World Academy of Science, Engineering and Technology

Authors: El Montassir Dahmane, Nadia Eladlani, Aziz Ouahrouch, Mohammed Rhazi, Moha Taourirte

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The present study was aimed to approximate the optimal conditions to chromium recovery from wastewater by nanoparticles and whiskers of chitosan. Chitosan with an average molecular weight of 63 kDa and a 96% deacetylation degree was prepared according to our previous study. Chromium recovery is influenced by different parameters. In our search, we determined the appropriate range of pH to form chitosan–Cr(III), nanoparticles Cr(III), and whiskers– Cr(III) complex. We studied also the influence of chromium concentration and the nature of chitosan-based materials on the complexation process. Our main aim is to approximate the optimal conditions to remove chromium(III) from the tanning bath, recuperated from tannery wastewater of Marrakech in Morocco. A Perkin Elmer optima 2000 Inductively Coupled Plasma- Optical Emission Spectrometer (ICP-OES), was used to determine the quantity of chromium persistent in tannery wastewater after complexation phenomenon. To the best of our knowledge, this is the first report interested in the optimal conditions for chromium recovery from wastewater by nanoparticles and whiskers of chitosan. From our research, we found that in chromium solution, the appropriate range of pH to form complex is between 5.6 and 6.7. Also, the complexation of Cr(III) is depending on the nature of complexing ligand and chromium concentration. The obtained results reveal that nanoparticles present an excellent adsorption capacity regardless of chromium concentration. In addition, after a critical chromium concentration (250 mg/l), our ligand becomes saturated, that requires an increase of ligand mass for increasing chromium concentration in order to have a better adsorption capacity. Hence, in the same conditions, we used chitosan, its nanoparticles, whiskers, and chitosan based films to remove Cr(III) from tannery wastewater. The pH of this effluent was around 6, and its chromium concentration was 300 mg/l. The results expose that the sequence of complexing ligand in the effluent is the same in chromium solution, determined via our previous study. However, the adsorbed quantity is less due to the presence of other metallic ions in tannery wastewater. We conclude that the best complexing ligand-based chitosan is chitosan nanoaprticles whether it’s in chromium solution or in tannery wastewater. Nanoparticles are the best complexing ligand after 24 h of contact nanoparticles can remove 70% of chromium from this tannery wastewater.

Keywords: nanoparticles, whiskers, chitosan, chromium

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Authors: Behnaz Baghaei, Mikael Skrifvars

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Sustainability is today a trend that is seen everywhere, with no exception for the textiles 31 industry. However, there is a rather significant downside regarding how the textile industry currently operates, namely the huge amount of end-of-life textiles coming along with it. Approximately 73% of the 53 million tonnes of fibres used annually for textile production is landfilled or incinerated, while only 12% is recycled as secondary products. Mechanical recycling of end-of-life textile fabrics into yarns and fabrics was before very common, but due to the low costs for virgin man-made fibres, the current textile material composition diversity, the fibre material quality variations and the high recycling costs this route is not feasible. Another way to decrease the ever-growing pile of textile waste is to repurpose the textile. If a feasible methodology can be found to reuse end-of life textiles as secondary market products including a manufacturing process that requires rather low investment costs, then this can be highly beneficial to counteract the increasing textile waste volumes. In structural composites, glass fibre textiles are used as reinforcements, but today there is a growing interest in biocomposites where the reinforcement and/or the resin are from a biomass resource. All-cellulose composites (ACCs) are monocomponent or single polymer composites, and they are entirely made from cellulose, ideally leading to a homogeneous biocomposite. Since the matrix and the reinforcement are both made from cellulose, and therefore chemically identical, they are fully compatible with each other which allow efficient stress transfer and adhesion at their interface. Apart from improving the mechanical performance of the final products, the recycling of the composites will be facilitated. This paper reports the recycling of end-of-life cellulose containing textiles by fabrication of all-cellulose composites (ACCs). Composite laminates were prepared by using an ionic liquid (IL) in a hot process, involving a partial dissolving of the cellulose fibres. Discharged denim fabrics were used as the reinforcement while dissolved cellulose from two different cellulose resources was used as the matrix phase. Virgin cotton staple fibres and recovered cotton from polyester/cotton (polycotton) waste fabrics were used to form the matrix phase. The process comprises the dissolving 6 wt.% cellulose solution in the ionic liquid 1-butyl-3-methyl imidazolium acetate ([BMIM][Ac]), this solution acted as a precursor for the matrix component. The denim fabrics were embedded in the cellulose/IL solution after which laminates were formed, which also involved removal of the IL by washing. The effect of reuse of the recovered IL was also investigated. The mechanical properties of the obtained ACCs were determined regarding tensile, impact and flexural properties. Mechanical testing revealed that there are no clear differences between the values measured for mechanical strength and modulus of the manufactured ACCs from denim/cotton-fresh IL, denim/recovered cotton-fresh IL and denim/cotton-recycled IL. This could be due to the low weight fraction of the cellulose matrix in the final ACC laminates and presumably the denim as cellulose reinforcement strongly influences and dominates the mechanical properties. Fabricated ACC composite laminates were further characterized regarding scanning electron microscopy.

Keywords: all-cellulose composites, denim fabrics, ionic liquid, mechanical properties

Procedia PDF Downloads 100

Authors: Ghada Ben Hamad, Zohir Younsi, Fabien Salaun, Hassane Naji, Noureddine Lebaz

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The graphene oxide (GO) material has attracted much attention for solar energy applications. This paper reports the synthesis and characterization of partially oxidized graphite oxide (GTO). GTO was obtained by modified Hummers method, which is based on the chemical oxidation of natural graphite. Several samples were prepared with different oxidation degree by an adjustment of the oxidizing agent’s amount. The effect of the oxidation degree on the chemical structure and on the morphology of GTO was determined by using Fourier transform infrared (FT-IR) spectroscopy, Energy Dispersive X-ray Spectroscopy (EDS), and scanning electronic microscope (SEM). The thermal stability of GTO was evaluated by using thermogravimetric analyzer (TGA) in Nitrogen atmosphere. The results indicate high degree oxidation of graphite oxide for each sample, proving that the process is efficient. The GTO synthesized by modified Hummers method shows promising characteristics. Graphene oxide (GO) obtained by exfoliation of GTO are recognized as a good candidate for thermal energy storage, and it will be used as solid shell material in the encapsulation of phase change materials (PCM).

Keywords: modified hummers method, graphite oxide, oxidation degree, solar energy storage

Procedia PDF Downloads 106

Authors: Zahrah Thamer Althagafi, Mohamed I. Awad

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A simple method for the fabrication of Au (111)-like electrode via controlled reductive desorption of a pre-adsorbed cysteine monolayer onto polycrystalline gold (poly-Au) electrode is introduced. Then, the voltammetric behaviour of dopamine (DA) and ascorbic acid (AA) on the thus modified electrode is investigated. Electrochemical characterization of the modified electrode is achieved using cyclic voltammetry and square wave voltammetry. For the binary mixture of DA and AA, the results showed that Au (111)-like electrode exhibits excellent electrocatalytic activity towards the oxidation of DA and AA. This allows highly selective and simultaneous determination of DA and AA. The effect of various experimental parameters on the voltammetric responses of DA and AA was investigated. The enrichment of the Au (111) facet of the poly-Au electrode is thought to be behind the electrocatalytic activity.

Keywords: gold electrode, electroanalysis, electrocatalysis, monolayers, self-assembly, cysteine, dopamine, ascorbic acid

Procedia PDF Downloads 183

Authors: Matthew Korey, Jeffrey Youngblood, John Howarter

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Background and Significance: Tannic acid (TA) is a bio-based high molecular weight organic, aromatic molecule that has been found to increase thermal stability and flame retardancy of many polymer matrices when used as an additive. Although it is biologically sourced, TA is a pollutant in industrial wastewater streams, and there is a desire to find applications in which to downcycle this molecule after extraction from these streams. Additionally, epoxy thermosets have revolutionized many industries, but are too flammable to be used in many applications without additives which augment their flame retardancy (FR). Many flame retardants used in epoxy thermosets are synthesized from petroleum-based monomers leading to significant environmental impacts on the industrial scale. Many of these compounds also have significant impacts on human health. Various bio-based modifiers have been developed to improve the FR of the epoxy resin; however, increasing FR of the system without tradeoffs with other properties has proven challenging, especially for TA. Methodologies: In this work, TA was incorporated into the thermoset by use of solvent-exchange using methyl ethyl ketone, a co-solvent for TA, and epoxy resin. Samples were then characterized optically (UV-vis spectroscopy and optical microscopy), thermally (thermogravimetric analysis and differential scanning calorimetry), and for their flame retardancy (mass loss calorimetry). Major Findings: Compared to control samples, all samples were found to have increased thermal stability. Further, the addition of tannic acid to the polymer matrix by the use of solvent greatly increased the compatibility of the additive in epoxy thermosets. By using solvent-exchange, the highest loading level of TA found in literature was achieved in this work (40 wt%). Conclusions: The use of solvent-exchange shows promises for circumventing the limitations of TA in epoxy.

Keywords: sustainable, flame retardant, epoxy, tannic acid

Procedia PDF Downloads 113

Authors: Adrian Ionut Nicoara, Denisa Ionela Ene, Alina Maria Holban, Cristina Busuioc

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At present, the development of materials with biomedical applications is a domain of interest that will produce a full series of benefits in engineering and medicine. In this sense, it is required to use a natural material, and this paper is focused on the development of a composite material based on bacterial cellulose – hydroxyapatite and silver nanoparticles with applications in hard tissue. Bacterial cellulose own features like biocompatibility, non-toxicity character and flexibility. Moreover, the bacterial cellulose can be conjugated with different forms of active silver to possess antimicrobial activity. Hydroxyapatite is well known that can mimic at a significant level the activity of the initial bone. The material was synthesized by using an ultrasound probe and finally characterized by several methods. Thereby, the morphological properties were analyzed by using Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). Because the synthesized material has medical application in restore the tissue and to fight against microbial invasion, the samples were tested from the biological point of view by evaluating the biodegradability in phosphate-buffered saline (PBS) and simulated body fluid (SBF) and moreover the antimicrobial effect was performed on Gram-positive bacterium Staphylococcus aureus, Gram-negative bacterium Escherichia coli, and fungi Candida albicans. The results reveal that the obtained material has specific characteristics for bone regeneration.

Keywords: bacterial cellulose, biomaterials, hydroxyapatite, scaffolds materials

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Authors: Ahmed El-Fiqi, Hae-Won Kim

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Incorporation of therapeutic elements such as Sr, Cu and Co into bioglass structure and their release as ions is considered as one of the promising approaches to enhance cellular responses, e.g., osteogenesis and angiogenesis. Here, cobalt as angiogenesis promoter has been incorporated (at 0, 1 and 4 mol%) into sol-gel derived calcium silicate mesoporous bioglass nanoparticles. The composition and structure of cobalt-free (CFN) and cobalt-doped (CDN) mesoporous bioglass nanoparticles have been analyzed by X-ray fluorescence (XRF), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Fourier-Transform Infra-red spectroscopy (FT-IR). The physicochemical properties of CFN and CDN have been investigated using high-resolution transmission electron microscopy (HR-TEM), Selected area electron diffraction (SAED), and Energy-dispersive X-ray (EDX). Furthermore, the textural properties, including specific surface area, pore-volume, and pore size, have been analyzed from N²⁻sorption analyses. Surface charges of CFN and CDN were also determined from surface zeta potential measurements. The release of ions, including Co²⁺, Ca²⁺, and SiO₄⁴⁻ has been analyzed using inductively coupled plasma atomic emission spectrometry (ICP-AES). Loading and release of diclofenac as an anti-inflammatory drug model were explored in vitro using Ultraviolet-visible spectroscopy (UV-Vis). XRD results ensured the amorphous state of CFN and CDN whereas, XRF further confirmed that their chemical compositions are very close to the designed compositions. HR-TEM analyses unveiled nanoparticles with spherical morphologies, highly mesoporous textures, and sizes in the range of 90 - 100 nm. Moreover, N²⁻ sorption analyses revealed that the nanoparticles have pores with sizes of 3.2 - 2.6 nm, pore volumes of 0.41 - 0.35 cc/g and highly surface areas in the range of 716 - 830 m²/g. High-resolution XPS analysis of Co 2p core level provided structural information about Co atomic environment and it confirmed the electronic state of Co in the glass matrix. ICP-AES analysis showed the release of therapeutic doses of Co²⁺ ions from 4% CDN up to 100 ppm within 14 days. Finally, diclofenac loading and release have ensured the drug/ion co-delivery capability of 4% CDN.

Keywords: mesoporous bioactive glass, nanoparticles, cobalt ions, release

Procedia PDF Downloads 93

Authors: C. Busuioc, I. Stancu, A. Nicoara, A. Zamfirescu, A. Evanghelidis

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The field of tissue engineering has expanded its potential due to the use of composite biomaterials belonging to increasingly complex systems, leading to bone substitutes with properties that are continuously improving to meet the patient's specific needs. Furthermore, the development of biomaterials based on ceramic and polymeric phases is an unlimited resource for future scientific research, with the final aim of restoring the original tissue functionality. Thus, in the first stage, composite scaffolds based on polycaprolactone (PCL) or polylactic acid (PLA) and inorganic powders were prepared by employing the electrospinning technique. The targeted powders were: commercial and laboratory synthesized hydroxyapatite (HAp), as well as barium titanate (BT). By controlling the concentration of the powder within the precursor solution, together with the processing parameters, different types of three-dimensional architectures were achieved. In the second stage, both the mineral powders and hybrid composites were investigated in terms of composition, crystalline structure, and microstructure so that to demonstrate their suitability for tissue engineering applications. Regarding the scaffolds, these were proven to be homogeneous on large areas and loaded with mineral particles in different proportions. The biological assays demonstrated that the addition of inorganic powders leads to modified responses in the presence of simulated body fluid (SBF) or cell cultures. Through SBF immersion, the biodegradability coupled with bioactivity were highlighted, with fiber fragmentation and surface degradation, as well as apatite layer formation within the testing period. Moreover, the final composites represent supports accepted by the cells, favoring implant integration. Concluding, the purposed fibrous materials based on bioresorbable polymers and mineral powders, produced by the electrospinning technique, represent candidates with considerable potential in the field of tissue engineering. Future improvements can be attained by optimizing the synthesis process or by simultaneous incorporation of multiple inorganic phases with well-defined biological action in order to fabricate multifunctional composites.

Keywords: barium titanate, electrospinning, fibre networks, hydroxyapatite, smart scaffolds

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Authors: Bilge Yaman Islak, Erhan Ayas

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The densification behavior of TiB₂ – Ti₃SiC₂ composites is investigated for temperatures in the range of 1200°C to 1400°C, for the pressure of 40 and 50MPa, and for holding time between 15-30 min by spark plasma sintering (SPS) technique. Ti, Si, TiC and 5 wt.% TiB₂ were used to synthesize TiB₂ – Ti₃SiC₂ composites and the effect of different sintering parameters on the densification and phase evolution of these composites were investigated. The bulk densities were determined by using the Archimedes method. The polished and fractured surfaces of the samples were examined using a scanning electron microscope equipped with an energy dispersive spectroscopy (EDS). The phase analyses were accomplished by using the X-Ray diffractometer. Sintering temperature and holding time are found to play a dominant role in the phase development of composites. TiₓCᵧ and TiSi₂ secondary phases were found in 5 wt.%TiB₂ – Ti₃SiC₂ composites densified at 1200°C and 1400°C under the pressure of 40 MPa, due to decomposition of Ti₃SiC₂. The results indicated that 5 wt.%TiB₂ – Ti₃SiC₂ composites were densified into the dense parts with a relative density of 98.77% by sintering at 1300 °C, for 15 min, under a pressure of 50 MPa via SPS without the formation of any other ancillary phase. This work was funded and supported by Scientific Research Projects Commission of Eskisehir Osmangazi University with the Project Number 201915C103 (2019-2517).

Keywords: densification, phase evolution, sintering, TiB₂ – Ti₃SiC₂ composites

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Authors: Anasheh Maridiroosi, Ali Reza Mahjoub, Hanieh Fakhri

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Heteropoly acid nanoparticles anchored on graphene oxide based on UiO-66 were synthesized via in-situ growth hydrothermal method and tested for photodegradation of a tetracycline as critical pollutant. Results showed that presence of graphene oxide and UiO-66 with high specific surface area, great electron mobility and various functional groups make an excellent support for heteropoly acid and improve photocatalytic efficiency up to 95% for tetracycline. Furthermore, total organic carbon (TOC) analysis verified 79% mineralization of this pollutant under optimum condition.

Keywords: heteropoly acid, graphene oxide, MOF, tetracycline

Procedia PDF Downloads 112

Authors: Ambrish Singh

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The corrosion inhibition performance of pyran derivatives (AP) on mild steel in 15% HCl was investigated by electrochemical impedance spectroscopy (EIS), potentiodynamic polarization, weight loss, contact angle, and scanning electron microscopy (SEM) measurements, DFT and molecular dynamic simulation. The adsorption of APs on the surface of mild steel obeyed Langmuir isotherm. The potentiodynamic polarization study confirmed that inhibitors are mixed type with cathodic predominance. Molecular dynamic simulation was applied to search for the most stable configuration and adsorption energies for the interaction of the inhibitors with Fe (110) surface. The theoretical data obtained are, in most cases, in agreement with experimental results.

Keywords: acidizing inhibitor, pyran derivatives, DFT, molecular simulation, mild steel, EIS

Procedia PDF Downloads 176

Authors: Sarra Boughaba

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The α-aminophosphonates have received considerable attention in organic and medicinal chemistry because of their structural resemblance with α-amino acids. They are used as antitumor agents, anti-inflammatory and antibiotics. As a result, a number of procedures have been developed for their synthesis. However, many of these methods suffer from some disadvantages such as long reaction times, environmental pollution caused by utilization of organic solvents, and expensive catalyst. On the other hand, thiazole components, particularly 2-aminothiazole is an important class of heterocyclic compounds. They appear in the structure of natural products and biologically actives compounds, thiamine (vitamin-B), and some antibiotics drugs (penicillin, micrococcin). In the past few years, heteropolyacids have received great attention as environmentally benign catalysts for organic synthetic processes, they possess unique physicochemical properties, such as super-acidity, high thermal and chemical stability, ability to accept and release electrons and high proton mobility, and the possibility of varying their acidity and oxidizing potential. In this study, an efficient and eco-friendly process has been developed for the synthesis of α-aminophosphonates containing aminothiazole moiety via Kabachnik-Field reaction catalyzed by H₆P₂W₁₈O₆₂.14H₂O as reusable catalyst, by condensation of aromatic aldehydes, 2-aminothiazole and triethylphosphite under free conditions. The X-ray crystallographic data of obtained compounds were provided. The main advantages of our protocol include the absence of solvent in the reaction, easy work-up, short reaction time, atom-economy and reusability of catalyst without significant loss of its activity.

Keywords: aminophosphonates, green synthesis, H₆P₂W₁₈O₆₂.14H₂O catalyst, x-ray study

Procedia PDF Downloads 94

Authors: A. Driouiche, S. Mohareb, A. Hadfi

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In Morocco’s Agadir region, the reuse of treated wastewater for irrigation of green spaces has faced the problem of scaling of the pipes of these waters. This research paper aims at studying the phenomenon of scaling caused by the treated wastewater from the Mzar sewage treatment plant. These waters are used in the irrigation of golf turf for the Ocean Golf Resort. Ocean Golf, located about 10 km from the center of the city of Agadir, is one of the most important recreation centers in Morocco. The course is a Belt Collins design with 27 holes, and is quite open with deep challenging bunkers. The formation of solid deposits in the irrigation systems has led to a decrease in their lifetime and, consequently, a loss of load and performance. Thus, the sprinklers used in golf turf irrigation are plugged in the first weeks of operation. To study this phenomenon, the wastewater used for the irrigation of the golf turf was taken and analyzed at various points, and also samples of scale formed in the circuits of the passage of these waters were characterized. This characterization of the scale was performed by X-ray fluorescence spectrometry, X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential thermal analysis (DTA), and scanning electron microscopy (SEM). The results of the physicochemical analysis of the waters show that they are full of bicarbonates (653 mg/L), chloride (478 mg/L), nitrate (412 mg/L), sodium (425 mg/L) and calcium (199mg/L). Their pH is slightly alkaline. The analysis of the scale reveals that it is rich in calcium and phosphorus. It is formed of calcium carbonate (CaCO₃), silica (SiO₂), calcium silicate (Ca₂SiO₄), hydroxylapatite (Ca₁₀P₆O₂₆), calcium carbonate and phosphate (Ca₁₀(PO₄) 6CO₃) and silicate calcium and magnesium (Ca₅MgSi₃O₁₂).

Keywords: Agadir, irrigation, scaling water, wastewater

Procedia PDF Downloads 105

Authors: V. Golubeva, O. Vakhnina, I. Konopkina, N. Gerasimova, N. Taturina, K. Zhogova

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To improve chemical current sources, the ion-conducting electrolytes based on Li halides (LiCl-KCl, LiCl-LiBr-KBr, LiCl-LiBr-LiF) are developed. It is necessary to have chemical analytical methods for determination of halides to control the electrolytes technology. The methods of classical analytical chemistry are of interest, as they are characterized by high accuracy. Using these methods is a difficult task because halides have similar chemical properties. The objective of this work is to develop a titrimetric method for determining the content of bromides, chlorides, and fluorides in their joint presence in an ion-conducting electrolyte. In accordance with the developed method of analysis to determine fluorides, electrolyte sample is dissolved in diluted HCl acid; fluorides are titrated by La(NO₃)₃ solution with potentiometric indication of equivalence point, fluoride ion-selective electrode is used as sensor. Chlorides and bromides do not form a hardly soluble compound with La and do not interfere in result of analysis. To determine the bromides, the sample is dissolved in a diluted H₂SO₄ acid. The bromides are oxidized with a solution of KIO₃ to Br₂, which is removed from the reaction zone by boiling. Excess of KIO₃ is titrated by iodometric method. The content of bromides is calculated from the amount of KIO₃ spent on Br₂ oxidation. Chlorides and fluorides are not oxidized by KIO₃ and do not interfere in result of analysis. To determine the chlorides, the sample is dissolved in diluted HNO₃ acid and the total content of chlorides and bromides is determined by method of visual mercurometric titration with diphenylcarbazone indicator. Fluorides do not form a hardly soluble compound with mercury and do not interfere with determination. The content of chlorides is calculated taking into account the content of bromides in the sample of electrolyte. The validation of the developed analytical method was evaluated by analyzing internal reference material with known chlorides, bromides and fluorides content. The analytical method allows to determine chlorides, bromides and fluorides in case of their joint presence in ion-conducting electrolyte within the range and with relative total error (δ): for bromides from 60.0 to 65.0 %, δ = ± 2.1 %; for chlorides from 8.0 to 15.0 %, δ = ± 3.6 %; for fluorides from 5.0 to 8.0%, ± 1.5% . The analytical method allows to analyze electrolytes and mixtures that contain chlorides, bromides, fluorides of alkali metals and their mixtures (K, Na, Li).

Keywords: bromides, chlorides, fluorides, ion-conducting electrolyte

Procedia PDF Downloads 111

Authors: Erfan Asghari Fesaghandis, Reza Ghaffari Adli, Abbas Kianvash, Hossein Aghajani, Homa Homaie

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NiTi alloys possess magnificent superelastic, shape memory, high strength and biocompatible properties. For improving mechanical properties, foremost, superelasticity behavior, heat treatment process is carried out. In this paper, two different heat treatment methods were undertaken: (1) solid solution, and (2) aging. The effect of each treatment in a constant time is investigated. Five samples were prepared to study the structure and optimize mechanical properties under different time and temperature. For measuring the upper plateau stress, lower plateau stress and residual strain, tensile test is carried out. The samples were aged at two different temperatures to see difference between aging temperatures. The sample aged at 500 °C has a bigger crystallite size and lower amount of Ni which causes the mentioned sample to possess poor pseudo elasticity behaviour than the other aged sample. The sample aged at 460 °C has shown remarkable superelastic properties. The mentioned sample’s higher plateau is 580 MPa with the lowest residual strain (0.17%) while other samples have possessed higher residual strains. X-ray diffraction was used to investigate the produced phases.

Keywords: heat treatment, phase transformation, superelasticity, NiTi alloy

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Authors: A. Kellou, L. Rouaiguia, L. Rabahi

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In the present work, the atomic hydrogen absorption trend in the GdNi5 and GdNi4Cu rare earth compounds within the hexagonal CaCu5 type of crystal structure (space group P6/mmm) is investigated. The density functional theory (DFT) combined with the generalized gradient approximation (GGA) is used to study the site preference of atomic hydrogen at 0K. The octahedral and tetrahedral interstitial sites are considered. The formation energies and structural properties are determined in order to evaluate hydrogen effects on the stability of the studied compounds. The energetic diagram of hydrogen storage is established and compared in GdNi5 and GdNi4Cu. The magnetic properties of the selected compounds are determined using spin polarized calculations. The obtained results are discussed with and without hydrogen addition taking into account available theoretical and experimental results.

Keywords: density functional theory, hydrogen storage, rare earth compounds, structural and magnetic properties

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Authors: Elene Tatunashvili, Bun Chan, Philippe E. Nashar, Christopher S. P. McErlean

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The reduction of aryl diazonium salts is one of the most efficient ways to generate aryl radicals for use in a wide range of transformations, including Sandmeyer-type reactions, Meerwein arylations of olefins and Gomberg-Bachmann-Hey arylations of heteroaromatic systems. The aryl diazonium species can be reduced electrochemically, by UV irradiation, inner-sphere and outer-sphere single electron transfer processes (SET) from metal salts, SET from photo-excited organic catalysts or fragmentation of adducts with weak bases (acetate, hydroxide, etc.). This paper details an approach for the metal-free reduction of aryl diazonium salts, which facilitates the efficient synthesis of various aromatic compounds under exceedingly mild reaction conditions. By measuring the oxidation potential of a number of organic molecules, a series of nucleophiles were identified that reduce aryl diazonium salts via the addition-fragmentation mechanism. This approach leads to unprecedented operational simplicity: The reactions are very rapid and proceed in the open air; there is no need for external irradiation or heating, and the process is compatible with a large number of radical reactions. We illustrate these advantages by using the addition-fragmentation strategy to regioselectively arylate a series of heterocyclic compounds, to synthesize ketones by arylation of silyl enol ethers, and to synthesize benzothiophene and phenanthrene derivatives by radical annulation reactions.

Keywords: diazonium salts, hantzsch esters, oxygen, radical reactions, synthetic methods

Procedia PDF Downloads 138

Authors: Zhanna Yermekova, Sergey Roslyakov

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Solution combustion synthesis (SCS) is the unique method which multiple times has proved itself as an effective and efficient approach for the versatile synthesis of a variety of materials. It has significant advantages such as relatively simple handling process, high rates of product synthesis, mixing of the precursors on a molecular level, and fabrication of the nanoproducts as a result. Nowadays, an overwhelming majority of solution combustion investigations performed through the volume combustion synthesis (VCS) where the entire liquid precursor is heated until the combustion self-initiates throughout the volume. Less amount of the experiments devoted to the steady-state self-propagating mode of SCS. Under the beforementioned regime, the precursor solution is dried until the gel-like media, and later on, the gel substance is locally ignited. In such a case, a combustion wave propagates in a self-sustaining mode as in conventional solid combustion synthesis. Even less attention is given to the impregnated active layer (IAL) mode of solution combustion. An IAL approach to the synthesis is implying that the solution combustion of the precursors should be initiated on the surface of the third chemical or inside the third substance. This work is aiming to emphasize an underestimated role of the impregnated active layer mode of the solution combustion synthesis for the fundamental studies of the combustion mechanisms. It also serves the purpose of popularizing the technical terms and clarifying the difference between them. In order to do so, the solution combustion synthesis of γ-FeNi (PDF#47-1417) alloy has been accomplished within short (seconds) one-step reaction of metal precursors with hexamethylenetetramine (HTMA) fuel. An idea of the special role of the Ni in a process of alloy formation was suggested and confirmed with the particularly organized set of experiments. The first set of experiments were conducted in a conventional steady-state self-propagating mode of SCS. An alloy was synthesized as a single monophasic product. In two other experiments, the synthesis was divided into two independent processes which are possible under the IAL mode of solution combustion. The sequence of the process was changed according to the equations which are describing an Experiment A and B below: Experiment A: Step 1. Fe(NO₃)₃*9H₂O + HMTA = FeO + gas products; Step 2. FeO + Ni(NO₃)₂*6H₂O + HMTA = Ni + FeO + gas products; Experiment B: Step 1. Ni(NO₃)₂*6H₂O + HMTA = Ni + gas products; Step 2. Ni + Fe(NO₃)₃*9H₂O + HMTA = Fe₃Ni₂+ traces (Ni + FeO). Based on the IAL experiment results, one can see that combustion of the Fe(NO₃)₃9H₂O on the surface of the Ni is leading to the alloy formation while presence of the already formed FeO does not affect the Ni(NO₃)₂*6H₂O + HMTA reaction in any way and Ni is the main product of the synthesis.

Keywords: alloy, hexamethylenetetramine, impregnated active layer mode, mechanism, solution combustion synthesis

Procedia PDF Downloads 115

Authors: Suboohi Shervani, Jingjing Ling, Jiabin Liu, Tahir Husain

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Offshore oil-spill has become the most emerging problem in the world. In the current paper, a graphene/ZnO/polymer nanocomposite thin film is coated on stainless steel mesh via layer by layer deposition method. The structural characterization of materials is determined by Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). The total petroleum hydrocarbons (TPHs) and separation efficiency have been measured via gas chromatography – flame ionization detector (GC-FID). TPHs are reduced to 2 ppm and separation efficiency of the nanocomposite coated mesh is reached ≥ 99% for the final sample. The nanocomposite coated mesh acts as a promising candidate for the separation of oil- water mixture.

Keywords: oil spill, graphene, oil-water separation, nanocomposite

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Authors: Md Azizul Islam

Abstract:

Seam is the line of joining two separate fabric layers for functional or aesthetic purposes. Different kinds of seams are used for assembling the different areas or parts of the garment to increase serviceability. To empirically support the importance of seam efficiency on serviceability of garments, this study is focused on choosing the right type of seams for particular sewing parts of the garments based on the seam efficiency to ensure better serviceability. Seam efficiency is the ratio of seam strength and fabric strength. Single jersey knitted finished fabrics of four different GSMs (gram per square meter) were used to make the test garments T-shirt. Three distinct types of the seam: superimposed, lapped and flat seam was applied to the side seams of T-shirt and sewn by lockstitch (stitch class- 301) in a flat-bed plain sewing machine (maximum sewing speed: 5000 rpm) to make (3x4) 12 T-shirts. For experimental purposes, needle thread count (50/3 Ne), bobbin thread count (50/2 Ne) and the stitch density (stitch per inch: 8-9), Needle size (16 in singer system), stitch length (31 cm), and seam allowance (2.5cm) were kept same for all specimens. The grab test (ASTM D5034-08) was done in the Universal tensile tester to measure the seam strength and fabric strength. The produced T-shirts were given to 12 soccer players who wore the shirts for 20 soccer matches (each match of 90 minutes duration). Serviceability of the shirt were measured by visual inspection of a 5 points scale based on the seam conditions. The study found that T-shirts produced with lapped seam show better serviceability and T-shirts made of flat seams perform the lowest score in serviceability score. From the calculated seam efficiency (seam strength/ fabric strength), it was obvious that the performance (in terms of strength) of the lapped and bound seam is higher than that of the superimposed seam and the performance of superimposed seam is far better than that of the flat seam. So it can be predicted that to get a garment of high serviceability, lapped seams could be used instead of superimposed or other types of the seam. In addition, less stressed garments can be assembled by others seems like superimposed seams or flat seams.

Keywords: seam, seam efficiency, serviceability, T-shirt

Procedia PDF Downloads 184

Authors: I. Irska, S. Paszkiewicz, D. Pawlikowska, E. Piesowicz, A. Linares, T. A. Ezquerra

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Due to the number of advantages such as high tensile strength, sensitivity to hydrolytic degradation, and biocompatibility poly(lactic acid) (PLA) is one of the most common polyesters for biomedical and pharmaceutical applications. However, PLA is a rigid, brittle polymer with low heat distortion temperature and slow crystallization rate. In order to broaden the range of PLA applications, it is necessary to improve these properties. In recent years a number of new strategies have been evolved to obtain PLA-based materials with improved characteristics, including manipulation of crystallinity, plasticization, blending, and incorporation into block copolymers. Among the other methods, synthesis of aliphatic-aromatic copolyesters has been attracting considerable attention as they may combine the mechanical performance of aromatic polyesters with biodegradability known from aliphatic ones. Given the need for highly flexible biodegradable polymers, in this contribution, a series of aromatic-aliphatic based on poly(butylene terephthalate) and poly(lactic acid) (PBT-b-PLA) copolyesters exhibiting superior mechanical properties were copolymerized with an additional poly(tetramethylene oxide) (PTMO) soft block. The structure and properties of both series were characterized by means of attenuated total reflectance – Fourier transform infrared spectroscopy (ATR-FTIR), nuclear magnetic resonance spectroscopy (¹H NMR), differential scanning calorimetry (DSC), wide-angle X-ray scattering (WAXS) and dynamic mechanical, thermal analysis (DMTA). Moreover, the related changes in tensile properties have been evaluated and discussed. Lastly, the viscoelastic properties of synthesized poly(ester-ether) copolymers were investigated in detail by step cycle tensile tests. The block lengths decreased with the advance of treatment, and the block-random diblock terpolymers of (PBT-ran-PLA)-b-PTMO were obtained. DSC and DMTA analysis confirmed unambiguously that synthesized poly(ester-ether) copolymers are microphase-separated systems. The introduction of polyether co-units resulted in a decrease in crystallinity degree and melting temperature. X-ray diffraction patterns revealed that only PBT blocks are able to crystallize. The mechanical properties of (PBT-ran-PLA)-b-PTMO copolymers are a result of a unique arrangement of immiscible hard and soft blocks, providing both strength and elasticity.

Keywords: aliphatic-aromatic copolymers, multiblock copolymers, phase behavior, thermoplastic elastomers

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Authors: Amir Peyman Soleymani, Jasna Jankovic

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The augmented demand of the clean and renewable energy has necessitated the fuel cell and battery industries to produce more efficient devices at the lower prices, which can be achieved through the improvement of the electrode. Microstructural characterization, as one of the main materials development tools, plays a pivotal role in the production of better clean energy devices. In this study, methods for characterization and studying of the defects and components distribution were performed on the polymer electrolyte membrane fuel cell (PEMFC) and Li-ion battery (LIB) electrodes in 2D and 3D. The particles distribution, porosity, mechanical defects, and component distribution were studied by Scanning Electron Microscope (SEM), SEM-Focused Ion Beam (SEM-FIB), and Scanning Transmission Electron Microscope equipped with Energy Dispersive Spectroscopy (STEM-EDS). The 3D results obtained from X-ray Computed Tomography (XCT) revealed the pathways for electron and ion conductivity and defects progression maps. Computer-aided methods (Avizo) were employed to simulate the properties and performance of the microstructure in the electrodes. The suggestions were provided to improve the performance of PEMFCs and LIBs by adjusting the microstructure and the distribution of the components in the electrodes.

Keywords: PEM fuel cells, Li-ion batteries, 2D and 3D imaging, materials characterizations

Procedia PDF Downloads 138

Authors: S. Paszkiewicz, A. Zubkiewicz, A. Szymczyk, D. Pawlikowska, I. Irska, E. Piesowicz, A. Linares, T. A. Ezquerra

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Over the last century, the world has become increasingly dependent on oil as its main source of chemicals and energy. Driven largely by the strong economic growth of India and China, demand for oil is expected to increase significantly in the coming years. This growth in demand, combined with diminishing reserves, will require the development of new, sustainable sources for fuels and bulk chemicals. Biomass is an attractive alternative feedstock, as it is widely available carbon source apart from oil and coal. Nowadays, academic and industrial research in the field of polymer materials is strongly oriented towards bio-based alternatives to petroleum-derived plastics with enhanced properties for advanced applications. In this context, 2,5-furandicarboxylic acid (FDCA), a biomass-based chemical product derived from lignocellulose, is one of the most high-potential biobased building blocks for polymers and the first candidate to replace the petro-derived terephthalic acid. FDCA has been identified as one of the top 12 chemicals in the future, which may be used as a platform chemical for the synthesis of biomass-based polyester. The aim of this study is to synthesize and characterize the multiblock copolymers containing rigid segments of poly(trimethylene 2,5-furanoate) (PTF) and soft segments of poly(tetramethylene oxide) (PTMO) with excellent elastic properties or aliphatic polyesters of polycaprolactone (PCL). Two series of PTF based copolymers, i.e., PTF-block-PTMO-T and PTF-block-PCL-T, with different content of flexible segments were synthesized by means of a two-step melt polycondensation process and characterized by various methods. The rigid segments of PTF, as well as the flexible PTMO/or PCL ones, were randomly distributed along the chain. On the basis of 1H NMR, SAXS and WAXS, DSC an DMTA results, one can conclude that both phases were thermodynamically immiscible and the values of phase transition temperatures varied with the composition of the copolymer. The copolymers containing 25, 35 and 45wt.% of flexible segments (PTMO) exhibited elastomeric property characteristics. Moreover, with respect to the flexible segments content, the temperatures corresponding to 5%, 25%, 50% and 90% mass loss as well as the values of tensile modulus decrease with the increasing content of aliphatic polyether or aliphatic polyester in the composition.

Keywords: furan based polymers, multiblock copolymers, supramolecular structure, functional properties

Procedia PDF Downloads 113

Authors: T. Kuchukhidze, N. Jalagonia, T. Archuadze, G. Bokuchava

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The growing scientific-technological progress in modern civilization causes actuality of producing construction materials which can successfully work in conditions of high temperature, radiation, pressure, speed, and chemically aggressive environment. Such extreme conditions can withstand very few types of materials and among them, ceramic materials are in the first place. Corundum ceramics is the most useful material for creation of constructive nodes and products of various purposes for its low cost, easy accessibility to raw materials and good combination of physical-chemical properties. However, ceramic composite materials have one disadvantage; they are less plastics and have lower toughness. In order to increase the plasticity, the ceramics are reinforced by various dopants, that reduces the growth of the cracks. It is shown, that adding of even small amount of carbon fibers and carbon nanotubes (CNT) as reinforcing material significantly improves mechanical properties of the products, keeping at the same time advantages of alundum ceramics. Graphene in composite material acts in the same way as inorganic dopants (MgO, ZrO2, SiC and others) and performs the role of aluminum oxide inhibitor, as it creates shell, that gives possibility to reduce sintering temperature and at the same time it acts as damper, because scattering of a shock wave takes place on carbon structures. Application of different structural modification of carbon (graphene, nanotube and others) as reinforced material, gives possibility to create multi-purpose highly requested composite materials based on alundum ceramics. In the present work offers simplified technology for obtaining of aluminum oxide ceramics, reinforced with carbon nanostructures, during which chemical modification with doping carbon nanostructures will be implemented in the process of synthesis of final powdery composite – Alumina. In charge doping carbon nanostructures connected to matrix substance with C-O-Al bonds, that provide their homogeneous spatial distribution. In ceramic obtained as a result of consolidation of such powders carbon fragments equally distributed in the entire matrix of aluminum oxide, that cause increase of bending strength and crack-resistance. The proposed way to prepare the charge simplifies the technological process, decreases energy consumption, synthesis duration and therefore requires less financial expenses. In the implementation of this work, modern instrumental methods were used: electronic and optical microscopy, X-ray structural and granulometric analysis, UV, IR, and Raman spectroscopy.

Keywords: ceramic materials, α-Al₂O₃, carbon nanostructures, composites, characterization, hot-pressing

Procedia PDF Downloads 105

Authors: Zahid Shafiq, Li Liu, Dong Wang, Yong-Jun Chen

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As synthetic organic methods are increasingly concerned with the growing importance of sustainable chemistry, iodine recently has emerged as an inexpensive, non-toxic, readily available and environmentally benign catalyst for various organic transformations to afford the corresponding products in high yields with high regio- and chemoselectivity. Iodine has found widespread applications in various organic synthesis such as Michael addition, coupling reaction and also in the multicomponent synthesis where it can efficiently activate C=C, C=O, C=N, and so forth. Iodine not only has been shown to be an efficient mild Lewis acid in various processes, but also due to its moderate nature, and water tolerance, reactions catalyzed by iodine can be effectively carried out in neutral media under very mild conditions. We have successfully described an efficient procedure for the nucleophilic substitution of the Baylis-Hillman (BH) adducts and their corresponding acetates with indoles to get α-substitution product using catalytic Silver Triflate (AgOTf) as Lewis acid. At this point, we were interested to develop an environmentally benign catalytic system to effect this substitution reaction and to avoid the use of metal Lewis acid as a catalyst. Since, we observed the formation of -product during the course of the reaction, we also became interested to explore the reaction conditions in order to control regioselectivity and to obtain both regioisomers. The developed methodology resulted in regioselective substitution products with controlled selectivity. Further, the substitution products were used to synthesize various Tri- and Tetracyclo Azepino indole derivatives via reductive amination.

Keywords: indole, regioselective, Baylis-Hillman, substitution

Procedia PDF Downloads 173

Authors: Rashad Al-Gaashani, Muataz A. Atieh

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In this study, the effect of preparation temperature, namely room temperature (RT), 40, 60, and 85°C, on producing of high-quality graphene oxide (GO) has been investigated. GO samples have been prepared by chemical oxidation of graphite via a safe improved chemical technique using a blend of two deferent acids: sulphuric acid (H₂SO₄) and phosphoric acid (H₃PO₄) with volume ratio 4:1, respectively. potassium permanganate (KMnO₄) and hydrogen peroxide (H₂O₂) were applied as oxidizing agents. In this work, sodium nitrate (NaNO₃) was excluded, so the emission of hazardous explosive gases such as NO₂ and N₂O₂ was shunned. Ice and oil baths were used to carefully control the temperature. Several characterization instruments including X-Ray diffraction, transmission electron microscopy, scanning electron microscopy, electron dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and UV-vis spectroscopy were used to study and compare the synthesized samples. The results indicated that GO can be prepared at RT with graphite oxide, and the purity of GO increased with rising of the solvent temperature. Optical properties of GO samples were studied using UV-vis absorption spectra.

Keywords: chemical method, graphite, graphene oxide, optical properties

Procedia PDF Downloads 145

Authors: Chukwudalu C. Nwazojie, Wole W. Soboyejo, John Obayemi, Ali Salifu Azeko, Sandra M. Jusu, Chinyerem M. Onyekanne

Abstract:

The conventional methods for the diagnosis and treatment of breast cancer include bulk systematic mammography, ultrasound, dynamic contrast-enhanced fast 3D gradient-echo (GRE) magnetic resonance imaging (MRI), surgery, chemotherapy, and radiotherapy. However, nanoparticles and drug-loaded polymer microspheres for disease (cancer) targeting and treatment have enormous potential to enhance the approaches that are used today. The goal is to produce an implantable biomedical device for localized breast cancer drug delivery within Africa and the world. The main advantage of localized delivery is that it reduces the amount of drug that is needed to have a therapeutic effect. Polymer blends of poly (D,L-lactide-co-glycolide) (PLGA) and polycaprolactone (PCL), which are biodegradable, is used as a drug excipient. This work focuses on the development of PLGA-PCL (poly (D,L-lactide-co-glycolide) (PLGA) blended with based injectable drug microspheres and are loaded with anticancer drugs (prodigiosin (PG), and paclitaxel (PTX) control) and also the conjugated forms of the drug functionalized with LHRH (luteinizing hormone-releasing hormone) (PG-LHRH, and PTX- LHRH control), using a single-emulsion solvent evaporation technique. The encapsulation was done in the presence of PLGA-PCL (as a polymer matrix) and poly-(vinyl alcohol) (PVA) (as an emulsifier). Comparative study of the various drugs release kinetics and degradation mechanisms of the PLGA-PCL with an encapsulated drug is achieved, and the implication of this study is for the potential application of prodigiosin PLGA-PCL loaded microparticles for controlled delivery of cancer drug and treatment to prevent the regrowth or locoregional recurrence, following surgical resection of triple-negative breast tumor.

Keywords: cancer, polymers, drug kinetics, nanoparticles

Procedia PDF Downloads 85

Authors: Sohaib Z. Khan, Farrukh Mustahsan, Essam R. I. Mahmoud, S. H. Masood

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Materials or structures that contract laterally on the application of a compressive load and vice versa are said to be Auxetic materials which exhibit Negative Poisson’s Ratio (NPR). Numerous auxetic structures are proposed in the literature. One of the most studied periodic auxetic structure is the re-entrant honeycomb model. In this paper, a modified re-entrant model is proposed to enhance the auxetic behavior. The paper aimed to investigate the elastic behaviour of the proposed model to improve Young’s modulus and NPR by evaluating the analytical model. Finite Element Analysis (FEA) is also conducted to support the analytical results. A significant increment in Young’s modulus and NPR can be achieved in one of the two orthogonal directions of the loading at the cost of compromising these values in other direction. The proposed modification resulted in lower relative densities when compared to the existing re-entrant honeycomb structure. A trade-off in the elastic properties in one direction at low relative density makes the proposed model suitable for uni-direction applications where higher stiffness and NPR is required, and strength to weight ratio is important.

Keywords: 2D model, auxetic materials, re-entrant honeycomb, negative Poisson's ratio

Procedia PDF Downloads 125

Authors: K. Uyanga, W. Daoud

Abstract:

Hydrogels have attracted much academic and industrial attention due to their unique properties and potential biomedical and non-biomedical applications. Limitations on extending their applications have resulted from the synthesis of hydrogels using toxic materials and complex irreproducible processing techniques. In order to promote environmental sustainability, hydrogel efficiency, and wider application, this study focused on the synthesis of composite hydrogels matrices from an edible non-toxic crosslinker-citric acid (CA) using a simple low energy processing method based on carboxymethyl cellulose (CMC) and chitosan (CSN) natural polymers. Composite hydrogels were developed by chemical crosslinking. The results demonstrated that CMC:2CSN:CA exhibited good performance properties and super-absorbency 21× its original weight. This makes it promising for biomedical applications such as chronic wound healing and regeneration, next generation skin substitute, in situ bone regeneration and cell delivery. On the other hand, CMC:CSN:CA exhibited durable well-structured internal network with minimum swelling degrees, water absorbency, excellent gel fraction, and infra-red reflectance. These properties make it a suitable composite hydrogel matrix for warming effect and controlled and efficient release of loaded materials. CMC:2CSN:CA and CMC:CSN:CA composite hydrogels developed also exhibited excellent chemical, morphological, and thermal properties.

Keywords: citric acid, fumaric acid, tartaric acid, zinc nitrate hexahydrate

Procedia PDF Downloads 127

Authors: Dileep Maarisetty, Janaki Komandur, Saroj S. Baral

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In the current work, photocatalytic degradation of phenol was carried both in UV and visible light to find the slowest step that is limiting the rate of photo-degradation process. Characterization such as XRD, SEM, FT-IR, TEM, XPS, UV-DRS, PL, BET, UPS, ESR and zeta potential experiments were conducted to assess the credibility of catalysts in boosting the photocatalytic activity. To explore the synergy, TiO₂ was doped with graphene and alumina. The orbital hybridization with alumina doping (mediated by graphene) resulted in higher electron transfer from the conduction band of TiO₂ to alumina surface where oxygen reduction reactions (ORR) occur. Besides, the doping of alumina and graphene introduced defects into Ti lattice and helped in improving the adsorptive properties of modified photo-catalyst. Results showed that these defects promoted the oxygen reduction reactions (ORR) on the catalyst’s surface. ORR activity aims at producing reactive oxygen species (ROS). These ROS species oxidizes the phenol molecules which is adsorbed on the surface of photo-catalysts, thereby driving the photocatalytic reactions. Since mass transfer is considered as rate limiting step, various mathematical models were applied to the experimental data to probe the best fit. By varying the parameters, it was found that intra-particle diffusion was the slowest step in the degradation process. Lagergren model gave the best R² values indicating the nature of rate kinetics. Similarly, different adsorption isotherms were employed and realized that Langmuir isotherm suits the best with tremendous increase in uptake capacity (mg/g) of TiO₂-rGO-Al₂O₃ as compared undoped TiO₂. This further assisted in higher adsorption of phenol molecules. The results obtained from experimental, kinetic modelling and adsorption isotherms; it is concluded that apart from changes in surface, optoelectronic and morphological properties that enhanced the photocatalytic activity, the intra-particle diffusion within the catalyst’s pores serve as rate-limiting step in deciding the fate of photo-catalytic degradation of phenol.

Keywords: ORR, phenol degradation, photo-catalyst, rate kinetics

Procedia PDF Downloads 131