorporating ionic liquids had further enhanced the capturing capability of CO₂ gas in the nanocomposite, revealing that this particular material has the potential to be an excellent adsorbent of carbon dioxide gas.

Keywords: CO₂ capture, hexagonal boron nitride nanosheets, porous network, sulfur doping

Procedia PDF Downloads 239

Authors: Samuel K. Degife, Kamal K. Pant, Sapna Jain

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The world´s population and industrialization of countries continued to grow in an alarming rate irrespective of the security for food, energy supply, and pure water availability. As a result, the global energy consumption is observed to increase significantly. Fossil energy resources that mainly comprised of crude oil, coal, and natural gas have been used by mankind as the main energy source for almost two centuries. However, sufficient evidences are revealing that the consumption of fossil resource as transportation fuel emits environmental pollutants such as CO2, NOx, and SOx. These resources are dwindling rapidly besides enormous amount of problems associated such as fluctuation of oil price and instability of oil-rich regions. Biomass is a promising renewable energy candidate to replace fossil-based transportation fuel and chemical production. The present study aims at valorization of hexose sugars (glucose and fructose) using zeolite based catalysts in imidazolium based ionic liquid (1-butyl-3-methylimidazolium chloride, [BMIM] Cl) reaction media. The catalytic effect chromium impregnated H-ZSM-5 (Cr/H-ZSM-5) was studied for dehydration of hexose sugars. The wet impregnation method was used to prepare Cr/H-ZSM-5 catalyst. The characterization of the prepared catalyst was performed using techniques such as Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction analysis (XRD), Temperature-programmed desorption of ammonia (NH3-TPD) and BET-surface area analysis. The dehydration product, 5-hydroxymethylfurfural (5-HMF), was analyzed using high-performance liquid chromatography (HPLC). Cr/H-ZSM-5 was effective in dehydrating fructose with 87% conversion and 55% yield 5-HMF at 180 oC for 30 min of reaction time compared with H-ZSM-5 catalyst which yielded only 31% of 5-HMF at identical reaction condition.

Keywords: chromium, hexose, ionic liquid, , zeolite

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Authors: Shashank Bahri, Divyanshu Arya, Rajni Jain, Sreedevi Upadhyayula

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Petroleum products can be obtained from syngas catalytic conversion using Fischer Tropsch Reaction. The liquid fuels obtained from FTS are sulphur and nitrogen free and thus may easily meet the increasing stringent environment regulations. In the present work we have synthesized Meso porous ZSM-5 supported catalyst. Meso structure were created in H-ZSM-5 crystallites by demetalation via subsequent base and acid treatment. Desilication through base treatment provides H-ZSM-5 with pore size and volumes similar to amorphous SiO2 (Conventional Carrier). Modifying the zeolite texture and surface chemistry by Desilication and acid washing alters its accessibility and interactions with metal phase and consequently the CO adsorption behavior and hydrocarbon product distribution. Increasing the mesoporosity via desilication provides the micro porous zeolite with essential surface area to support optimally sized metal crystallites. This improves the metal dispersion and hence improve the activity of the catalyst. Transition metal (Co) was loaded using wet impregnation method. Synthesized catalysts were characterized by Infrared Spectroscopy, Powdered X-Ray Diffraction, Scanning Electron Microscopy (SEM), BET Method analytical techniques. Acidity of the catalyst which plays an important role in FTS reaction was measured by DRIFT setup pyridine adsorption instead of NH3 Temperature Programmed Desorption. The major difference is that, Pyridine Adsorption can distinguish between Lewis acidity and Bronsted Acidity, thus giving their relative strengths in the catalyst sample, whereas TPD gives total acidity including Lewis and Bronsted ones.

Keywords: mesopourus, fischer tropsch reaction, pyridine adsorrption, drift study

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Authors: Frank Jaksoni Mweta, Nozomu Adachi, Yoshikazu Todaka, Hirokazu Sato, Yuta Sato, Hiromi Miura, Masakazu Kobayashi, Chihiro Watanabe, Yoshiteru Aoyagi

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Advances in the consumption of hydrogen fuel increase demands of high strength steel pipes and storage tanks. However, high strength steels are highly sensitive to hydrogen embrittlement. Because the introduction of hydrogen into steel during the fabrication process or from the environment is unavoidable, it is essential to improve hydrogen embrittlement resistance of high strength steels through microstructural control. In the present study, the heterogeneous nanostructure with a tensile strength of about 1.8 GPa and the homogeneous nanostructure with a tensile strength of about 2.0 GPa of 316LN steels were generated after 92% heavy cold rolling and high-pressure torsion straining, respectively. The heterogeneous nanostructure is composed of twin domains, shear bands, and lamellar grains. The homogeneous nanostructure is composed of uniformly distributed ultrafine nanograins. The influence of heterogeneous and homogenous nanostructures on the hydrogen embrittlement resistance was investigated. The specimen for each nanostructure was electrochemically charged with hydrogen for 3, 6, 12, and 24 hours, respectively. Under the same hydrogen charging time, both nanostructures show almost the same concentration of the diffusible hydrogen based on the thermal desorption analysis. The tensile properties of the homogenous nanostructure were severely affected by the diffusible hydrogen. However, the diffusible hydrogen shows less impact on the tensile properties of the heterogeneous nanostructure. The difference in embrittlement behavior between the heterogeneous and homogeneous nanostructures was elucidated based on the mechanism of the cracks' growth observed in the tensile fractography. The hydrogen embrittlement was suppressed in the heterogeneous nanostructure because the twin domain became an obstacle for crack growth. The homogeneous nanostructure was not consisting an obstacle such as a twin domain; thus, the crack growth resistance was low in this nanostructure.

Keywords: diffusible hydrogen, heterogeneous nanostructure, homogeneous nanostructure, hydrogen embrittlement

Procedia PDF Downloads 117