Search results for: in situ FTIR

Authors: Sima Shakoorjavan, Mahdieh Eskafi, Dawid Stawski, Somaye Akbari

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In this study, poly (amidoamine) dendritic material (PAMAM) and poly (acrylic acid) (PAA) as polycation and polyanion were deposited on surface charged polylactide (PLA) nonwoven to study the relationship of dye absorption capacity of layered-PLA with the number of deposited layers. To produce negatively charged-PLA, acrylic acid (AA) was grafted on the PLA surface (PLA-g-AA) through a chemical redox reaction with the strong oxidizing agent. Spectroscopy analysis, water contact measurement, and FTIR-ATR analysis confirm the successful grafting of AA on the PLA surface through the chemical redox reaction method. In detail, an increase in dye absorption percentage by 19% and immediate absorption of water droplets ensured hydrophilicity of PLA-g-AA surface; and the presence of new carbonyl bond at 1530 cm-¹ and a wide peak of hydroxyl between 3680-3130 cm-¹ confirm AA grafting. In addition, PLA as linear polyester can undergo aminolysis, which is the cleavage of ester bonds and replacement with amid bonds when exposed to an aminolysis agent. Therefore, to produce positively charged PLA, PAMAM as amine-terminated dendritic material was introduced to PLA molecular chains at different conditions; (1) at 60 C for 0.5, 1, 1.5, 2 hours of aminolysis and (2) at room temperature (RT) for 1, 2, 3, and 4 hours of aminolysis. Weight changes and spectrophotometer measurements showed a maximum in weight gain graph and K/S value curve indicating the highest PAMAM attachment at 60 C for 1 hour and RT for 2 hours which is considered as an optimum condition. Also, the emerging new peak around 1650 cm-1 corresponding to N-H bending vibration and double wide peak at around 3670-3170 cm-1 corresponding to N-H stretching vibration confirm PAMAM attachment in selected optimum condition. In the following, regarding the initial surface charge of grafted-PLA, lbl deposition was performed and started with PAA or PAMAM. FTIR-ATR results confirm chemical changes in samples due to deposition of the first layer (PAA or PAMAM). Generally, spectroscopy analysis indicated that an increase in layer number costed dye absorption capacity. It can be due to the partial deposition of a new layer on the previously deposited layer; therefore, the available PAMAM at the first layer is more than the third layer. In detail, in the case of layer-PLA starting lbl with negatively charged, having PAMAM as the first top layer (PLA-g-AA/PAMAM) showed the highest dye absorption of both cationic and anionic model dye.

Keywords: surface modification, layer-by-layer technique, dendritic materials, PAMAM, dye absorption capacity, PLA nonwoven

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Authors: A. V. Shelke, P. S. More

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This research aimed to study the kinetic reaction of reused cooking oil and to find the optimum condition of its process. The feedstock was collected from the street sellers and also prepared at laboratory. From this research, it is found that the kinetic reaction of reused sunflower oil (auto-oxidation) is obtained in terms of variation of the absorption coefficient of unexposed sunflower oil as 0.05 which is very close to that of exposed sunflower oil 0.075. At room temperature, the optimum intensity obtained from optical absorption spectroscopy study is 0.267 for unexposed sunflower oil and 0.194 for exposed sunflower oil. However, results indicated that FTIR spectroscopy is accurate and precise enough for such determination. Free Fatty Acid (FFA% = 026), acid ~53% and safonication ~%192 get reduce in exposed oil was investigated.

Keywords: friction, oxidation, sunflower oil, vegetable oils

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Authors: El Hatka Hicham, Hafidi Youssef, Saghiri Khalid, Ittobane Najim

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Flexible polyurethane foam (FPUF) is a low-density cellular material generally used as a cushioning material in many applications such as furniture, bedding, packaging, etc. It is commercially produced during a continuous process, where a reactive mixture of foam chemicals is poured onto a moving conveyor. FPUFs are produced by the catalytic balancing of two reactions involved, the blowing reaction (isocyanate-water) and the gelation reaction (isocyanate-polyol). The microstructure of FPUF is generally composed of soft phases (polyol phases) and rigid domains that separate into two domains of different sizes: the rigid polyurea microdomains and the macrodomains (larger aggregates). The morphological features of FPUF are strongly influenced by the phase separation morphology that plays a key role in determining the global FPUF properties. This phase-separated morphology results from a thermodynamic incompatibility between soft segments derived from aliphatic polyether and hard segments derived from the commonly used aromatic isocyanate. In order to improve the properties of FPUF against the different stresses faced by this material during its use, we report in this work a study of the phase separation phenomenon in FPUF that has been examined using SAXS WAXS and FTIR. Indeed, we have studied with these techniques the effect of water, isocyanates, and alkaline chlorides on the phase separation behavior. SAXS was used to study the morphology of the microphase separated, WAXS to examine the nature of the hard segment packing, and FTIR to investigate the hydrogen bonding characteristics of the materials studied. The prepared foams were shown to have different levels of urea phase connectivity; the increase in water content in the FPUF formulation leads to an increase in the amount of urea formed and consequently the increase of the size of urea aggregates formed. Alkali chlorides (NaCl, KCl, and LiCl) incorporated into FPUF formulations show that is the ability to prevent hydrogen bond formation and subsequently alter the rigid domains. FPUFs prepared by different isocyanate structures showed that urea aggregates are difficult to be formed in foams prepared by asymmetric diisocyanate, while are more easily formed in foams prepared by symmetric and aliphatic diisocyanate.

Keywords: flexible polyurethane foam, hard segments, phase separation, soft segments

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Authors: D. Önen, N. Kızılcan, B. Yıldız, A. Akar

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In situ modified cyclohexanone-formaldehyde resins were prepared by addition of alendronic acid during resin preparation. Clay nanocomposites in ketonic resins were achieved by adding clay into the flask at the beginning of the resin preparation. The prepared resins were used for the synthesis of fire resistant polyurethanes foam. Both phosphorous containing modifier compound alendronic acid and nanoclay increases fire resistance of the cyclohexanone-formaldehyde resin thus polyurethane produced from these resins. The effect of the concentrations of alendronic acid and clay on the fire resistance and physical properties of polyurethanes was studied.

Keywords: alendronic acid, clay, ketonic resin, polyurethane

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Authors: Irshad U. Khan, Tanmay Paul, Murali Mohan Seepana

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This paper presents a study on synthesizing and characterizing a Copper oxide doped Carbon (CuO-C) electrocatalyst for the negative half-cell reactions of Vanadium Redox Flow Battery (VRFB). The CuO was synthesized using a microreactor. The electrocatalyst was characterized using X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Field Emission Scanning Electron Microscopy (SEM). The electrochemical performance was assessed by linear sweep voltammetry (LSV). The findings suggest that the synthesized CuO exhibited favorable crystallinity, morphology, and surface area, which reflects improved cell performance.

Keywords: ECSA, electrocatalyst, energy storage, Tafel

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Authors: Paresh Patel, Priya Patel, Vaidehi Sorathiya, Navin Sheth

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The aim of present work was to fabricate Salmeterol Xinafoate (SX) metered dose inhaler (MDI) for asthma and to evaluate the SX loaded solid lipid nanoparticles (SLNs) for pulmonary delivery. Solid lipid nanoparticles can be used to deliver particles to the lungs via MDI. A modified solvent emulsification diffusion technique was used to prepare Salmeterol Xinafoate loaded solid lipid nanoparticles by using compritol 888 ATO as lipid, tween 80 as surfactant, D-mannitol as cryoprotecting agent and L-leucine was used to improve aerosolization behaviour. Box-Behnken design was applied with 17 runs. 3-D surface response plots and contour plots were drawn and optimized formulation was selected based on minimum particle size and maximum % EE. % yield, in vitro diffusion study, scanning electron microscopy, X-ray diffraction, DSC, FTIR also characterized. Particle size, zeta potential analyzed by Zetatrac particle size analyzer and aerodynamic properties was carried out by cascade impactor. Pre convulsion time was examined for control group, treatment group and compare with marketed group. MDI was evaluated for leakage test, flammability test, spray test and content per puff. By experimental design, particle size and % EE found to be in range between 119-337 nm and 62.04-76.77% by solvent emulsification diffusion technique. Morphologically, particles have spherical shape and uniform distribution. DSC & FTIR study showed that no interaction between drug and excipients. Zeta potential shows good stability of SLNs. % respirable fraction found to be 52.78% indicating reach to the deep part of lung such as alveoli. Animal study showed that fabricated MDI protect the lungs against histamine induced bronchospasm in guinea pigs. MDI showed sphericity of particle in spray pattern, 96.34% content per puff and non-flammable. SLNs prepared by Solvent emulsification diffusion technique provide desirable size for deposition into the alveoli. This delivery platform opens up a wide range of treatment application of pulmonary disease like asthma via solid lipid nanoparticles.

Keywords: salmeterol xinafoate, solid lipid nanoparticles, box-behnken design, solvent emulsification diffusion technique, pulmonary delivery

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Authors: Debdut Roy, Vidyasagar Guggilla

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In this research, we highlight our exploratory work on modified zeolite based catalysts for catalytic cracking of hydrocarbons for production of light olefin i.e. ethylene and propylene. The work is focused on understanding the catalyst structure and activity correlation. Catalysts are characterized by surface area and pore size distribution analysis, inductively coupled plasma optical emission spectrometry (ICP-OES), Temperature Programmed Desorption (TPD) of ammonia, pyridine Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Thermo-gravimetric Analysis (TGA) and correlated with the catalytic activity. It is observed that the yield of lighter olefins increases with increase of Bronsted acid strength.

Keywords: catalytic cracking, zeolite, propylene, structure-activity correlation

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Authors: Mohammadreza Biabani, Mohammad Azadfallah

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A facile and robust strategy is required to fabricate films with high special optical properties for application in the field of anti-counterfeit marking. Nanocellulose, derived from bioresources, is a renewable material with broad application prospects. In this paper, a method for grafting the eco-friendly Berberine cationic dye on cellulose nanofiber is proposed. A functional modification was carried out by in-situ polymerization along with a grafting approach with acrylic acid(AA) in order to develop cationic dyeability of the cellulose nanofiber (CNF). The Berberine grafting on nanocellulose was significantly influenced by the reaction time and temperature during the dyeing process. The dyed CNF-films exhibited appropriate characteristics like appearance, color strength, and fastness for anti-counterfeiting application.

Keywords: Cellulose nanofiber, Berberine, Grafting, anti-counterfeiting, film

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Authors: Kittisak Jantanasakulwong, Toshiaki Ougizawa

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Thermoplastic starch (TPS) was prepared by melt-blending of cassava starch with glycerol (70/30 wt%/wt%) at 130 ◦C for 10 min. Chitosan (CTS) was used as a compatibilizer. TPS/CTS blend was melt-blended with maleic anhydride grafted ethylene-1-butene rubber (EB-MAH) in the composition of 80/20 respectively. Addition of CTS in TPS/EB-MAH blend decreased particles size of EB-MAH rubber to 1µm in TPS matrix. Mechanical properties, solubility, swelling property, morphology, and water contact angle of TPS/EB-MAH blend were improved by CTS incorporation. FTIR confirmed a reaction had occurred between amino groups (-NH2) of CTS and the MAH groups of EB-MAH. This reaction and the enhanced miscibility between TPS and CTS improved morphology and properties of the TPS/EB-MAH/CTS blend.

Keywords: thermoplastic starch, rubber, reactive blending, chitosan

Procedia PDF Downloads 194

Authors: Ahmed F. Ghanem, Marwa I. Wahba, Asmaa N. El-Dein, Mohamed A. EL-Raey, Ghada E. A. Awad

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Numerous attempts are being performed in order to formulate suitable packaging materials for the meat products. However, to the best of our knowledge, the incorporation of the free hibiscus extract or its microcapsules in the pure polyvinyl alcohol (PVA) matrix as packaging materials for the meats is seldom reported. Therefore, this study aims at the protection of the aqueous crude extract of the hibiscus flowers utilizing the spry drying encapsulation technique. Results of the Fourier transform infrared (FTIR), the scanning electron microscope (SEM), and the particle size analyzer confirmed the successful formation of the assembled capsules via strong interactions, the spherical rough microparticles, and the particle size of ~ 235 nm, respectively. Also, the obtained microcapsules enjoy higher thermal stability than the free extract. Then, the obtained spray-dried particles were incorporated into the casting solution of the pure PVA film with a concentration of 10 wt. %. The segregated free-standing composite films were investigated, compared to the neat matrix, with several characterization techniques such as FTIR, SEM, thermal gravimetric analysis (TGA), mechanical tester, contact angle, water vapor permeability, and oxygen transmission. The results demonstrated variations in the physicochemical properties of the PVA film after the inclusion of the free and the extract microcapsules. Moreover, biological studies emphasized the biocidal potential of the hybrid films against the microorganisms contaminating the meat. Specifically, the microcapsules imparted not only antimicrobial but also antioxidant activities to the PVA matrix. Application of the prepared films on the real meat samples displayed a low bacterial growth with a slight increase in the pH over the storage time which continued up to 10 days at 4 oC, as further evidence to the meat safety. Moreover, the colors of the films did not significantly changed except after 21 days indicating the spoilage of the meat samples. No doubt, the dual-functional of the prepared composite films pave the way towards combined active and smart food packaging applications. This would play a vital role in the food hygiene, including also the quality control and the assurance.

Keywords: PVA, hibiscus, extraction, encapsulation, active packaging, smart and intelligent packaging, meat spoilage

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Authors: Reyhan Özdoğan, Mithat Çelebi, Özgür Ceylan, Mehmet Arif Kaya

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Super absorbent polymers (SAPs) are defined as materials that can absorb huge amount of water or aqueous solution in comparison to their own mass and retain in their lightly cross-linked structure. SAPs were produced from water soluble monomers via polymerization subsequently controlled crosslinking. SAPs are generally used for water absorbing applications such as baby diapers, patient or elder pads and other hygienic product industries. Crosslinking density (CD) of SAP structure is an essential factor for water absortion capacity (WAC). Low internal CD leads to high WAC values and vice versa. However, SAPs have low CD and high swelling capacities and tend to disintegrate when pressure is applied upon them, so SAPs under load cannot absorb liquids effectively. In order to prevent this undesired situation and to obtain suitable SAP structures having high swelling capacity and ability to work under load, surface crosslinking can be the answer. In industry, these superabsorbent gels are mostly produced via solution polymerization and then they need to be dried, grinded, sized, post polymerized and finally surface croslinked (involves spraying of a crosslinking solution onto dried and grinded SAP particles, and then curing by heat). It can easily be seen that these steps are time consuming and should be handled carefully for the desired final product. If we could synthesize desired final SAPs using less processes it will help reducing time and production costs which are very important for any industries. In this study, synthesis of SAPs were achieved successfully by inverse suspension (Pickering type) polymerization and subsequently in-situ surface cross-linking via using proper surfactants in high boiling point solvents. Our one-pot synthesis of surface cross-linked SAPs invovles only one-step for preparation, thus it can be said that this technique exhibits more preferable characteristic for the industry in comparison to conventional methods due to its one-step easy process. Effects of different surface crosslinking agents onto properties of poly(acrylic acid-co-sodium acrylate) based SAPs are investigated. Surface crosslink degrees are evaluated by swelling under load (SUL) test. It was determined water absorption capacities of obtained SAPs decrease with the increasing surface crosslink density while their mechanic properties are improved.

Keywords: inverse suspension polymerization, polyacrylic acid, super absorbent polymers (SAPs), surface crosslinking, sodium polyacrylate

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Authors: Hilal Kivrak, Aykut ÇağLar, Nahit Aktaş, Ali Osman Solak

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At present, Cd/TiO₂ and CdTe/TiO₂ catalysts are prepared via sodium borohydride (NaBH4) reduction method. These catalysts are characterized by fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). These Cd/TiO₂ and CdTe/TiO₂ are employed as catalysts for the photocatalytic oxidation of glucose. Cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) measurements are used to investigate their glucose electrooxidation activities of catalysts at long and under UV illumination (ʎ=354 nm). CdTe/TiO₂ catalyst is showed the best photocatalytic glucose electrooxidation activity compared to Cd/TiO₂ catalyst.

Keywords: cadmium, NaBH4 reduction method, photocatalytic glucose electrooxidation, Tellerium, TiO2

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Authors: Grigoria Athanasaki, Veerarajan Vimala, A. M. Kannan, Louis Cindrella

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Energy usage has been increased throughout the years, leading to severe environmental impacts. Since the majority of the energy is currently produced from fossil fuels, there is a global need for clean energy solutions. Proton Exchange Membrane Fuel Cells (PEMFCs) offer a very promising solution for transportation applications because of their solid configuration and low temperature operations, which allows them to start quickly. One of the main components of PEMFCs is the Gas Diffusion Layer (GDL), which manages water and gas transport and shows direct influence on the fuel cell performance. In this work, a novel dual-layer GDL with gradient porosity was prepared, using polyethylene glycol (PEG) as pore former, to improve the gas diffusion and water management in the system. The microporous layer (MPL) of the fabricated GDL consists of carbon powder PUREBLACK, sodium dodecyl sulfate as a surfactant, 34% wt. PTFE and the gradient porosity was created by applying one layer using 30% wt. PEG on the carbon substrate, followed by a second layer without using any pore former. The total carbon loading of the microporous layer is ~ 3 mg.cm-2. For the assembly of the catalyst layer, Nafion membrane (Ion Power, Nafion Membrane NR211) and Pt/C electrocatalyst (46.1% wt.) were used. The catalyst ink was deposited on the membrane via microspraying technique. The Pt loading is ~ 0.4 mg.cm-2, and the active area is 5 cm2. The sample was ex-situ characterized via wetting angle measurement, Scanning Electron Microscopy (SEM), and Pore Size Distribution (PSD) to evaluate its characteristics. Furthermore, for the performance evaluation in-situ characterization via Fuel Cell Testing using H2/O2 and H2/air as reactants, under 50, 60, 80, and 100% relative humidity (RH), took place. The results were compared to a single layer GDL, fabricated with the same carbon powder and loading as the dual layer GDL, and a commercially available GDL with MPL (AvCarb2120). The findings reveal high hydrophobic properties of the microporous layer of the GDL for both PUREBLACK based samples, while the commercial GDL demonstrates hydrophilic behavior. The dual layer GDL shows high and stable fuel cell performance under all the RH conditions, whereas the single layer manifests a drop in performance at high RH in both oxygen and air, caused by catalyst flooding. The commercial GDL shows very low and unstable performance, possibly because of its hydrophilic character and thinner microporous layer. In conclusion, the dual layer GDL with PEG appears to have improved gas diffusion and water management in the fuel cell system. Due to its increasing porosity from the catalyst layer to the carbon substrate, it allows easier access of the reactant gases from the flow channels to the catalyst layer, and more efficient water removal from the catalyst layer, leading to higher performance and stability.

Keywords: gas diffusion layer, microporous layer, proton exchange membrane fuel cells, relative humidity

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Authors: Merve Küçük, M. Lütfi Öveçoğlu

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Zinc oxide particles were synthesized using the sol-gel method and dip coated on polyester fabric. X-ray diffraction (XRD) analysis revealed a single crystal phase of ZnO particles. Chemical characteristics of the polyester fabric surface were investigated using attenuated total reflection-Fourier transform infrared (ATR-FTIR) measurements. Morphology of ZnO coated fabric was analyzed using field emission scanning electron microscopy (FESEM). After particle analysis, the aqueous ZnO solution resulted in a narrow size distribution at submicron levels. The deposit of ZnO on polyester fabrics yielded a homogeneous spread of spherical particles. Energy dispersive X-ray spectroscopy (EDX) results also affirmed the presence of ZnO particles on the polyester fabrics.

Keywords: dip coating, polyester fabrics, sol gel, zinc oxide

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Authors: Krittapast Dara-Opast, Sureeporn Ruengsangtongkul, Jumreang Tummatorn, Kittipong Chainok, Onrapak Reamtong, Somsak Ruchirawat, Charnsak Thongsornkleeb

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Selective synthesis of gem-dihalo spiroisobenzofuran and spiroisocoumarin can be performed via halogenative double cyclization of methyl 2-(hydroxyalk-1-yn-1-yl) benzoates in the presence of either N-chlorosuccinimide (NCS) or N-bromosuccinimide (NBS) and chlorotrimethylsilane (TMSCl). The combination of NCS and TMSCl led to the generation of electrophilic chlorine in situ, which activated the alkyne functional group of the substrate leading to the cyclization via either 5-exo-dig or 6-endo-dig mode of cyclization to produce the target compounds in moderate yields. The protocol could be carried on a broad scope of substrates under mild conditions (0 °C to rt). The parent compounds showed good antiparasitic activity compared to standard drug albendazole. Further investigation of the scope of the reaction and their antiparasitic activities is underway.

Keywords: antiparasitic activities, halogenative annulation, spirocycles, spirocyclization

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Authors: Anika Zafiah M. Rus, Nur Munirah Abdullah, M. F. L. Abdullah

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The fabrication and characterization of composite films of graphite- bioepoxy is described. Free-standing thin films of ~0.1 mm thick are prepared using a simple solution mixing with mass proportion of 7/3 (bioepoxy/graphite) and drop casting at room temperature. Fourier transform infra-red spectroscopy (FTIR) and Ultraviolet-visible (UV-vis) spectrophotometer are performed to evaluate the changes in chemical structure and adsorption spectra arising with the increasing of graphite weight loading (wt.%) into the biopolymer matrix. The morphologic study shows a homogeneously dispersed and strong particle bonding between the graphite and the bioepoxy, with conductivity of the film 103 S/m, confirming the efficiency of the processes.

Keywords: absorbance peak, biopolymer, graphite- bioepoxy composites, particle bonding

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Authors: Jong-Ho Moon, Dong-Ho Lee, Hyunuk Kim, Young Cheol Park, Jong-Seop Lee, Jae-deok Jeon, Hyung-Keun Lee

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A novel membrane reactor process for DMC synthesis from carbon dioxide has been developing in Korea Institute of Energy Research. The scheme of direct synthesis of DMC from CO₂ and Methanol is 'CO₂ + 2MeOH ↔ DMC + H₂O'. Among them, reactants are CO₂ and MeOH, product is DMC, and byproduct is H₂O (water). According to Le Chatelier’s principle, removing byproduct (water) can shift the reaction equilibrium to the right (DMC production). The main purpose of this process is removing water during the reaction. For efficient in situ water removal (dehydration) and DMC separation, zeolite 4A membranes with very small pore diameter and hydrophilicity were introduced. In this study, pervaporation performances of binary and ternary DMC / methanol / water mixtures were evaluated.

Keywords: dimehtyl carbonate, methanol, water, zeolite membrane, pervaporation

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Authors: M. Kalyan Raj, Vinay Umesh Rao, M. Sudhakar

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The work focuses on the development of a directly compressible controlled release co-processed excipient using melt granulation technique. Erodible wax matrix systems are fabricated in which three different types of waxes are co processed separately with Maize starch in different ratios by melt granulation. The resultant free flowing powder is characterized by FTIR, NMR, Mass spectrophotometer and gel permeation chromatography. Also, controlled release tablets of Aripiprazole were formulated and dissolution profile was compared with that of the target product profile given in Zysis patent (Patent no. 20100004262) for Aripiprazole once a week formulation.

Keywords: co-processing, hot melt extrusion, direct compression, maize starch, stearic acid, aripiprazole

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Authors: Hamad Almohamadi, Nabeel H. Alharthi, Abdulrahman Aljabri

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In this study, two-dimensional CuFeOx is deposited on nickel foam for the fabrication of electrocatalyst for oxygen evolution reaction (OER). The in-situ hydrothermal synthesis of CuFeOx in presence of aloe vera extract was found to yield unique nano-rose-like morphology which aided to improve the electrochemical surface area of the electrode. The phytochemical assisted synthesis of CuFeOx using 75% aloe vera extract resulted in improved OER electrocatalytic performance by attaining the overpotential of 310 mV for 50 mA cm−2 and 410 mV for 100 mA cm−2. The electrode also sustained robust stability throughout the 50 h of chronopotentiometry studies under alkaline electrolyte conditions, thus proving to be prospective electrode material for efficient OER in electrochemical water splitting.

Keywords: water splitting, phytochemicals, oxygen evaluation reaction, Tafel's slope, stability

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Authors: Fatima Zahra Mahjoubi, Abderrahim Khalidi, Mohamed Abdennouri, Omar Cherkaoui, Noureddine Barka

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Industrial effluents are one of the major causes of environmental pollution, especially effluents discharged from various dyestuff manufactures, plastic, and paper making industries. These effluents can give rise to certain hazards and environmental problems for their highly colored suspended organic solid. Dye effluents are not only aesthetic pollutants, but coloration of water by the dyes may affect photochemical activities in aquatic systems by reducing light penetration. It has been also reported that several commonly used dyes are carcinogenic and mutagenic for aquatic organisms. Therefore, removing dyes from effluents is of significant importance. Many adsorbent materials have been prepared in the removal of dyes from wastewater, including anionic clay or layered double hydroxyde. The zinc/aluminium (Zn-AlNO₃), magnesium/aluminium (Mg-AlNO₃) and nickel/aluminium (Ni-AlNO₃) layered double hydroxides (LDHs) were successfully synthesized via coprecipitation method. Samples were characterized by XRD, FTIR, TGA/DTA, TEM and pHPZC analysis. XRD patterns showed a basal spacing increase in the order of Zn-AlNO₃ (8.85Å)> Mg-AlNO₃ (7.95Å)> Ni-AlNO₃ (7.82Å). FTIR spectrum confirmed the presence of nitrate anions in the LDHs interlayer. The TEM images indicated that the Zn-AlNO3 presents circular to shaped particles with an average particle size of approximately 30 to 40 nm. Small plates assigned to sheets with hexagonal form were observed in the case of Mg-AlNO₃. Ni-AlNO₃ display nanostructured sphere in diameter between 5 and 10 nm. The LDHs were used as adsorbents for the removal of methyl orange (MO), as a model dye and for the treatment of an effluent generated by a textile factory. Adsorption experiments for MO were carried out as function of solution pH, contact time and initial dye concentration. Maximum adsorption was occurred at acidic solution pH. Kinetic data were tested using pseudo-first-order and pseudo-second-order kinetic models. The best fit was obtained with the pseudo-second-order kinetic model. Equilibrium data were correlated to Langmuir and Freundlich isotherm models. The best conditions for color and COD removal from textile effluent sample were obtained at lower values of pH. Total color removal was obtained with Mg-AlNO₃ and Ni-AlNO₃ LDHs. Reduction of COD to limits authorized by Moroccan standards was obtained with 0.5g/l LDHs dose.

Keywords: chemical oxygen demand, color removal, layered double hydroxides, textile wastewater treatment

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Authors: Sarah Fahad Alajmi, Tamer Ezzat Youssef

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Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.

Keywords: green chemistry, 1H-indole, heteroaromatic, organic electrosynthesis

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Authors: Sarwar Beg, Gajanand Sharma, O. P. Katare, Bhupinder Singh

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The current studies entail development of self-nano emulsifying drug delivery systems (SNEDDS) of rosuvastatin, employing rational QbD-based approach for enhancing its oral bioavailability. SNEDDS were prepared using the blend of lipidic and emulsifying excipients, i.e., Peceol, Tween 80, and Transcutol HP. The prepared formulations evaluated for in vitro drug release, ex vivo permeation, in situ perfusion studies and in vivo pharmacokinetic studies in rats, which demonstrated 3-4 fold improvement in biopharmaceutical performance of the developed formulations. Cytotoxicity studies using MTT assay and histopathological studies in intestinal cells revealed the lack of cytotoxicity and thereby safety and efficacy of the developed formulations.

Keywords: SNEDDS, bioavailability, solubility, Quality by Design (QbD)

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Authors: M. A. Islam, P. J. Hazell, J. P. Escobedo, M. Saadatfar

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Quasistatic compression and micro structural characterization of closed cell aluminium foams of different pore size and cell distributions has been carried out. Metallic foams have good potential for lightweight structures for impact and blast mitigation and therefore it is important to find out the optimized foam structure (i.e. cell size, shape, relative density, and distribution) to maximize energy absorption. In this paper, we present results for two different aluminium metal foams of density 0.5 g/cc and 0.7 g/cc respectively that have been tested in quasi-static compression. The influence of cell geometry and cell topology on quasistatic compression behavior has been investigated using computed tomography (micro-CT) analysis. The compression behavior and micro structural characterization will be presented.

Keywords: metal foams, micro-CT, cell topology, quasistatic compression

Procedia PDF Downloads 447

Authors: P. Raajeswari, S. M. Devatha, S. Yuvajanani, U. Rashika

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Edible food packaging are the need of the hour to save life on land and under water by eliminating waste cycle and replacing Single Use Plastics at grass root level as it can be eaten or composted as such. Cassava (Manihot esculenta) selected for making edible films are rich source of starch, and also it exhibit good sheeting propertiesdue to the high amylose: amylopectin content. Cassava starch was extracted by manual method at a laboratory scale and yielded 65 per cent. Edible films were developed by adding food grade plasticizers and water. Glycerol showed good plasticizing property as compared to sorbitol and polylactic acid in both manual (petri dish) and machine (film making machine) production. The thickness of the film is 0.25±0.03 mm. Essential oil and components from peels like pomegranate, orange, pumpkin, onion, and banana brat, and herbs like tulsi and country borage was extracted through the standardized aqueous and alkaline method. In the standardized film, the essential oil and components from selected peel and herbs were added to the casting solution separately and casted the film. It was added to improve the anti-oxidant, anti-microbial and optical properties. By inclusion of extracts, it reduced the bubble formation while casting. FTIR, Water Vapor and Oxygen Transmission Rate (WVTR and OTR), tensile strength, microbial load, shelf life, and degradability of the films were done to analyse the mechanical property of the standardized films. FTIR showed the presence of essential oil. WVTR and OTR of the film was improved after inclusion of essential oil and extracts from 1.312 to 0.811 cm₃/m₂ and 15.12 to 17.81 g/ m₂.d. Inclusion of essential oil from herbs showed better WVTR and OTR than the inclusion of peel extract and standard. Tensile strength and Elongation at break has not changed by essential oil and extracts at 0.86 ± 0.12 mpa and 14 ± 2 at 85 N force. By inclusion of extracts, an optical property of the film enhanced, and it increases the appearance of the packaging material. The films were completely degraded on 84thdays and partially soluble in water. Inclusion of essential oil does not have impact on degradability and solubility. The microbial loads of the active films were decreased from 15 cfu/gm to 7 cfu/gm. The films can be stored at frozen state for 24 days and 48 days at atmospheric temperature when packed with South Indian snacks and savories.

Keywords: active films, cassava starch, plasticizer, characterization

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Authors: Yogesh S. Patel

Abstract:

Novel polyimides were synthesized by Diels–Alder polymerization. Bisfuran was reacted with a couple of bismaleimides containing diglycidyl ether of bisphenol-A and F (epoxy) segment to obtain Diels–Alder polyadducts. Polyadducts were then aromatized and imidized (i.e. cyclized) through carboxylic and amide groups to afford polyimides. Synthesized polyadducts and polyimides were characterized by elemental analysis, spectral features, the number of average molecular weight (Mn) and thermal analysis. The ‘in situ’ glass fiber reinforced composites were prepared and characterized by mechanical, electrical, and chemical properties. These properties were compared with the other reported polyimides. All the composites showed good mechanical and electrical properties and good resistance to organic solvents and mineral acids.

Keywords: Diels-Alder reaction, bisfuran, bismaleimides, polyimide

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Authors: Shimaa M. Elsaeed, Reem K. Farag, Ibrahim M. Nassar

Abstract:

Hydrogel conductive polymer nanocomposite fabricated via in-situ polymerization of polyaniline (PANI) inside thermosensitive hydrogels based on hydroxy ethyl meth acrylate (HEMA) copolymer with 2-acrylamido-2-methyl propane sulfonic acid (AMPS). SEM micrographs show the nanometric size of the conductive material (polyaniline, PANI) dispersed in the hydrogel matrix. The swelling parameters of hydrogel are measured. The incorporation of PANI improves the mechanical properties and swelling up to 30,000% without breaking. X-ray diffraction shows that typical polyaniline crystallization is formed in composite, which is advantageous to increase the electrical conductivity of the composite hydrogel. Open-circuit voltage (I-V) curve fill factor of the highest photo-conversion efficiency and enhanced to use in solar cell.

Keywords: hydrogel, solar cell, conductive polymer, nanocomposite

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Authors: Nouf Alharbi

Abstract:

The electrospray deposition technique became an important method that enables fragile, nonvolatile molecules to be deposited in situ in high vacuum environments. Furthermore, it is considered one of the ways to close the gap between basic surface science and molecular engineering, which represents a gradual change in the range of scientist research. Also, this paper talked about one of the most important techniques that have been developed and aimed for helping to further develop and characterize the electrospray by providing data collected using an image charge detection instrument. Image charge detection mass spectrometry (CDMS) is used to measure speed and charge distributions of the molecular ions. As well as, some data has been included using SIMION simulation to simulate the energies and masses of the molecular ions through the system in order to refine the mass-selection process.

Keywords: charge, deposition, electrospray, image, ions, molecules, SIMION

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Authors: Haythem Barrak, Gaetan Laroche, Adel M’nif, Ahmed Hichem Hamzaoui

Abstract:

The use of semiconductor oxides, as chemical or biological, requires their functionalization with appropriate dependent molecules of the substance to be detected. generally, the support materials used are TiO2 and SiO2. In the present work, we used zinc oxide (ZnO) known for its interesting physical properties. The synthesis of nano scale ZnO was performed by co-precipitation at low temperature (60 ° C).To our knowledge, the obtaining of this material at this temperature was carried out for the first time. This shows the low cost of this operation. On the other hand, the surface functionalization of ZnO was performed with (3-aminopropyl) triethoxysilane (APTES) by using a specific method using ethanol for the first time. In addition, the duration of this stage is very low compared to literature. The samples obtained were analyzed by XRD, TEM, DLS, FTIR, and TGA shows that XPS that the operation of grafting of APTES on our support was carried out with success.

Keywords: functionalization, nanoparticle, ZnO, APTES, caractérisation

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Authors: Endalkachew Abebe Kebede, Bojin Bojinov, Andon Vasilev Andonov, Orhan Dengiz

Abstract:

Remote sensing has a potential application in assessing and monitoring the plants' biophysical properties using the spectral responses of plants and soils within the electromagnetic spectrum. However, only a few reports compare the performance of different remote sensing sensors against in-situ field spectral measurement. The current study assessed the potential applications of open data source satellite images (Sentinel 2 and Landsat 9) in estimating the biophysical properties of the wheat crop on a study farm found in the village of OvchaMogila. A Landsat 9 (30 m resolution) and Sentinel-2 (10 m resolution) satellite images with less than 10% cloud cover have been extracted from the open data sources for the period of December 2021 to April 2022. An Unmanned Aerial Vehicle (UAV) has been used to capture the spectral response of plant leaves. In addition, SpectraVue 710s Leaf Spectrometer was used to measure the spectral response of the crop in April at five different locations within the same field. The ten most common vegetation indices have been selected and calculated based on the reflectance wavelength range of remote sensing tools used. The soil samples have been collected in eight different locations within the farm plot. The different physicochemical properties of the soil (pH, texture, N, P₂O₅, and K₂O) have been analyzed in the laboratory. The finer resolution images from the UAV and the Leaf Spectrometer have been used to validate the satellite images. The performance of different sensors has been compared based on the measured leaf spectral response and the extracted vegetation indices using the five sampling points. A scatter plot with the coefficient of determination (R2) and Root Mean Square Error (RMSE) and the correlation (r) matrix prepared using the corr and heatmap python libraries have been used for comparing the performance of Sentinel 2 and Landsat 9 VIs compared to the drone and SpectraVue 710s spectrophotometer. The soil analysis revealed the study farm plot is slightly alkaline (8.4 to 8.52). The soil texture of the study farm is dominantly Clay and Clay Loam.The vegetation indices (VIs) increased linearly with the growth of the plant. Both the scatter plot and the correlation matrix showed that Sentinel 2 vegetation indices have a relatively better correlation with the vegetation indices of the Buteo dronecompared to the Landsat 9. The Landsat 9 vegetation indices somewhat align better with the leaf spectrometer. Generally, the Sentinel 2 showed a better performance than the Landsat 9. Further study with enough field spectral sampling and repeated UAV imaging is required to improve the quality of the current study.

Keywords: landsat 9, leaf spectrometer, sentinel 2, UAV

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Authors: Rio Hirakawa, Christian Gundlach, Sven Hartwig

Abstract:

In recent years, the use of aluminium has further expanded and is expected to replace steel in the future as vehicles become lighter and more recyclable in order to reduce greenhouse gas (GHG) emissions and improve fuel economy. In line with this, structures and components are becoming increasingly multi-material, with different materials, including aluminium, being used in combination to improve mechanical utility and performance. A common method of assembling dissimilar materials is mechanical fastening, but it has several drawbacks, such as increased manufacturing processes and the influence of substrate-specific mechanical properties. Adhesive bonding and fusion bonding are methods that overcome the above disadvantages. In these two joining methods, surface pre-treatment of the substrate is always necessary to ensure the strength and durability of the joint. Previous studies have shown that laser surface treatment improves the strength and durability of the joint. Yan et al. showed that laser surface treatment of aluminium alloys changes α-Al2O3 in the oxide layer to γ-Al2O3. As γ-Al2O3 has a large specific surface area, is very porous and chemically active, laser-treated aluminium surfaces are expected to undergo physico-chemical changes over time and adsorb moisture and organic substances from the air or storage atmosphere. The impurities accumulated on the laser-treated surface may be released at the adhesive and bonding interface by the heat input to the bonding system during the joining phase, affecting the strength and durability of the joint. However, only a few studies have discussed the effect of such storage periods on laser-treated surfaces. This paper, therefore, investigates the ageing of laser-treated aluminium alloy surfaces through thermal analysis, electrochemical analysis and microstructural observations.AlMg3 of 0.5 mm and 1.5 mm thickness was cut using a water-jet cutting machine, cleaned and degreased with isopropanol and surface pre-treated with a pulsed fibre laser at 1060 nm wavelength, 70 W maximum power and 55 kHz repetition frequency. The aluminium surface was then analysed using SEM, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR) and cyclic voltammetry (CV) after storage in air for various periods ranging from one day to several months TGA and FTIR analysed impurities adsorbed on the aluminium surface, while CV revealed changes in the true electrochemically active surface area. SEM also revealed visual changes on the treated surface. In summary, the changes in the laser-treated aluminium surface with storage time were investigated, and the final results were used to determine the appropriate storage period.

Keywords: laser surface treatment, pre-treatment, adhesion, bonding, corrosion, durability, dissimilar material interface, automotive, aluminium alloys

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