Search results for: porous titanium alloy

Authors: Anuruddha Jayasuriya, Thanakorn Pheeraphan

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In this paper, a review of different mathematical models which can be used as prediction tools to assess the time to crack reinforced concrete (RC) due to corrosion is investigated. This investigation leads to an experimental study to validate a selected prediction model. Most of these mathematical models depend upon the mechanical behaviors, chemical behaviors, electrochemical behaviors or geometric aspects of the RC members during a corrosion process. The experimental program is designed to verify the accuracy of a well-selected mathematical model from a rigorous literature study. Fundamentally, the experimental program exemplifies both one-dimensional chloride diffusion using RC squared slab elements of 500 mm by 500 mm and two-dimensional chloride diffusion using RC squared column elements of 225 mm by 225 mm by 500 mm. Each set consists of three water-to-cement ratios (w/c); 0.4, 0.5, 0.6 and two cover depths; 25 mm and 50 mm. 12 mm bars are used for column elements and 16 mm bars are used for slab elements. All the samples are subjected to accelerated chloride corrosion in a chloride bath of 5% (w/w) sodium chloride (NaCl) solution. Based on a pre-screening of different models, it is clear that the well-selected mathematical model had included mechanical properties, chemical and electrochemical properties, nature of corrosion whether it is accelerated or natural, and the amount of porous area that rust products can accommodate before exerting expansive pressure on the surrounding concrete. The experimental results have shown that the selected model for both one-dimensional and two-dimensional chloride diffusion had ±20% and ±10% respective accuracies compared to the experimental output. The half-cell potential readings are also used to see the corrosion probability, and experimental results have shown that the mass loss is proportional to the negative half-cell potential readings that are obtained. Additionally, a statistical analysis is carried out in order to determine the most influential factor that affects the time to corrode the reinforcement in the concrete due to chloride diffusion. The factors considered for this analysis are w/c, bar diameter, and cover depth. The analysis is accomplished by using Minitab statistical software, and it showed that cover depth is the significant effect on the time to crack the concrete from chloride induced corrosion than other factors considered. Thus, the time predictions can be illustrated through the selected mathematical model as it covers a wide range of factors affecting the corrosion process, and it can be used to predetermine the durability concern of RC structures that are vulnerable to chloride exposure. And eventually, it is further concluded that cover thickness plays a vital role in durability in terms of chloride diffusion.

Keywords: accelerated corrosion, chloride diffusion, corrosion cracks, passivation layer, reinforcement corrosion

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Authors: Aman Johri, Sidhant Sood, Pooja Suresh

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This paper suggests a new and more efficient method of atomization of fuel in a combustor nozzle of a high bypass turbofan engine, using ultrasonic vibrations. Since atomization of fuel just before the fuel spray is injected into the combustion chamber is an important and crucial aspect related to functioning of a propulsion system, the technology suggested by this paper and the experimental analysis on the system components eventually proves to assist in complete and rapid combustion of the fuel in the combustor module of the engine. Current propulsion systems use carburetors, atomization nozzles and apertures in air intake pipes for atomization. The idea of this paper is to deploy new age hybrid technology, namely the Ultrasound Field Effect (UFE) to effectively atomize fuel before it enters the combustion chamber, as a viable and effective method to increase efficiency and improve upon existing designs. The Ultrasound Field Effect is applied axially, on diametrically opposite ends of an atomizer tube that gloves onto the combustor nozzle, where the fuel enters and exits under a pre-defined pressure. The Ultrasound energy vibrates the fuel particles to a breakup frequency. At reaching this frequency, the fuel particles start disintegrating into smaller diameter particles perpendicular to the axis of application of the field from the parent boundary layer of fuel flow over the baseplate. These broken up fuel droplets then undergo swirling effect as per the original nozzle design, with a higher breakup ratio than before. A significant reduction of the size of fuel particles eventually results in an increment in the propulsive efficiency of the engine. Moreover, the Ultrasound atomizer operates within a control frequency such that effects of overheating and induced vibrations are least felt on the overall performance of the engine. The design of an electrical manifold for the multiple-nozzle system over a typical can-annular combustor is developed along with this study, such that the product can be installed and removed easily for maintenance and repairing, can allow for easy access for inspections and transmits least amount of vibrational energy to the surface of the combustor. Since near-field ultrasound is used, the vibrations are easily controlled, thereby successfully reducing vibrations on the outer shell of the combustor. Experimental analysis is carried out on the effect of ultrasonic vibrations on flowing jet turbine fuel using an ultrasound generator probe and results of an effective decrease in droplet size across a constant diameter, away from the boundary layer of flow is noted using visual aid by observing under ultraviolet light. The choice of material for the Ultrasound inducer tube and crystal along with the operating range of temperatures, pressures, and frequencies of the Ultrasound field effect are also studied in this paper, while taking into account the losses incurred due to constant vibrations and thermal loads on the tube surface.

Keywords: atomization, ultrasound field effect, titanium mesh, breakup frequency, parent boundary layer, baseplate, propulsive efficiency, jet turbine fuel, induced vibrations

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Authors: A. Hamza, H. Kathyayini, N. Nagaraju

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Aluminophosphates, both amorphous and crystalline materials find applications as adsorbents, ceramics, and pigments and as catalysts/catalyst supports in organic fine chemical synthesis. Most of the applications are varied depending on the type of metal incorporated, particle size, surface area, porosity and morphology of aluminophosphate. The porous and surface properties of these materials are normally fine-tuned by adopting various preparation methodologies. Numerous crystalline microporous and mesoporous aluminophosphates and metal-aluminophosphates have been reported in literature, in which the synthesis has been carried out by using structure directing organic molecules/surfactants. In present work, amorphous aluminophosphate (AlP) and metal-aluminophosphates MAlP (M = Cu, Zn, Cr, Fe, Ce and Zr) and their mixed forms M-1M2AlP are prepared under a typical precipitation condition, i.e. at low temperature in order to keep the Von-Weirmann relative super saturation of the precipitating medium and obtain small size precipitate particles. These materials are prepared without using any surfactants. All materials are thoroughly characterised for surface and bulk properties by N2 adsorption-desorption technique, XRD, FT-IR, TG and SEM. The materials are also analysed for the amount and the strength of their surface acid sites, by NH3-TPD and CO2-TPD techniques respectively. All the materials prepared in the work are investigated for their catalytic activity in following applications in the synthesis of industrially important Jasminaldehyde via, aldol condensation of n-heptanal and benzaldehyde, in the synthesis of biologically important chalcones by Claisen-shmidth condensation of benzaldehyde and substituted chalcones. The effect of the amount of the catalysts, duration of the reaction, temperature of the reaction, molar ratio of the reactants has been studied. The porosity of pure aluminophosphate is found to be changed significantly by the incorporation of transition metals during preparation of aluminophosphate. The pore size increased from microporous to mesoporous and finally to macroporous by following order of metals Cu = Zn < Cr < Ce < Fe = Zr. The change in surface area and porosity of double metal-aluminophosphates depended on the concentration of both the metals. The acidity of aluminophosphate is either increased or decreased which depended on the type and valence of metals loaded. A good number of basic sites are created in metal-aluminophosphates irrespective of the metals used. A maximum catalytic activity for synthesis of both jasminaldehyde and chalcone is obtained by FeAlP as catalysts; these materials are characterized by decreased strength and concentration of acidic sites with optimum level basic sites.

Keywords: amorphous metal-aluminophosphates, surface properties, acidic-basic properties, Aldol, Claisen-Shmidth condensation, jasminaldehyde, chalcone

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Authors: Turin Datta, Kisor K. Sahu

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Structural materials used in today’s oil and gas exploration and drilling of both onshore and offshore oil and gas wells must possess superior tensile properties, excellent resistance to corrosive degradation that includes general, localized (pitting and crevice) and environment assisted cracking such as stress corrosion cracking and hydrogen embrittlement. The High Pressure and High Temperature (HPHT) wells are typically operated at temperature and pressure that can exceed 300-3500F and 10,000psi (69MPa) respectively which necessitates the use of exotic materials in these exotic sources of natural resources. This research investigation is focussed on the evaluation of tensile properties and corrosion behavior of AISI 4140 High-Strength Low Alloy Steel (HSLA) possessing tempered martensitic microstructure and Duplex 2205 Stainless Steel (DSS) having austenitic and ferritic phase. The selection of this two alloys are primarily based on economic considerations as 4140 HSLA is cheaper when compared to DSS 2205. Due to the harsh aggressive chemical species encountered in deep oil and gas wells like chloride ions (Cl-), carbon dioxide (CO2), hydrogen sulphide (H2S) along with other mineral organic acids, DSS 2205, having a dual-phase microstructure can mitigate the degradation resulting from the presence of both chloride ions (Cl-) and hydrogen simultaneously. Tensile properties evaluation indicates a ductile failure of DSS 2205 whereas 4140 HSLA exhibit quasi-cleavage fracture due to the phenomenon of ‘tempered martensitic embrittlement’. From the potentiodynamic polarization testing, it is observed that DSS 2205 has higher corrosion resistance than 4140 HSLA; the former exhibits passivity signifying resistance to localized corrosion while the latter exhibits active dissolution in all the environmental parameters space that was tested. From the Scanning Electron Microscopy (SEM) evaluation, it is understood that stable pits appear in DSS 2205 only when the temperature exceeds the critical pitting temperature (CPT). SEM observation of the corroded 4140 HSLA specimen tested in aqueous 3.5 wt.% NaCl solution reveals intergranular cracking which appears due to the adsorption and diffusion of hydrogen during polarization, thus, causing hydrogen-induced cracking/hydrogen embrittlement. General corrosion testing of DSS 2205 in acidic brine (pH~3.0) solution at ambient temperature using coupons indicate no weight loss even after three months whereas the corrosion rate of AISI 4140 HSLA is significantly higher after one month of testing.

Keywords: DSS 2205, polarization, pitting, SEM

Procedia PDF Downloads 264

Authors: S. Trafela, X. Xua, K. Zuzek Rozmana

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In this study, we used an accurate and precise method to measure the electrochemically active surface areas (Aecsa) of nickel electrodes. Calculated Aecsa is really important for the evaluation of an electro-catalyst’s activity in electrochemical reaction of different organic compounds. The method involves the electrochemical formation of Ni(OH)₂ and NiOOH in the presence of adsorbed oxalate in alkaline media. The studies were carried out using cyclic voltammetry with polycrystalline nickel as a reference material and electrodeposited nickel nanowires, homogeneous and heterogeneous nickel films. From cyclic voltammograms, the charge (Q) values for the formation of Ni(OH)₂ and NiOOH surface oxides were calculated under various conditions. At sufficiently fast potential scan rates (200 mV s⁻¹), the adsorbed oxalate limits the growth of the surface hydroxides to a monolayer. Although the Ni(OH)₂/NiOOH oxidation peak overlaps with the oxygen evolution reaction, in the reverse scan, the NiOOH/ Ni(OH)₂ reduction peak is well-separated from other electrochemical processes and can be easily integrated. The values of these integrals were used to correlate experimentally measured charge density with an electrochemically active surface layer. The Aecsa of the nickel nanowires, homogeneous and heterogeneous nickel films were calculated to be Aecsa-NiNWs = 4.2066 ± 0.0472 cm², Aecsa-homNi = 1.7175 ± 0.0503 cm² and Aecsa-hetNi = 2.1862 ± 0.0154 cm². These valuable results were expanded and used in electrochemical studies of formaldehyde oxidation. As mentioned nickel nanowires, heterogeneous and homogeneous nickel films were used as simple and efficient sensor for formaldehyde detection. For this purpose, electrodeposited nickel electrodes were modified in 0.1 mol L⁻¹ solution of KOH in order to expect electrochemical activity towards formaldehyde. The investigation of the electrochemical behavior of formaldehyde oxidation in 0.1 mol L⁻¹ NaOH solution at the surface of modified nickel nanowires, homogeneous and heterogeneous nickel films were carried out by means of electrochemical techniques such as cyclic voltammetric and chronoamperometric methods. From investigations of effect of different formaldehyde concentrations (from 0.001 to 0.1 mol L⁻¹) on electrochemical signal - current we provided catalysis mechanism of formaldehyde oxidation, detection limit and sensitivity of nickel electrodes. The results indicated that nickel electrodes participate directly in the electrocatalytic oxidation of formaldehyde. In the overall reaction, formaldehyde in alkaline aqueous solution exists predominantly in form of CH₂(OH)O⁻, which is oxidized to CH₂(O)O⁻. Taking into account the determined (Aecsa) values we have been able to calculate the sensitivities: 7 mA mol L⁻¹ cm⁻² for nickel nanowires, 3.5 mA mol L⁻¹ cm⁻² for heterogeneous nickel film and 2 mA mol L⁻¹ cm⁻² for heterogeneous nickel film. The detection limit was 0.2 mM for nickel nanowires, 0.5 mM for porous Ni film and 0.8 mM for homogeneous Ni film. All of these results make nickel electrodes capable for further applications.

Keywords: electrochemically active surface areas, nickel electrodes, formaldehyde, electrocatalytic oxidation

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Authors: Marta Paszkiewicz, Justyna Łuczak, Martyna Marchelek, Adriana Zaleska-Medynska

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In recent years, photocatalytical processes have been intensively investigated for destruction of pollutants, hydrogen evolution, disinfection of water, air and surfaces, for the construction of self-cleaning materials (tiles, glass, fibres, etc.). Titanium dioxide (TiO2) is the most popular material used in heterogeneous photocatalysis due to its excellent properties, such as high stability, chemical inertness, non-toxicity and low cost. It is well known that morphology and microstructure of TiO2 significantly influence the photocatalytic activity. This characteristics as well as other physical and structural properties of photocatalysts, i.e., specific surface area or density of crystalline defects, could be controlled by preparation route. In this regard, TiO2 particles can be obtained by sol-gel, hydrothermal, sonochemical methods, chemical vapour deposition and alternatively, by ionothermal synthesis using ionic liquids (ILs). In the TiO2 particles synthesis ILs may play a role of a solvent, soft template, reagent, agent promoting reduction of the precursor or particles stabilizer during synthesis of inorganic materials. In this work, the effect of the ILs anion type on morphology and photoactivity of TiO2 is presented. The preparation of TiO2 microparticles with spherical structure was successfully achieved by solvothermal method, using tetra-tert-butyl orthotitatane (TBOT) as the precursor. The reaction process was assisted by an ionic liquids 1-butyl-3-methylimidazolium bromide [BMIM][Br], 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF4] and 1-butyl-3-methylimidazolium haxafluorophosphate [BMIM][PF6]. Various molar ratios of all ILs to TBOT (IL:TBOT) were chosen. For comparison, reference TiO2 was prepared using the same method without IL addition. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Brenauer-Emmett-Teller surface area (BET), NCHS analysis, and FTIR spectroscopy were used to characterize the surface properties of the samples. The photocatalytic activity was investigated by means of phenol photodegradation in the aqueous phase as a model pollutant, as well as formation of hydroxyl radicals based on detection of fluorescent product of coumarine hydroxylation. The analysis results showed that the TiO2 microspheres had spherical structure with the diameters ranging from 1 to 6 µm. The TEM micrographs gave a bright observation of the samples in which the particles were comprised of inter-aggregated crystals. It could be also observed that the IL-assisted TiO2 microspheres are not hollow, which provides additional information about possible formation mechanism. Application of the ILs results in rise of the photocatalytic activity as well as BET surface area of TiO2 as compared to pure TiO2. The results of the formation of 7-hydroxycoumarin indicated that the increased amount of ·OH produced at the surface of excited TiO2 for samples TiO2_ILs well correlated with more efficient degradation of phenol. NCHS analysis showed that ionic liquids remained on the TiO2 surface confirming structure directing role of that compounds.

Keywords: heterogeneous photocatalysis, IL-assisted synthesis, ionic liquids, TiO2

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Authors: Bina Gupta, Rashmi Singh, Harshit Mahandra

Abstract:

Molybdenum is a strategic metal and finds applications in petroleum refining, thermocouples, X-ray tubes and in making of steel alloy owing to its high melting temperature and tensile strength. The growing significance and economic value of molybdenum has increased interest in the development of efficient processes aiming its recovery from secondary sources. Main secondary sources of Mo are molybdenum catalysts which are used for hydrodesulphurisation process in petrochemical refineries. The activity of these catalysts gradually decreases with time during the desulphurisation process as the catalysts get contaminated with toxic material and are dumped as waste which leads to environmental issues. In this scenario, recovery of molybdenum from spent catalyst is significant from both economic and environmental point of view. Recently ionic liquids have gained prominence due to their low vapour pressure, high thermal stability, good extraction efficiency and recycling capacity. The present study reports recovery of molybdenum from Mo-Co spent leach liquor using Cyphos IL 102[trihexyl(tetradecyl)phosphonium bromide] as an extractant. Spent catalyst was leached with 3.0 mol/L HCl, and the leach liquor containing Mo-870 ppm, Co-341 ppm, Al-508 ppm and Fe-42 ppm was subjected to extraction step. The effect of extractant concentration on the leach liquor was investigated and almost 85% extraction of Mo was achieved with 0.05 mol/L Cyphos IL 102. Results of stripping studies revealed that 2.0 mol/L HNO3 can effectively strip 94% of the extracted Mo from the loaded organic phase. McCabe- Thiele diagrams were constructed to determine the number of stages required for quantitative extraction and stripping of molybdenum and were confirmed by countercurrent simulation studies. According to McCabe- Thiele extraction and stripping isotherms, two stages are required for quantitative extraction and stripping of molybdenum at A/O= 1:1. Around 95.4% extraction of molybdenum was achieved in two-stage counter current at A/O= 1:1 with the negligible extraction of Co and Al. However, iron was coextracted and removed from the loaded organic phase by scrubbing with 0.01 mol/L HCl. Quantitative stripping (~99.5 %) of molybdenum was achieved with 2.0 mol/L HNO₃ in two stages at O/A=1:1. Overall ~95.0% molybdenum with 99 % purity was recovered from Mo-Co spent catalyst. From the strip solution, MoO₃ was obtained by crystallization followed by thermal decomposition. The product obtained after thermal decomposition was characterized by XRD, FE-SEM and EDX techniques. XRD peaks of MoO₃ correspond to molybdite Syn-MoO₃ structure. FE-SEM depicts the rod-like morphology of synthesized MoO₃. EDX analysis of MoO₃ shows 1:3 atomic percentage of molybdenum and oxygen. The synthesised MoO₃ can find application in gas sensors, electrodes of batteries, display devices, smart windows, lubricants and as a catalyst.

Keywords: cyphos Il 102, extraction, spent mo-co catalyst, recovery

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Authors: M. François, L. Sigot, C. Vallières

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Volatile Organic Compounds (VOCs) are a real health issue, particularly in domestic indoor environments. Among these VOCs, acetaldehyde is frequently monitored in dwellings ‘air, especially due to smoking and spontaneous emissions from the new wall and soil coverings. It is responsible for respiratory complaints and is classified as possibly carcinogenic to humans. Adsorption processes are commonly used to remove VOCs from the air. Metal-Organic Frameworks (MOFs) are a promising type of material for high adsorption performance. These hybrid porous materials composed of metal inorganic clusters and organic ligands are interesting thanks to their high porosity and surface area. The HKUST-1 (also referred to as MOF-199) is a copper-based MOF with the formula [Cu₃(BTC)₂(H₂O)₃]n (BTC = benzene-1,3,5-tricarboxylate) and exhibits unsaturated metal sites that can be attractive sites for adsorption. The objective of this study is to investigate the impact of HKUST-1 pretreatment on acetaldehyde adsorption. Thus, dynamic adsorption experiments were conducted in 1 cm diameter glass column packed with 2 cm MOF bed height. MOF were sieved to 630 µm - 1 mm. The feed gas (Co = 460 ppmv ± 5 ppmv) was obtained by diluting a 1000 ppmv acetaldehyde gas cylinder in air. The gas flow rate was set to 0.7 L/min (to guarantee a suitable linear velocity). Acetaldehyde concentration was monitored online by gas chromatography coupled with a flame ionization detector (GC-FID). Breakthrough curves must allow to understand the interactions between the MOF and the pollutant as well as the impact of the HKUST-1 humidity in the adsorption process. Consequently, different MOF water content conditions were tested, from a dry material with 7 % water content (dark blue color) to water saturated state with approximately 35 % water content (turquoise color). The rough material – without any pretreatment – containing 30 % water serves as a reference. First, conclusions can be drawn from the comparison of the evolution of the ratio of the column outlet concentration (C) on the inlet concentration (Co) as a function of time for different HKUST-1 pretreatments. The shape of the breakthrough curves is significantly different. The saturation of the rough material is slower (20 h to reach saturation) than that of the dried material (2 h). However, the breakthrough time defined for C/Co = 10 % appears earlier in the case of the rough material (0.75 h) compared to the dried HKUST-1 (1.4 h). Another notable difference is the shape of the curve before the breakthrough at 10 %. An abrupt increase of the outlet concentration is observed for the material with the lower humidity in comparison to a smooth increase for the rough material. Thus, the water content plays a significant role on the breakthrough kinetics. This study aims to understand what can explain the shape of the breakthrough curves associated to the pretreatments of HKUST-1 and which mechanisms take place in the adsorption process between the MOF, the pollutant, and the water.

Keywords: acetaldehyde, dynamic adsorption, HKUST-1, pretreatment influence

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Authors: A. T. Perez Fontenla, S. Sgobba, A. Bartkowska, Y. Askar, M. Dalemir Celuch, A. Newborough, M. Karppinen, H. Haalien, S. Deleval, S. Larcher, C. Charvet, L. Bruno, R. Trant

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The present study investigates the corrosion behavior of copper (Cu) based conducts predominantly brazed with Sil-Fos (self-fluxing copper-based filler with silver and phosphorus) within various cooling circuits of demineralized water across different particle accelerator components at CERN. The study covers a range of sample service time, from a few months to fifty years, and includes various accelerator components such as quadrupoles, dipoles, and bending magnets. The investigation comprises the established sample extraction procedure, examination methodology including non-destructive testing, evaluation of the corrosion phenomena, and identification of commonalities across the studied components as well as analysis of the environmental influence. The systematic analysis included computed microtomography (CT) of the joints that revealed distributed defects across all brazing interfaces. Some defects appeared to result from areas not wetted by the filler during the brazing operation, displaying round shapes, while others exhibited irregular contours and radial alignment, indicative of a network or interconnection. The subsequent dry cutting performed facilitated access to the conduct's inner surface and the brazed joints for further inspection through light and electron microscopy (SEM) and chemical analysis via Energy Dispersive X-ray spectroscopy (EDS). Brazing analysis away from affected areas identified the expected phases for a Sil-Fos alloy. In contrast, the affected locations displayed micrometric cavities propagating into the material, along with selective corrosion of the bulk Cu initiated at the conductor-braze interface. Corrosion product analysis highlighted the consistent presence of sulfur (up to 6 % in weight), whose origin and role in the corrosion initiation and extension is being further investigated. The importance of this study is paramount as it plays a crucial role in comprehending the underlying factors contributing to recently identified water leaks and evaluating the extent of the issue. Its primary objective is to provide essential insights for the repair of impacted brazed joints when accessibility permits. Moreover, the study seeks to contribute to the improvement of design and manufacturing practices for future components, ultimately enhancing the overall reliability and performance of magnet systems within CERN accelerator facilities.

Keywords: accelerator facilities, brazed copper conducts, demineralized water, magnets

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Authors: Osman Adiguzel

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Shape memory effect is a peculiar property exhibited by certain alloy systems and based on martensitic transformation, and shape memory properties are closely related to the microstructures of the material. Shape memory effect is linked with martensitic transformation, which is a solid state phase transformation and occurs with the cooperative movement of atoms by means of lattice invariant shears on cooling from high-temperature parent phase. Lattice twinning and detwinning can be considered as elementary processes activated during the transformation. Thermally induced martensite occurs as martensite variants, in self-accommodating manner and consists of lattice twins. Also, this martensite is called the twinned martensite or multivariant martensite. Deformation of shape memory alloys in martensitic state proceeds through a martensite variant reorientation. The martensite variants turn into the reoriented single variants with deformation, and the reorientation process has great importance for the shape memory behavior. Copper based alloys exhibit this property in metastable β- phase region, which has DO3 –type ordered lattice in ternary case at high temperature, and these structures martensiticaly turn into the layered complex structures with lattice twinning mechanism, on cooling from high temperature parent phase region. The twinning occurs as martensite variants with lattice invariant shears in two opposite directions, <110 > -type directions on the {110}- type plane of austenite matrix. Lattice invariant shear is not uniform in copper based ternary alloys and gives rise to the formation of unusual layered structures, like 3R, 9R, or 18R depending on the stacking sequences on the close-packed planes of the ordered lattice. The unit cell and periodicity are completed through 18 atomic layers in case of 18R-structure. On the other hand, the deformed material recovers the original shape on heating above the austenite finish temperature. Meanwhile, the material returns to the twinned martensite structures (thermally induced martensite structure) in one way (irreversible) shape memory effect on cooling below the martensite finish temperature, whereas the material returns to the detwinned martensite structure (deformed martensite) in two-way (reversible) shape memory effect. Shortly one can say that the microstructural mechanisms, responsible for the shape memory effect are the twinning and detwinning processes as well as martensitic transformation. In the present contribution, x-ray diffraction, transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) studies were carried out on two copper-based ternary alloys, CuZnAl, and CuAlMn.

Keywords: shape memory effect, martensitic transformation, twinning and detwinning, layered structures

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Authors: Bina Gupta, Rashmi Singh, Harshit Mahandra

Abstract:

Molybdenum is a strategic metal and finds applications in petroleum refining, thermocouples, X-ray tubes and in making of steel alloy owing to its high melting temperature and tensile strength. The growing significance and economic value of molybdenum have increased interest in the development of efficient processes aiming its recovery from secondary sources. Main secondary sources of Mo are molybdenum catalysts which are used for hydrodesulphurisation process in petrochemical refineries. The activity of these catalysts gradually decreases with time during the desulphurisation process as the catalysts get contaminated with toxic material and are dumped as waste which leads to environmental issues. In this scenario, recovery of molybdenum from spent catalyst is significant from both economic and environmental point of view. Recently ionic liquids have gained prominence due to their low vapour pressure, high thermal stability, good extraction efficiency and recycling capacity. Present study reports recovery of molybdenum from Mo-Co spent leach liquor using Cyphos IL 102[trihexyl(tetradecyl)phosphonium bromide] as an extractant. Spent catalyst was leached with 3 mol/L HCl and the leach liquor containing Mo-870 ppm, Co-341 ppm, Al-508 ppm and Fe-42 ppm was subjected to extraction step. The effect of extractant concentration on the leach liquor was investigated and almost 85% extraction of Mo was achieved with 0.05 mol/L Cyphos IL 102. Results of stripping studies revealed that 2 mol/L HNO3 can effectively strip 94% of the extracted Mo from the loaded organic phase. McCabe-Thiele diagrams were constructed to determine the number of stages required for quantitative extraction and stripping of molybdenum and were confirmed by counter current simulation studies. According to McCabe-Thiele extraction and stripping isotherms, two stages are required for quantitative extraction and stripping of molybdenum at A/O= 1:1. Around 95.4% extraction of molybdenum was achieved in two stage counter current at A/O= 1:1 with negligible extraction of Co and Al. However, iron was coextracted and removed from the loaded organic phase by scrubbing with 0.01 mol/L HCl. Quantitative stripping (~99.5 %) of molybdenum was achieved with 2.0 mol/L HNO3 in two stages at O/A=1:1. Overall ~95.0% molybdenum with 99 % purity was recovered from Mo-Co spent catalyst. From the strip solution, MoO3 was obtained by crystallization followed by thermal decomposition. The product obtained after thermal decomposition was characterized by XRD, FE-SEM and EDX techniques. XRD peaks of MoO3correspond to molybdite Syn-MoO3 structure. FE-SEM depicts the rod like morphology of synthesized MoO3. EDX analysis of MoO3 shows 1:3 atomic percentage of molybdenum and oxygen. The synthesised MoO3 can find application in gas sensors, electrodes of batteries, display devices, smart windows, lubricants and as catalyst.

Keywords: cyphos IL 102, extraction, Mo-Co spent catalyst, recovery

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Authors: Asad Hanif, Pavithra Parthasarathy, Zongjin Li

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Thermal insulating composites help to reduce the total power consumption in a building by creating a barrier between external and internal environment. Such composites can be used in the roofing tiles or wall panels for exterior surfaces. This study purposes to develop lightweight cement-based composites for thermal insulating applications. Waste materials like silica fume (an industrial by-product) and fly ash cenosphere (FAC) (hollow micro-spherical shells obtained as a waste residue from coal fired power plants) were used as partial replacement of cement and lightweight filler, respectively. Moreover, aerogel, a nano-porous material made of silica, was also used in different dosages for improved thermal insulating behavior, while poly vinyl alcohol (PVA) fibers were added for enhanced toughness. The raw materials including binders and fillers were characterized by X-Ray Diffraction (XRD), X-Ray Fluorescence spectroscopy (XRF), and Brunauer–Emmett–Teller (BET) analysis techniques in which various physical and chemical properties of the raw materials were evaluated like specific surface area, chemical composition (oxide form), and pore size distribution (if any). Ultra-lightweight cementitious composites were developed by varying the amounts of FAC and aerogel with 28-day unit weight ranging from 1551.28 kg/m³ to 1027.85 kg/m³. Excellent mechanical and thermal insulating properties of the resulting composites were obtained ranging from 53.62 MPa to 8.66 MPa compressive strength, 9.77 MPa to 3.98 MPa flexural strength, and 0.3025 W/m-K to 0.2009 W/m-K as thermal conductivity coefficient (QTM-500). The composites were also tested for peak temperature difference between outer and inner surfaces when subjected to heating (in a specially designed experimental set-up) by a 275W infrared lamp. The temperature difference up to 16.78 ^oC was achieved, which indicated outstanding properties of the developed composites to act as a thermal barrier for building envelopes. Microstructural studies were carried out by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) for characterizing the inner structure of the composite specimen. Also, the hydration products were quantified using the surface area mapping and line scale technique in EDS. The microstructural analyses indicated excellent bonding of FAC and aerogel in the cementitious system. Also, selective reactivity of FAC was ascertained from the SEM imagery where the partially consumed FAC shells were observed. All in all, the lightweight fillers, FAC, and aerogel helped to produce the lightweight composites due to their physical characteristics, while exceptional mechanical properties, owing to FAC partial reactivity, were achieved.

Keywords: aerogel, cement-based, composite, fly ash cenosphere, lightweight, sustainable development, thermal conductivity

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Authors: Mehran Nozari-Asbemarz, Italo Pisano, Simin Arshi, Edmond Magner, James J. Leahy

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Integrating electrolytic synthesis with renewable energy makes it feasible to address urgent environmental and energy challenges. Conventional water electrolyzers concurrently produce H₂ and O₂, demanding additional procedures in gas separation to prevent contamination of H₂ with O₂. Moreover, the oxygen evolution reaction (OER), which is sluggish and has a low overall energy conversion efficiency, does not deliver a significant value product on the electrode surface. Compared to conventional water electrolysis, integrating electrolytic hydrogen generation from water with thermodynamically more advantageous aqueous organic oxidation processes can increase energy conversion efficiency and create value-added compounds instead of oxygen at the anode. One strategy is to use renewable and sustainable carbon sources from biomass, which has a large annual production capacity and presents a significant opportunity to supplement carbon sourced from fossil fuels. Numerous catalytic techniques have been researched in order to utilize biomass economically. Because of its safe operating conditions, excellent energy efficiency, and reasonable control over production rate and selectivity using electrochemical parameters, electrocatalytic upgrading stands out as an appealing choice among the numerous biomass refinery technologies. Therefore, we propose a broad framework for coupling H2 generation from water splitting with oxidative biomass upgrading processes. Four representative biomass targets were considered for oxidative upgrading that used a hierarchically porous CoFe-MOF/LDH @ Graphite Paper bifunctional electrocatalyst, including glucose, ethanol, benzyl, furfural, and 5-hydroxymethylfurfural (HMF). The potential required to support 50 mA cm-2 is considerably lower than (~ 380 mV) the potential for OER. All four compounds can be oxidized to yield liquid byproducts with economic benefit. The electrocatalytic oxidation of glucose to the value-added products, gluconic acid, glucuronic acid, and glucaric acid, was examined in detail. The cell potential for combined H₂ production and glucose oxidation was substantially lower than for water splitting (1.44 V(RHE) vs. 1.82 V(RHE) for 50 mA cm-2). In contrast, the oxidation byproduct at the anode was significantly more valuable than O₂, taking advantage of the more favorable glucose oxidation in comparison to the OER. Overall, such a combination of HER and oxidative biomass valorization using electrocatalysts prevents the production of potentially explosive H₂/O₂mixtures and produces high-value products at both electrodes with lower voltage input, thereby increasing the efficiency and activity of electrocatalytic conversion.

Keywords: biomass, electrocatalytic, glucose oxidation, hydrogen evolution

Procedia PDF Downloads 97

Authors: Majid Farsadrouh Rashti, Alireza Mohammadinejad, Amir Shafiee Kisomi

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Lead (Pb²⁺), a cation, is a prime constituent of the majority of the industrial effluents such as mining, smelting and coal combustion, Pb-based painting and Pb containing pipes in water supply systems, paper and pulp refineries, printing, paints and pigments, explosive manufacturing, storage batteries, alloy and steel industries. The maximum permissible limit of lead in the water used for drinking and domesticating purpose is 0.01 mg/L as advised by Bureau of Indian Standards, BIS. This becomes the acceptable 'safe' level of lead(II) ions in water beyond which, the water becomes unfit for human use and consumption, and is potential enough to lead health problems and epidemics leading to kidney failure, neuronal disorders, and reproductive infertility. Superabsorbent hydrogels are loosely crosslinked hydrophilic polymers that in contact with aqueous solution can easily water and swell to several times to their initial volume without dissolving in aqueous medium. Superabsorbents are kind of hydrogels capable to swell and absorb a large amount of water in their three-dimensional networks. While the shapes of hydrogels do not change extensively during swelling, because of tremendously swelling capacity of superabsorbent, their shape will broadly change.Because of their superb response to changing environmental conditions including temperature pH, and solvent composition, superabsorbents have been attracting in numerous industrial applications. For instance, water retention property and subsequently. Natural-based superabsorbent hydrogels have attracted much attention in medical pharmaceutical, baby diapers, agriculture, and horticulture because of their non-toxicity, biocompatibility, and biodegradability. Novel superabsorbent hydrogel nanocomposites were prepared by graft copolymerization of acrylamide and itaconic acid in the presence of nanoclay (laponite), using methylene bisacrylamide (MBA) and potassium persulfate, former as a crosslinking agent and the second as an initiator. The superabsorbent hydrogel nanocomposites structure was characterized by FTIR spectroscopy, SEM and TGA Spectroscopy adsorption of metal ions on poly (AAm-co-IA). The equilibrium swelling values of copolymer was determined by gravimetric method. During the adsorption of metal ions on polymer, residual metal ion concentration in the solution and the solution pH were measured. The effects of the clay content of the hydrogel on its metal ions uptake behavior were studied. The NC hydrogels may be considered as a good candidate for environmental applications to retain more water and to remove heavy metals.

Keywords: adsorption, hydrogel, nanocomposite, super adsorbent

Procedia PDF Downloads 187

Authors: Boriana Karamanova, Svetlana Veleva, Luybomir Soserov, Ana Arenillas, Francesco Lufrano, Antonia Stoyanova

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Supercapacitors have received a lot of research attention and are promising energy storage devices due to their high power and long cycle life. In order to developed an advanced device with significant capacity for storing charge and cheap carbon materials, efforts must focus not only on improving synthesis by controlling the morphology and pore size but also on improving electrode-electrolyte compatibility of the resulting systems. The present study examines the relationship between the surface chemistry of two activated carbon xerogels, the electrolyte type, and the electrochemical properties of supercapacitors. Activated carbon xerogels were prepared by varying the initial pH of the resorcinol-formaldehyde aqueous solution. The materials produced are physicochemical characterized by DTA/TGA, porous characterization, and SEM analysis. The carbon xerogel based electrodes were prepared by spreading over glass plate a slurry containing the carbon gel, graphite, and poly vinylidene difluoride (PVDF) binder. The layer formed was dried consecutively at different temperatures and then detached by water. After, the layer was dried again to improve its mechanical stability. The developed electrode materials and the Aquivion® E87-05S membrane (Solvay Specialty Polymers), socked in Na2SO4 as a polymer electrolyte, were used to assembly the solid-state supercapacitor. Symmetric supercapacitor cells composed by same electrodes and 1 M KOH electrolytes are also assembled and tested for comparison. The supercapacitor performances are verified by different electrochemical methods - cyclic voltammetry, galvanostatic charge/discharge measurements, electrochemical impedance spectroscopy, and long-term durability tests in neutral and alkaline electrolytes. Specific capacitances, energy, and power density, energy efficiencies, and durability were compared into studied supercapacitors. Ex-situ physicochemical analyses on the synthesized materials have also been performed, which provide information about chemical and structural changes in the electrode morphology during charge / discharge durability tests. They are discussed on the basis of electrode-electrolyte interaction. The obtained correlations could be of significance in order to design sustainable solid-state supercapacitors with high power and energy density. Acknowledgement: This research is funded by the Ministry of Education and Science of Bulgaria under the National Program "European Scientific Networks" (Agreement D01-286 / 07.10.2020, D01-78/30.03.2021). Authors gratefully acknowledge.

Keywords: carbon xerogel, electrochemical tests, neutral and alkaline electrolytes, supercapacitors

Procedia PDF Downloads 136

Authors: Chien-Chun Huang, Yi-U Chiou, Chiun-C.R. Wang

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For longer shelf life of noodles, air-dried method is the traditional way for the noodle preparation. Microwave drying has the specific advantage of rapid and uniform heating due to the penetration of microwaves into the body of the product. Microwave-assisted facility offers a quick and energy saving method during food dehydration as compares to the conventional air-dried method. Recently, numerous studies in the rheological characteristics of pasta or spaghetti were carried out with microwave–assisted air driers and many agricultural products were dried successfully. There are few researches about the evaluation of physicochemical characteristics and cooking quality of microwave-assisted air dried salted noodles. The purposes of this study were to compare the difference between conventional and microwave-assisted drying method on the physicochemical properties and eating quality of rice bran noodles. Three different microwave power including 0.5 KW, 0.75 KW and 1.0 KW installing with 50℃ hot air were applied for dehydration of rice bran noodles in this study. Three proportion of rice bran ranging in 0-20% were incorporated into salted noodles processing. The appearance, optimum cooking time, cooking yield and losses, textural profiles analysis, sensory evaluation of rice bran noodles were measured in this study. The results indicated that high power (1.0 KW) microwave facility caused partially burnt and porous on the surface of rice bran noodles. However, no characteristic of noodle was appeared on the surface of noodles preparing by low power (0.5 KW) microwave facility. The optimum cooking time of noodles was decreased as higher power microwave or higher proportion of rice bran was incorporated into noodles preparation. The higher proportion of rice bran (20%) or higher power of microwave-assisted dried noodles obtained the higher color intensity and the higher cooking losses as compared with conventional air dried noodles. The firmness of cooked rice bran noodles slightly decreased in the cooked noodles which were dried by high power microwave-assisted method. The shearing force, tensile strength, elasticity and texture profiles of cooked rice noodles decreased with the progress of the proportion of rice bran. The results of sensory evaluation indicated conventional dried noodles obtained the higher springiness, cohesiveness and acceptability of cooked noodles than high power (1.0 KW) microwave-assisted dried noodles. However, low power (0.5 KW) microwave-assisted dried noodles showed the comparable sensory attributes and acceptability with conventional dried noodles. Moreover, the sensory attributes including firmness, springiness, cohesiveness decreased, but stickiness increased, with the increases of rice bran proportion. These results inferred that incorporation of lower proportion of rice bran and lower power microwave-assisted dried noodles processing could produce faster cooking time and acceptable quality of cooked noodles as compared to conventional dried noodles.

Keywords: microwave-assisted drying method, physicochemical characteristics, rice bran noodles, sensory evaluation

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Authors: Hsyi-En Cheng, Ying-Yi Liou

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Metal-oxide semiconductor (MOS) gas sensors are widely used in the gas-detection market due to their high sensitivity, fast response, and simple device structures. However, the high working temperature of MOS gas sensors makes them difficult to integrate with the appliance or consumer goods. One-dimensional (1-D) nanostructures are considered to have the potential to lower their working temperature due to their large surface-to-volume ratio, confined electrical conduction channels, and small feature sizes. Unfortunately, the difficulty of fabricating 1-D nanostructure electrodes has hindered the development of low-temperature MOS gas sensors. In this work, we proposed a method to fabricate nanotube-arrays, and the SnO₂ nanotube-array sensors with different wall thickness were successfully prepared and examined. The fabrication of SnO₂ nanotube arrays incorporates the techniques of barrier-free anodic aluminum oxide (AAO) template and atomic layer deposition (ALD) of SnO₂. First, 1.0 µm Al film was deposited on ITO glass substrate by electron beam evaporation and then anodically oxidized by five wt% phosphoric acid solution at 5°C under a constant voltage of 100 V to form porous aluminum oxide. As the Al film was fully oxidized, a 15 min over anodization and a 30 min post chemical dissolution were used to remove the barrier oxide at the bottom end of pores to generate a barrier-free AAO template. The ALD using reactants of TiCl4 and H₂O was followed to grow a thin layer of SnO₂ on the template to form SnO₂ nanotube arrays. After removing the surface layer of SnO₂ by H₂ plasma and dissolving the template by 5 wt% phosphoric acid solution at 50°C, upright standing SnO₂ nanotube arrays on ITO glass were produced. Finally, Ag top electrode with line width of 5 μm was printed on the nanotube arrays to form SnO₂ nanotube-array sensor. Two SnO₂ nanotube-arrays with wall thickness of 30 and 60 nm were produced in this experiment for the evaluation of gas sensing ability. The flat SnO₂ films with thickness of 30 and 60 nm were also examined for comparison. The results show that the properties of ALD SnO₂ films were related to the deposition temperature. The films grown at 350°C had a low electrical resistivity of 3.6×10-3 Ω-cm and were, therefore, used for the nanotube-array sensors. The carrier concentration and mobility of the SnO₂ films were characterized by Ecopia HMS-3000 Hall-effect measurement system and were 1.1×1020 cm-3 and 16 cm3/V-s, respectively. The electrical resistance of SnO₂ film and nanotube-array sensors in air and in a 5% H₂-95% N₂ mixture gas was monitored by Pico text M3510A 6 1/2 Digits Multimeter. It was found that, at 200 °C, the 30-nm-wall SnO₂ nanotube-array sensor performs the highest responsivity to 5% H₂, followed by the 30-nm SnO₂ film sensor, the 60-nm SnO₂ film sensor, and the 60-nm-wall SnO₂ nanotube-array sensor. However, at temperatures below 100°C, all the samples were insensitive to the 5% H₂ gas. Further investigation on the sensors with thinner SnO₂ is necessary for improving the sensing ability at temperatures below 100 °C.

Keywords: atomic layer deposition, nanotube arrays, gas sensor, tin dioxide

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Authors: Burçak Boztemur, Yue Xu, Laima Luo, M. Lütfi Öveçoğlu, Duygu Ağaoğulları

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Tungsten (W) is used chiefly as plasma-facing material. However, it has some problems, such as brittleness after plasma exposure. High-entropy alloys (RHEAs) are a new opportunity for this deficiency. So, the neutron shielding behavior of WNbMoVTa and WNbMoVTaCr₀.₅Al compositions were examined against He⁺ irradiation in this study. The mechanical and irradiation properties of the WNbMoVTa base composition were investigated by adding the Al and Cr elements. The mechanical alloying (MA) for 6 hours was applied to obtain RHEA powders. According to the X-ray diffraction (XRD) method, the body-centered cubic (BCC) phase and NbTa phase with a small amount of WC impurity that comes from vials and balls were determined after 6 h MA. Also, RHEA powders were consolidated with the spark plasma sintering (SPS) method (1500 ºC, 30 MPa, and 10 min). After the SPS method, (Nb,Ta)C and W₂C₀.₈₅ phases were obtained with the decomposition of WC and stearic acid that is added during MA based on XRD results. Also, the BCC phase was obtained for both samples. While the Al₂O₃ phase with a small intensity was seen for the WNbMoVTaCr₀.₅Al sample, the Ta₂VO₆ phase was determined for the base sample. These phases were observed as three different regions according to scanning electron microscopy (SEM). All elements were distributed homogeneously on the white region by measuring an electron probe micro-analyzer (EPMA) coupled with a wavelength dispersive spectroscope (WDS). Also, the grey region of the WNbMoVTa sample was rich in Ta, V, and O elements. However, the amount of Al and O elements was higher for the grey region of the WNbMoVTaCr₀.₅Al sample. The high amount of Nb, Ta, and C elements were determined for both samples. Archimedes’ densities that were measured with alcohol media were closer to the theoretical densities of RHEAs. These values were important for the microhardness and irradiation resistance of compositions. While the Vickers microhardness value of the WNbMoVTa sample was measured as ~11 GPa, this value increased to nearly 13 GPa with the WNbMoVTaCr₀.₅Al sample. These values were compatible with the wear behavior. The wear volume loss was decreased to 0.16×10⁻⁴ from 1.25×10⁻⁴ mm³ by the addition of Al and Cr elements to the WNbMoVTa. The He⁺ irradiation was conducted on the samples to observe surface damage. After irradiation, the XRD patterns were shifted to the left because of defects and dislocations. He⁺ ions were infused under the surface, so they created the lattice expansion. The peak shifting of the WNbMoVTaCr₀.₅Al sample was less than the WNbMoVTa base sample, thanks to less impact. A small amount of fuzz was observed for the base sample. This structure was removed and transformed into a wavy structure with the addition of Cr and Al elements. Also, the deformation hardening was actualized after irradiation. A lower amount of hardening was obtained with the WNbMoVTaCr₀.₅Al sample based on the changing microhardness values. The surface deformation was decreased in the WNbMoVTaCr₀.₅Al sample.

Keywords: refractory high entropy alloy, microhardness, wear resistance, He⁺ irradiation

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Authors: Irina Veselova, Maria Makedonskaya, Olga Eremina, Alexandr Sidorov, Eugene Goodilin, Tatyana Shekhovtsova

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Such catecholamines as dopamine, norepinephrine, and epinephrine are the principal neurotransmitters in the sympathetic nervous system. Catecholamines and their metabolites are considered to be important markers of socially significant diseases such as atherosclerosis, diabetes, coronary heart disease, carcinogenesis, Alzheimer's and Parkinson's diseases. Currently, neurotransmitters can be studied via electrochemical and chromatographic techniques that allow their characterizing and quantification, although these techniques can only provide crude spatial information. Besides, the difficulty of catecholamine determination in biological materials is associated with their low normal concentrations (~ 1 nM) in biomaterials, which may become even one more order lower because of some disorders. In addition, in blood they are rapidly oxidized by monoaminooxidases from thrombocytes and, for this reason, the determination of neurotransmitter metabolism indicators in an organism should be very rapid (15—30 min), especially in critical states. Unfortunately, modern instrumental analysis does not offer a complex solution of this problem: despite its high sensitivity and selectivity, HPLC-MS cannot provide sufficiently rapid analysis, while enzymatic biosensors and immunoassays for the determination of the considered analytes lack sufficient sensitivity and reproducibility. Fluorescent and SERS-sensors remain a compelling technology for approaching the general problem of selective neurotransmitter detection. In recent years, a number of catecholamine sensors have been reported including RNA aptamers, fluorescent ribonucleopeptide (RNP) complexes, and boronic acid based synthetic receptors and the sensor operated in a turn-off mode. In this work we present the fluorescent and SERS turn-on sensor systems based on the bio- or chemorecognizing nanostructured films {chitosan/collagen-Tb/Eu/Cu-nanoparticles-indicator reagents} that provide the selective recognition, visualization, and sensing of the above mentioned catecholamines on the level of nanomolar concentrations in biomaterials (cell cultures, tissue etc.). We have (1) developed optically transparent porous films and gels of chitosan/collagen; (2) ensured functionalization of the surface by molecules-'recognizers' (by impregnation and immobilization of components of the indicator systems: biorecognizing and auxiliary reagents); (3) performed computer simulation for theoretical prediction and interpretation of some properties of the developed materials and obtained analytical signals in biomaterials. We are grateful for the financial support of this research from Russian Foundation for Basic Research (grants no. 15-03-05064 a, and 15-29-01330 ofi_m).

Keywords: biomaterials, fluorescent and SERS-recognition, neurotransmitters, solid-phase turn-on sensor system

Procedia PDF Downloads 406

Authors: Bolysbek Utelbayev, Tasmagambetova Aigerim, Toktasyn Raila, Markayev Yergali, Myrzakhanov Maxat

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Intensive development of secondary processes of destructive processing of crude oil has led to the occurrence of oil refining factories resources of C2-C4 hydrocarbons. Except for oil gases also contain basically C2-C4 hydrocarbon gases where some of the amounts are burned. All these data has induced interest to the study of producing alkylate from hydrocarbons С2-С4 which being as components of motor fuels. The purpose of this work was studying transformation propane-propene, butane-butene fractions at the presence of the ruthenium-chromic support catalyst whereas the carrier is served pillar - structural montmorillonite containing in native bentonite clay. In this work is considered condition and structure of the bentonite clay from the South-Kazakhstan area of the Republic Kazakhstan. For preparation rhodium support catalyst (0,5-1,0 mass. % Rh) was used chloride of rhodium-RhCl3∙3H2O, as a carrier was used modified bentonite clay. For modifying natural clay to pillar structural form were used polyhydroxy complexes of chromium. To aqueous solution of chloride chromium gradually flowed the solution of sodium hydroxide at gradual hashing up to pH~3-4. The concentration of chloride chromium was paid off proceeding from calculation 5-30 mmole Cr3+ per gram clay. Suspension bentonite (~1,0 mass. %) received by intensive washing it in water during 4 h, pH-water extract of clay makes -8-9. The acidity of environment supervised by means of digital pH meter OP-208/1. In order to prevent coagulation of a solution polyhydroxy complexes of chromium, it was slowly added to a suspension of clay. "Reserve of basicity" Cr3+:/OH-allowing to prevent coagulation chloride of rhodium made 1/3. After endurance processed suspensions of clay during 24 h, a deposit was washed by water and condensed. The sample, after separate from a liquid phase, dried at first at the room temperature, and then at 110°C (2h) with the subsequent rise the temperature up to 180°C (4h). After cooling the firm mass was pounded to a powder, it was shifted infractions with the certain sizes of particles. Fractions of particles modifying clay in the further were impregnated with an aqueous solution with rhodium-RhCl3∙3H2O (0,5-1,0 mаss % Rh ). Obtained pillar structural bentonite approaches heat resistance and its porous structure above the 773K. Pillar structural bentonite was used for preparation 1.0% Ru/Carrier (modifying bentonite) support catalysts where is realised alkylation of C2-C4 hydrocarbons. The process of alkylation is carried out at a partial pressure of hydrogen 0.5-1.0MPa. Outcome 2.2.4 three methyl pentane and 2.2.3 trimethylpentane achieved 40%. At alkylation butane-butene mixture outcome of the isooctane is achieved 60%. In this condition of studying the ethene is not undergoing to alkylation.

Keywords: alkylation, butene, pillar structure, ruthenium catalyst

Procedia PDF Downloads 396

Authors: Peter Kus, Anna Ostroverkh, Yurii Yakovlev, Yevheniia Lobko, Roman Fiala, Ivan Khalakhan, Vladimir Matolin

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Hydrogen economy is a concept of low-emission society which harvests most of its energy from renewable sources (e.g., wind and solar) and in case of overproduction, electrochemically turns the excess amount into hydrogen, which serves as an energy carrier. Proton exchange membrane water electrolyzers (PEMWE) are the backbone of this concept. By fast-response electricity to hydrogen conversion, the PEMWEs will not only stabilize the electrical grid but also provide high-purity hydrogen for variety of fuel cell powered devices, ranging from consumer electronics to vehicles. Wider commercialization of PEMWE technology is however hindered by high prices of noble metals which are necessary for catalyzing the redox reactions within the cell. Namely, platinum for hydrogen evolution reaction (HER), running on cathode, and iridium for oxygen evolution reaction (OER) on anode. Possible way of how to lower the loading of Pt and Ir is by using conductive high-surface nanostructures as catalyst supports in conjunction with thin-film catalyst deposition. The presented study discusses unconventional technique of membrane electron assembly (MEA) preparation. Noble metal catalysts (Pt and Ir) were magnetron sputtered in very low loadings onto the surface of porous sublayers (located on gas diffusion layer or directly on membrane), forming so to say localized three-phase boundary. Ultrasonically sprayed corrosion resistant TiC-based sublayer was used as a support material on anode, whereas magnetron sputtered nanostructured etched nitrogenated carbon (CNx) served the same role on cathode. By using this configuration, we were able to significantly decrease the amount of noble metals (to thickness of just tens of nanometers), while keeping the performance comparable to that of average state-of-the-art catalysts. Complex characterization of prepared supported catalysts includes in-cell performance and durability tests, electrochemical impedance spectroscopy (EIS) as well as scanning electron microscopy (SEM) imaging and X-ray photoelectron spectroscopy (XPS) analysis. Our research proves that magnetron sputtering is a suitable method for thin-film deposition of electrocatalysts. Tested set-up of thin-film supported anode and cathode catalysts with combined loading of just 120 ug.cm⁻² yields remarkable values of specific current. Described approach of thin-film low-loading catalyst deposition might be relevant when noble metal reduction is the topmost priority.

Keywords: hydrogen economy, low-loading catalyst, magnetron sputtering, proton exchange membrane water electrolyzer

Procedia PDF Downloads 163

Authors: Akmez Nabeerasool, Michaelis Massaros, Nigel Brown, David Sanderson, David Parocki, Charlotte Thompson, Mike Lodge, Mikael Khan

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The provision of clean and safe drinking water is of paramount importance and is a basic human need. Water scarcity coupled with tightening of regulations and the inability of current treatment technologies to deal with emerging contaminants and Pharmaceuticals and personal care products means that alternative treatment technologies that are viable and cost effective are required in order to meet demand and regulations for clean water supplies. Logistically, the application of water treatment in rural areas presents unique challenges due to the decentralisation of abstraction points arising from low population density and the resultant lack of infrastructure as well as the need to treat water at the site of use. This makes it costly to centralise treatment facilities and hence provide potable water direct to the consumer. Furthermore, across the UK there are segments of the population that rely on a private water supply which means that the owner or user(s) of these supplies, which can serve one household to hundreds, are responsible for the maintenance. The treatment of these private water supply falls on the private owners, and it is imperative that a chemical free technological solution that can operate unattended and does not produce any waste is employed. Arvia’s patented advanced oxidation technology combines the advantages of adsorption and electrochemical regeneration within a single unit; the Organics Destruction Cell (ODC). The ODC uniquely uses a combination of adsorption and electrochemical regeneration to destroy organics. Key to this innovative process is an alternative approach to adsorption. The conventional approach is to use high capacity adsorbents (e.g. activated carbons with high porosities and surface areas) that are excellent adsorbents, but require complex and costly regeneration. Arvia’s technology uses a patent protected adsorbent, Nyex™, which is a non-porous, highly conductive, graphite based adsorbent material that enables it to act as both the adsorbent and as a 3D electrode. Adsorbed organics are oxidised and the surface of the Nyex™ is regenerated in-situ for further adsorption without interruption or replacement. Treated water flows from the bottom of the cell where it can either be re-used or safely discharged. Arvia™ Technology Ltd. has trialled the application of its tertiary water treatment technology in treating reservoir water abstracted near Glasgow, Scotland, with promising results. Several other pilot plants have also been successfully deployed at various locations in the UK showing the suitability and effectiveness of the technology in removing recalcitrant organics (including pharmaceuticals, steroids and hormones), COD and colour.

Keywords: Arvia™ process, adsorption, water treatment, electrochemical oxidation

Procedia PDF Downloads 263

Authors: Z. Karahaliloğlu, E. Yalçın, M. Demirbilek, E.B. Denkbaş

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Critical-sized bone defects caused by trauma, bone diseases, prosthetic implant revision or tumor excision cannot be repaired by physiological regenerative processes. Current orthopedic applications for critical-sized bone defects are to use autologous bone grafts, bone allografts, or synthetic graft materials. However, these strategies are unable to solve completely the problem, and motivate the development of novel effective biological scaffolds for tissue engineering applications and regenerative medicine applications. In particular, scaffolds combined with a variety of bio-agents as fundamental tools emerge to provide the regeneration of damaged bone tissues due to their ability to promote cell growth and function. In this study, a magnetic silk fibroin (SF) hydrogel scaffold was prepared by electrogelation process of the concentrated Bombxy mori silk fibroin (8 %wt) aqueous solution. For enhancement of osteoblast-like cells (SaOS-2) growth and adhesion, basal fibroblast growth factor (bFGF) were conjugated physically to the HSA-coated magnetic nanoparticles (Fe3O4) and magnetic SF e-gel scaffolds were prepared by incorporation of Fe3O4, HSA (human serum albumin)=Fe3O4 and HSA=Fe3O4-bFGF nanoparticles. HSA=Fe3O4, HSA=Fe3O4-bFGF loaded and bare SF e-gels scaffolds were characterized using scanning electron microscopy (SEM.) For cell studies, human osteoblast-like cell line (SaOS-2) was used and an MTT assay was used to assess the cytotoxicity of magnetic silk fibroin e-gel scaffolds and cell density on these surfaces. For the evaluation osteogenic activation, ALP (alkaline phosphatase), the amount of mineralized calcium, total protein and collagen were studied. Fe3O4 nanoparticles were successfully synthesized and bFGF was conjugated to HSA=Fe3O4 nanoparticles with %97.5 of binding yield which has a particle size of 71.52±2.3 nm. Electron microscopy images of the prepared HSA and bFGF incorporated SF e-gel scaffolds showed a 3D porous morphology. In terms of water uptake results, bFGF conjugated HSA=Fe3O4 nanoparticles has the best water absorbability behavior among all groups. In the in-vitro cell culture studies realized using SaOS-2 cell line, the coating of Fe3O4 nanoparticles surface with a protein enhance the cell viability and HSA coating and bFGF conjugation, the both have an inductive effect in the cell proliferation. One of the markers of bone formation and osteoblast differentiation, according to the ALP activity and total protein results, HSA=Fe3O4-bFGF loaded SF e-gels had significantly enhanced ALP activity. Osteoblast cultured HSA=Fe3O4-bFGF loaded SF e-gels deposited more calcium compared with SF e-gel. The proposed magnetic scaffolds seem to be promising for bone tissue regeneration and used in future work for various applications.

Keywords: basic fibroblast growth factor (bFGF), e-gel, iron oxide nanoparticles, silk fibroin

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Authors: Ayoti Banerjee, Meenakshi Banerjee

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The study of metamorphic reaction textures is important in contributing to our understanding of the evolution of metamorphic terranes. Where preserved, they provide information on changes in the P-T conditions during the metamorphic history of the rock, and thus allow us to speculate on the P-T-t evolution of the terrane. Mafic dykes have attracted the attention of petrologists because they act as window to mantle. This rock represents a mafic dyke of doleritic composition. It is fine to medium grained in which clinopyroxene are enclosed by the lath shaped plagioclase grains to form spectacular ophitic texture. At places, sub ophitic texture was also observed. Grains of pyroxene and plagioclase show very less deformation typically plagioclase showing deformed lamella along with plagioclase-clinopyroxene-phyric granoblastic fabric within a groundmass of feldspar microphenocrysts and Fe–Ti oxides. Both normal and reverse zoning were noted in the plagioclase laths. The clinopyroxene grains contain exsolved phases such as orthopyroxene, plagioclase, magnetite, ilmenite along the cleavage traces and the orthopyroxene lamella form granules in the periphery of the clinopyroxene grains. Garnet corona also develops preferentially around plagioclase at the contact of clinopyroxene, ilmenite or magnetite. Tiny quartz and K-fs grains showed symplectic intergrowth with garnet at a few places. The product quartz formed along with garnet rims the coronal garnet and the reacting clinopyroxene. Thin amphibole corona formed along the periphery of deformed plagioclase and clinopyroxene occur as patches over the magmatic minerals. The amphibole coronas cannot be assigned to a late magmatic stage and are interpreted as reactive being restricted to the contact between clinopyroxene and plagioclase, thus postdating the crystallization of both. The amphibole and garnet do not share grain boundary in the entire rock and is thus pointing towards simultaneous crystallization. Olivine is absent. Spectacular myrmekitic growth of orthoclase and quartz rimming the plagioclase is consistent with the potash metasomatic effects that is also found in other rocks of this region. These textural features are consistent with a phase of fluid induced metamorphism (retrogression). But the appearance of coronal garnet and amphibole exclusive of each other reflects the participation if Ti as the prime reason. Presence of Ti as a reactant phase is a must for amphibole forming reactions whereas it is not so in case of garnet forming reactions although the reactants are the same plagioclase and clinopyroxene in both cases. These findings are well validated by petrographical and textural analysis. In order to obtain balanced chemical reactions that explain formation of amphibole and garnet in the mafic dyke rocks a matrix operation technique called Singular Value Decomposition (SVD) was adopted utilizing the measured chemical compositions of the minerals. The computer program C-Space was used for this purpose and the required compositional matrix. Data fed to C-Space was after doing cation-calculation of the oxide percentages obtained from EPMA analysis. The Garnet-Clinopyroxene geothermometer yielded a temperature of 650 degrees Celsius. The Garnet-Clinopyroxene-Plagioclase geobarometer and Al-in amphibole yielded roughly 7.5 kbar pressure.

Keywords: corona, dolerite, geothermometer, metasomatism, metamorphic reaction texture, retrogression

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Authors: M. A. Rahman, A. T. Ohta, H. V. Trinh, J. Hyvl

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Atmospheric pressure and oxygen (O2) concentration are critical life support parameters for human-occupied aerospace vehicles and habitats. Various medical conditions may require medical O2; for example, the American Medical Association has determined that commercial air travel exposes passengers to altitude-related hypoxia and gas expansion. It may cause some passengers to experience significant symptoms and medical complications during the flight, requiring supplemental medical-grade O2 to maintain adequate tissue oxygenation and prevent hypoxemic complications. Although supplemental medical grade O2 is a successful lifesaver for respiratory and cardiac failure, O2-enriched exhaled air can contain more than 95 % O2, increasing the likelihood of a fire. In an aerospace environment, a localized high concentration O2 bubble forms around a patient being treated for hypoxia, increasing the cabin O2 beyond the safe limit. To address this problem, this work describes a medical O2 delivery system that can reduce the O2 concentration from patient-exhaled O2-rich air to safe levels while maintaining the prescribed O2 administration to the patient. The O2 delivery system is designed to be a part of the medical O2 kit. The system uses cationic multimetallic cobalt complexes to reversibly, selectively, and stoichiometrically chemisorb O2 from the exhaled air. An air-release sub-system monitors the exhaled air, and as soon the O2 percentage falls below 21%, the air is released to the room air. The O2-enriched exhaled air is channeled through a layer of porous, thin-film heaters coated with the cobalt complex. The complex absorbs O2, and when saturated, the complex is heated to 100°C using the thin-film heater. Upon heating, the complex desorbs O2 and is once again ready to absorb or remove the excess O2 from exhaled air. The O2 absorption is a sub-second process, and desorption is a multi-second process. While heating at 0.685 °C/sec, the complex desorbs ~90% O2 in 110 sec. These fast reaction times mean that a simultaneous absorb/desorb process in the O2 delivery system will create a continuous absorption of O2. Moreover, the complex can concentrate O2 by a factor of 160 times that in air and desorb over 90% of the O2 at 100°C. Over 12 cycles of thermogravimetry measurement, less than 0.1% decrease in reversibility in O2 uptake was observed. The 1 kg complex can desorb over 20L of O2, so simultaneous O2 desorption by 0.5 kg of complex and absorption by 0.5 kg of complex can potentially continuously remove 9L/min O2 (~90% desorbed at 100°C) from exhaled air. The complex is synthesized and characterized for reversible O2 absorption and efficacy. The complex changes its color from dark brown to light gray after O2 desorption. In addition to thermogravimetric analysis, the O2 absorption/desorption cycle is characterized using optical imaging, showing stable color changes over ten cycles. The complex was also tested at room temperature in a low O2 environment in its O2 desorbed state, and observed to hold the deoxygenated state under these conditions. The results show the feasibility of using the complex for reversible O2 absorption in the proposed fire safe medical O2 delivery system.

Keywords: fire risk, medical oxygen, oxygen removal, reversible absorption

Procedia PDF Downloads 104

Authors: S. Maniruzzaman, N. Ramanujam, Qazi Akhter Rasool, Swapan Kumar Biswas, P. Prasad, Chandrakanta Ojha

Abstract:

Landslide is one of the major natural disasters in South Asian countries. Applying 2D Electrical Resistivity Tomographic Imaging estimation of geometry, thickness, and depth of failure zone of the landslide can be made. Landslide is a pertinent problem in Nilgris plateau next to Himalaya. Nilgris range consists of hard Archean metamorphic rocks. Intense weathering prevailed during the Pre-Cambrian time had deformed the rocks up to 45m depth. The landslides are dominant in the southern and eastern part of plateau of is comparatively smaller than the northern drainage basins, as it has low density of drainage; coarse texture permitted the more of infiltration of rainwater, whereas in the northern part of the plateau entombed with high density of drainage pattern and fine texture with less infiltration than run off, and low to the susceptible to landslide. To get comprehensive information about the landslide zone 2D Electrical Resistivity Tomographic imaging study with CRM 500 Resistivity meter are used in Coonoor– Mettupalyam sector of Nilgiris plateau. To calculate Factor of Safety the infinite slope model of Brunsden and Prior is used. Factor of Safety can be expressed (FS) as the ratio of resisting forces to disturbing forces. If FS < 1 disturbing forces are larger than resisting forces and failure may occur. The geotechnical parameters of soil samples are calculated on the basis upon the apparent resistivity values for litho units of measured from 2D ERT image of the landslide zone. Relationship between friction angles for various soil properties is established by simple regression analysis from apparent resistivity data. Increase of water content in slide zone reduces the effectiveness of the shearing resistance and increase the sliding movement. Time-lapse resistivity changes to slope failure is determined through geophysical Factor of Safety which depends on resistivity and site topography. This ERT technique infers soil property at variable depths in wider areas. This approach to retrieve the soil property and overcomes the limit of the point of information provided by rain gauges and porous probes. Monitoring of slope stability without altering soil structure through the ERT technique is non-invasive with low cost. In landslide prone area an automated Electrical Resistivity Tomographic Imaging system should be installed permanently with electrode networks to monitor the hydraulic precursors to monitor landslide movement.

Keywords: 2D ERT, landslide, safety factor, slope stability

Procedia PDF Downloads 317

Authors: Celine Bonnaud, Isabelle Billard, Nicolas Papaiconomou, Eric Chainet

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Thanks to their high magnetization and low mass, permanent magnets (NdFeB and SmCo) have quickly became essential for new energies (wind turbines, electrical vehicles…). They contain large quantities of neodymium, samarium and dysprosium, that have been recently classified as critical elements and that therefore need to be recycled. Electrochemical processes including electrodissolution followed by electrodeposition are an elegant and environmentally friendly solution for the recycling of such lanthanides contained in permanent magnets. However, electrochemistry of the lanthanides is a real challenge as their standard potentials are highly negative (around -2.5V vs ENH). Consequently, non-aqueous solvents are required. Ionic liquids (IL) are novel electrolytes exhibiting physico-chemical properties that fulfill many requirements of the sustainable chemistry principles, such as extremely low volatility and non-flammability. Furthermore, their chemical and electrochemical properties (solvation of metallic ions, large electrochemical windows, etc.) render them very attractive media to implement alternative and sustainable processes in view of integrated processes. All experiments that will be presented were carried out using butyl-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide. Linear sweep, cyclic voltammetry and potentiostatic electrochemical techniques were used. The reliability of electrochemical experiments, performed without glove box, for the classic three electrodes cell used in this study has been assessed. Deposits were obtained by chronoamperometry and were characterized by scanning electron microscopy and energy-dispersive X-ray spectroscopy. The IL cathodic behavior under different constraints (argon, nitrogen, oxygen atmosphere or water content) and using several electrode materials (Pt, Au, GC) shows that with argon gas flow and gold as a working electrode, the cathodic potential can reach the maximum value of -3V vs Fc+/Fc; thus allowing a possible reduction of lanthanides. On a gold working electrode, the reduction potential of samarium and neodymium was found to be -1.8V vs Fc+/Fc while that of dysprosium was -2.1V vs Fc+/Fc. The individual deposits obtained were found to be porous and presented some significant amounts of C, N, F, S and O atoms. Selective deposition of neodymium in presence of dysprosium was also studied and will be discussed. Next, metallic Sm, Nd and Dy electrodes were used in replacement of Au, which induced changes in the reduction potential values and the deposit structures of lanthanides. The individual corrosion potentials were also measured in order to determine the parameters influencing the electrodissolution of these metals. Finally, a full recycling process was investigated. Electrodissolution of a real permanent magnet sample was monitored kinetically. Then, the sequential electrodeposition of all lanthanides contained in the IL was investigated. Yields, quality of the deposits and consumption of chemicals will be discussed in depth, in view of the industrial feasibility of this process for real permanent magnets recycling.

Keywords: electrodeposition, electrodissolution, ionic liquids, lanthanides, rcycling

Procedia PDF Downloads 274

Authors: M. Shopska, D. Paneva, G. Kadinov, Z. Cherkezova-Zheleva, I. Mitov

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The iron containing materials are used as catalysts in different processes. The chemical methods of their synthesis use toxic and expensive chemicals; sophisticated devices; energy consumption processes that raise their cost. Besides, dangerous waste products are formed. At present time such syntheses are out of date and wasteless technologies are indispensable. The bioinspired technologies are consistent with the ecological requirements. Different microorganisms participate in the biomineralization of the iron and some phytochemicals are involved, too. The methods for biogenic production of iron containing materials are clean, simple, nontoxic, realized at ambient temperature and pressure, cheaper. The biogenic iron materials embrace different iron compounds. Due to their origin these substances are nanosized, amorphous or poorly crystalline, porous and have number of useful properties like SPM, high magnetism, low toxicity, biocompatibility, absorption of microwaves, high surface area/volume ratio, active sites on the surface with unusual coordination that distinguish them from the bulk materials. The biogenic iron materials are applied in the heterogeneous catalysis in different roles - precursor, active component, support, immobilizer. The application of biogenic iron oxide materials gives rise to increased catalytic activity in comparison with those of abiotic origin. In our study we investigated the catalytic behavior of biomasses obtained by cultivation of Leptothrix bacteria in three nutrition media – Adler, Fedorov, and Lieske. The biomass composition was studied by Moessbauer spectroscopy and transmission IRS. Catalytic experiments on CO oxidation were carried out using in situ DRIFTS. Our results showed that: i) the used biomasses contain α-FeOOH, γ-FeOOH, γ-Fe2O3 in different ratios; ii) the biomass formed in Adler medium contains γ-FeOOH as main phase. The CO conversion was about 50% as evaluated by decreased integrated band intensity in the gas mixture spectra during the reaction. The main phase in the spent sample is γ-Fe2O3; iii) the biomass formed in Lieske medium contains α-FeOOH. The CO conversion was about 20%. The main phase in the spent sample is α-Fe2O3; iv) the biomass formed in Fedorov medium contains γ-Fe2O3 as main phase. CO conversion in the test reaction was about 19%. The results showed that the catalytic activity up to 200°C resulted predominantly from α-FeOOH and γ-FeOOH. The catalytic activity at temperatures higher than 200°C was due to the formation of γ-Fe2O3. The oxyhydroxides, which are the principal compounds in the biomass, have low catalytic activity in the used reaction; the maghemite has relatively good catalytic activity; the hematite has activity commensurate with that of the oxyhydroxides. Moreover it can be affirmed that catalytic activity is inherent in maghemite, which is obtained by transformation of the biogenic lepidocrocite, i.e. it has biogenic precursor.

Keywords: nanosized biogenic iron compounds, catalytic behavior in reaction of CO oxidation, in situ DRIFTS, Moessbauer spectroscopy

Procedia PDF Downloads 369

Authors: H. Arceo, S. Rincon, C. Ben-Youssef, J. Rivera, A. Zepeda

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Biodiesel has emerged as a material with great potential as a renewable energy replacement to current petroleum-based diesel. Recently, biodiesel production is focused on the development of more efficient, sustainable process with lower costs of production. In this sense, a “green” approach to biodiesel production has stimulated the use of sustainable heterogeneous acid catalysts, that are better alternatives to conventional processes because of their simplicity and the simultaneous promotion of esterification and transesterification reactions from low-grade, highly-acidic and water containing oils without the formation of soap. The focus of this methodology is the development of new heterogeneous catalysts that under ordinary reaction conditions could reach yields similar to homogeneous catalysis. In recent years, metal organic frameworks (MOF) have attracted much interest for their potential as heterogeneous acid catalysts. They are crystalline porous solids formed by association of transition metal ions or metal–oxo clusters and polydentate organic ligands. This hybridization confers MOFs unique features such as high thermal stability, larger pore size, high specific area, high selectivity and recycling potential. Thus, MOF application could be a way to improve the biodiesel production processes. In this work, we evaluated the catalytic activity of MOF [(4,4-bipyridine)2(O₂CCH₃)2Zn]n (MOF Zn-I) for the synthesis of biodiesel from canola oil. The reaction conditions were optimized using the response surface methodology with a compound design central with 24. The variables studied were: Reaction temperature, amount of catalyst, molar ratio oil: MetOH and reaction time. The preparation MOF Zn-I was performed by mixing 5 mmol 4´4 dipyridine dissolved in 25 mL methanol with 10 mmol Zn(O₂CCH₃)₂ ∙ 2H₂O in 25 mL water. The crystals were obtained by slow evaporation of the solvents at 60°C for 18 h. The prepared catalyst was characterized using X-ray diffraction (XRD) and Fourier transform infrared spectrometer (FT-IR). The prepared catalyst was characterized using X-ray diffraction (XRD) and Fourier transform infrared spectrometer (FT-IR). Experiments were performed using commercially available canola oil in ace pressure tube under continuous stirring. The reaction was filtered and vacuum distilled to remove the catalyst and excess alcohol, after which it was centrifuged to separate the obtained biodiesel and glycerol. 1H NMR was used to calculate the process yield. GC-MS was used to quantify the fatty acid methyl ester (FAME). The results of this study show that the acid catalyst MOF Zn-I could be used as catalyst for biodiesel production through heterogeneous transesterification of canola oil with FAME yield 82 %. The optimum operating condition for the catalytic reaction were of 142°C, 0.5% catalyst/oil weight ratio, 1:30 oil:MeOH molar ratio and 5 h reaction time.

Keywords: fatty acid methyl ester, heterogeneous acid catalyst, metal organic framework, transesterification

Procedia PDF Downloads 279

Authors: Kanchan Maji, Debasmita Pani, Sudip Dasgupta

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Calcium phosphate cement (CPC) due to its high bioactivity and optimum bioresorbability shows excellent bone regeneration capability. Despite it has limited applications as bone implant due to its macro-porous microstructure causing its poor mechanical strength. The reinforcement of apatitic CPCs with biocompatible fibre glass phase is an attractive area of research to improve its mechanical strength. Here we study the setting behaviour of Si-doped and un-doped alpha tri-calcium phosphate (α-TCP) based CPC and its reinforcement with the addition of E-glass fibre. Alpha tri-calcium phosphate powders were prepared by solid state sintering of CaCO3, CaHPO4 and tetra ethyl ortho silicate (TEOS) was used as silicon source to synthesise Si doped α-TCP powders. Alpha tri-calcium phosphate based CPC hydrolyzes to form hydroxyapatite (HA) crystals having excellent osteoconductivity and bone-replacement capability thus self-hardens through the entanglement of HA crystals. Setting time, phase composition, hydrolysis conversion rate, microstructure, and diametral tensile strength (DTS) of un-doped CPC and Si-doped CPC were studied and compared. Both initial and final setting time of the developed cement was delayed because of Si addition. Crystalline phases of HA (JCPDS 9-432), α-TCP (JCPDS 29-359) and β-TCP (JCPDS 9-169) were detected in the X-ray diffraction (XRD) pattern after immersion of CPC in simulated body fluid (SBF) for 0 hours to 10 days. The intensities of the α-TCP peaks of (201) and (161) at 2θ of 22.2°and 24.1° decreased when the time of immersion of CPC in SBF increased from 0 hours to 10 days, due to its transformation into HA. As Si incorporation in the crystal lattice stabilised the TCP phase, Si doped CPC showed a little slower rate of conversion into HA phase as compared to un-doped CPC. The SEM image of the microstructure of hardened CPC showed lower grain size of HA in un-doped CPC because of premature setting and faster hydrolysis of un-doped CPC in SBF as compared that in Si-doped CPC. Premature setting caused generation of micro and macro porosity in un-doped CPC structure which resulted in its lower mechanical strength as compared to that in Si-doped CPC. This lower porosity and greater compactness in the microstructure attributes to greater DTS values observed in Si-doped CPC. E-glass fibres of the average diameter of 12 μm were cut into approximately 1 mm in length and immersed in SBF to deposit carbonated apatite on its surface. This was performed to promote HA crystal growth and entanglement along the fibre surface to promote stronger interface between dispersed E-glass fibre and CPC matrix. It was found that addition of 10 wt% of E-glass fibre into Si-doped α-TCP increased the average DTS of CPC from 8 MPa to 15 MPa as the fibres could resist the propagation of crack by deflecting the crack tip. Our study shows that biocompatible E-glass fibre in optimum proportion in CPC matrix can enhance the mechanical strength of CPC without affecting its bioactivity.

Keywords: Calcium phosphate cement, biocompatibility, e-glass fibre, diametral tensile strength

Procedia PDF Downloads 346