Search results for: silver nanoparticles synthesis

Authors: Kausar Harun, Ahmad Azmin Mohamad

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Zinc oxide (ZnO) has been extensively used in optoelectronic devices, with recent interest as photoanode material in dye-sensitize solar cell. Numerous methods employed to experimentally synthesized ZnO, while some are theoretically-modeled. Both approaches provide information on ZnO properties, but theoretical calculation proved to be more accurate and timely effective. Thus, integration between these two methods is essential to intimately resemble the properties of synthesized ZnO. In this study, experimentally-grown ZnO nanoparticles were prepared by sol-gel storage method with zinc acetate dihydrate and methanol as precursor and solvent. A 1 M sodium hydroxide (NaOH) solution was used as stabilizer. The optimum time to produce ZnO nanoparticles were recorded as 12 hours. Phase and structural analysis showed that single phase ZnO produced with wurtzite hexagonal structure. Further work on quantitative analysis was done via Rietveld-refinement method to obtain structural and crystallite parameter such as lattice dimensions, space group, and atomic coordination. The lattice dimensions were a=b=3.2498Å and c=5.2068Å which were later used as main input in first-principles calculations. By applying density-functional theory (DFT) embedded in CASTEP computer code, the structure of synthesized ZnO was built and optimized using several exchange-correlation functionals. The generalized-gradient approximation functional with Perdew-Burke-Ernzerhof and Hubbard U corrections (GGA-PBE+U) showed the structure with lowest energy and lattice deviations. In this study, emphasize also given to the modification of valence electron energy level to overcome the underestimation in DFT calculation. Both Zn and O valance energy were fixed at Ud=8.3 eV and Up=7.3 eV, respectively. Hence, the following electronic and optical properties of synthesized ZnO were calculated based on GGA-PBE+U functional within ultrasoft-pseudopotential method. In conclusion, the incorporation of Rietveld analysis into first-principles calculation was valid as the resulting properties were comparable with those reported in literature. The time taken to evaluate certain properties via physical testing was then eliminated as the simulation could be done through computational method.

Keywords: density functional theory, first-principles, Rietveld-refinement, ZnO nanoparticles

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Authors: Satam Alotibi, Haya A. Al-Sunaidi, Almaymunah M. AlRoibah, Zahraa H. Al-Omaran, Mohammed Alyami, Fatehia S. Alhakami, Abdellah Kaiba, Mazen Alshaaer, Talal F. Qahtan

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This research study presents a novel approach to harnessing the potential of natural geopolymer in conjunction with TiO₂ nanoparticles (TiO₂ NPs) for the development of highly efficient photocatalytic materials for water decontamination. The study begins with the formulation of a geopolymer paste derived from natural sources, which is subsequently applied as a coating on glass substrates and allowed to air-dry at room temperature. The result is a series of geopolymer-coated glass films, serving as the foundation for further experimentation. To enhance the photocatalytic capabilities of these films, a critical step involves immersing them in a suspension of TiO₂ nanoparticles (TiO₂ NPs) in water for varying durations. This immersion process yields geopolymer-loaded TiO₂ NPs films with varying concentrations, setting the stage for comprehensive characterization and analysis. A range of advanced analytical techniques, including UV-Vis spectroscopy, Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM), were meticulously employed to assess the structural, morphological, and chemical properties of the geopolymer-based TiO₂ films. These analyses provided invaluable insights into the materials' composition and surface characteristics. The culmination of this research effort sees the geopolymer-based TiO₂ films being repurposed as immobilized photocatalytic reactors for water decontamination under natural sunlight irradiation. Remarkably, the results revealed exceptional photocatalytic performance that exceeded the capabilities of conventional TiO₂-based photocatalysts. This breakthrough underscores the significant potential of natural geopolymer as a versatile and highly effective matrix for enhancing the photocatalytic efficiency of TiO₂ nanoparticles in water treatment applications. In summary, this study represents a significant advancement in the quest for sustainable and efficient photocatalytic materials for environmental remediation. By harnessing the synergistic effects of natural geopolymer and TiO₂ nanoparticles, these geopolymer-based films exhibit outstanding promise in addressing water decontamination challenges and contribute to the development of eco-friendly solutions for a cleaner and healthier environment.

Keywords: geopolymer, TiO2 nanoparticles, photocatalytic materials, water decontamination, sustainable remediation

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Authors: Meksem Nabila, Bordjiba Ouahiba, Meraghni Messaouda, Meksem Amara Leila, Djebar Mohhamed Reda

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The problems of protection of the cultures are being more and more important that they interest great number of farmers and scientists because of the excessive use of the organic phytosanitary products of synthesis that causes fatal damages on the environment. To reduce the inconveniences produced by these pesticides, the use of "biopesticides" originated from plants could be an alternative. The aim of this work is the valuation of a botanical species: Eucalyptus camaldulensis from Northeastern Algeria which extracts are supposed to have an antimicrobial activity, similar to pesticides. The extraction of secondary metabolites from the leaves of E. camaldulensis was realized using methanol and water, and measurements of total polyphenols were made by spectrometric method. Determination of the antimicrobial activity of the extracts at issue was realized in vitro on phyto-pathogenic fungal and bacterial stumps. Tests of comparison were included in the essays by using the chemical pesticidal products of synthesis. The obtained results show that the plant contains polyphenols with an efficiency mattering of the order of 22 %. These polyphenols have a strong fungicidal and bactericidal pesticidal activity against various microbial stumps and the values of the zones of inhibition are more important compared with that obtained in the presence of the chemicals of synthesis (fungicide).

Keywords: eucalyptus camaldulensis, biopesticide, polyphenols, antimicrobial activity

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Authors: Qinglei Liu, Ali Charkhesht, Tiva Sharifi, Ashkan Bahadoran

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Graphene sheets are promising nanoscale building blocks as a support material for the dispersion of nanoparticles. In this work, a solvothermal method employed to directly grow Co1-xZnxFe2O4 ferrite nanospheres on graphene oxide support that is subsequently reduced to graphene. The samples morphology, structure and crystallography were investigated using field-emission scanning electron microscopy (FE-SEM) and powder X-ray diffraction (XRD). The influences of the Zn2+ content on photocatalytic activity, electrical conductivity and magnetic property of the samples are also investigated. The results showed that Co1-x Znx Fe2 O4 nanoparticles are dispersed on graphene sheets and obtained nanocomposites are soft magnetic materials. In addition the samples showed excellent photocatalytic activity under visible light irradiation.

Keywords: reduced graphene oxide, ferrite, magnetic nanocomposite, photocatalytic activity, solvothermal method

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Authors: Dionisios Panagiotaras, Dimitrios Papoulis, Elias Stathatos

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Microfibrous palygorskite and tubular halloysite clay mineral combined with nanocrystalline TiO2 are incorporating in the preparation of nanocomposite films on glass substrates via sol-gel route at 450 °C. The synthesis is employing nonionic surfactant molecule as pore directing agent along with acetic acid-based sol-gel route without addition of water molecules. Drying and thermal treatment of composite films ensure elimination of organic material lead to the formation of TiO2 nanoparticles homogeneously distributed on the palygorskite or halloysite surfaces. Nanocomposite films without cracks of active anatase crystal phase on palygorskite and halloysite surfaces are characterized by microscopy techniques, UV-Vis spectroscopy, and porosimetry methods in order to examine their structural properties. The composite palygorskite-TiO2 and halloysite-TiO2 films with variable quantities of palygorskite and halloysite were tested as photocatalysts in the photo-oxidation of Basic Blue 41 azo dye in water. These nanocomposite films proved to be most promising photocatalysts and highly effective to dye’s decoloration in spite of small amount of palygorskite -TiO2 or halloysite- TiO2 catalyst immobilized onto glass substrates mainly due to the high surface area and uniform distribution of TiO2 on clay minerals avoiding aggregation.

Keywords: halloysite, palygorskite, photocatalysis, titanium dioxide

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Authors: A. Julio, R. Caparica, S. Costa Lima, S. Reis, J. G. Costa, P. Fonte, T. Santos De Almeida

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The Mycobacterium leprae causes a chronic and infectious disease called leprosy, which the most common symptoms are peripheral neuropathy and deformation of several parts of the body. The pharmacological treatment of leprosy is a combined therapy with three different drugs, rifampicin, clofazimine, and dapsone. However, clofazimine and dapsone have poor solubility in water and also low bioavailability. Thus, it is crucial to develop strategies to overcome such drawbacks. The use of ionic liquids (ILs) may be a strategy to overcome the low solubility since they have been used as solubility promoters. ILs are salts, liquid below 100 ºC or even at room temperature, that may be placed in water, oils or hydroalcoholic solutions. Another approach may be the encapsulation of drugs into polymeric nanoparticles, which improves their bioavailability. In this study, two different classes of ILs were used, the imidazole- and the choline-based ionic liquids, as solubility enhancers of the poorly soluble antileprotic drugs. Thus, after the solubility studies, it was developed IL-PLGA nanoparticles hybrid systems to deliver such drugs. First of all, the solubility studies of clofazimine and dapsone were performed in water and in water: IL mixtures, at ILs concentrations where cell viability is maintained, at room temperature for 72 hours. For both drugs, it was observed an improvement on the drug solubility and [Cho][Phe] showed to be the best solubility enhancer, especially for clofazimine, where it was observed a 10-fold improvement. Later, it was produced nanoparticles, with a polymeric matrix of poly(lactic-co-glycolic acid) (PLGA) 75:25, by a modified solvent-evaporation W/O/W double emulsion technique in the presence of [Cho][Phe]. Thus, the inner phase was an aqueous solution of 0.2 % (v/v) of the above IL with each drug to its maximum solubility determined on the previous study. After the production, the nanosystem hybrid was physicochemically characterized. The produced nanoparticles had a diameter of around 580 nm and 640 nm, for clofazimine and dapsone, respectively. Regarding the polydispersity index, it was in agreement of the recommended value of this parameter for drug delivery systems (around 0.3). The association efficiency (AE) of the developed hybrid nanosystems demonstrated promising AE values for both drugs, given their low solubility (64.0 ± 4.0 % for clofazimine and 58.6 ± 10.0 % for dapsone), that prospects the capacity of these delivery systems to enhance the bioavailability and loading of clofazimine and dapsone. Overall, the study achievement may signify an upgrading of the patient’s quality of life, since it may mean a change in the therapeutic scheme, not requiring doses of drug so high to obtain a therapeutic effect. The authors would like to thank Fundação para a Ciência e a Tecnologia, Portugal (FCT/MCTES (PIDDAC), UID/DTP/04567/2016-CBIOS/PRUID/BI2/2018).

Keywords: ionic liquids, ionic liquids-PLGA nanoparticles hybrid systems, leprosy treatment, solubility

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Authors: Chia-Ling Li

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The scope of this article includes the production of 10,000 metric tons of non-phthalate per annum. The production process will include hydrogenation, separation, purification, and recycling of unprocessed feedstock. Based on experimental data, conversion and selectivity were chosen as reaction model parameters. The synthesis and separation processes of non-phthalate and phthalate were established by using Aspen Plus software. The article will be divided into six parts: estimation of physical properties, integration of production processes, purification case study, utility consumption, economic feasibility study and identification of bottlenecks. The purities of products was higher than 99.9 wt. %. Process parameters have important guiding significance to the commercialization of hydrogenation of phthalate.

Keywords: economic analysis, hydrogenation, non-phthalate, process simulation

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Authors: S. Ghanaraja, Subrata Ray, S. K. Nath

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Particle reinforced Metal Matrix Composite (MMC) succeeds in synergizing the metallic matrix with ceramic particle reinforcements to result in improved strength, particularly at elevated temperatures, but adversely it affects the ductility of the matrix because of agglomeration and porosity. The present study investigates the outcome of tensile properties in a cast and hot forged composite reinforced simultaneously with coarse and fine particles. Nano-sized alumina particles have been generated by milling mixture of aluminum and manganese dioxide powders. Milled particles after drying are added to molten metal and the resulting slurry is cast. The microstructure of the composites shows good distribution of both the size categories of particles without significant clustering. The presence of nanoparticles along with coarser particles in a composite improves both strength and ductility considerably. Delay in debonding of coarser particles to higher stress is due to reduced mismatch in extension caused by increased strain hardening in presence of the nanoparticles. However, higher addition of powder mix beyond a limit results in deterioration of mechanical properties, possibly due to clustering of nanoparticles. The porosity in cast composite generally increases with the increasing addition of powder mix as observed during process and on forging it has got reduced. The base alloy and nanocomposites show improvement in flow stress which could be attributed to lowering of porosity and grain refinement as a consequence of forging.

Keywords: aluminium, alumina, nano-particle reinforced composites, porosity

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Authors: Dipranjan Laha, Parimal Karmakar

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Metal oxide nanoparticles are well known to generate oxidative stress and deregulate normal cellular activities. Among these, transition metals copper oxide nanoparticles (CuO NPs) are more compelling than others and able to modulate different cellular responses. In this work, we have synthesized and characterized CuO NPs by various biophysical methods. These CuO NPs (~30 nm) induce autophagy in human breast cancer cell line, MCF7 in a time and dose-dependent manner. Cellular autophagy was tested by MDC staining, induction of green fluorescent protein light chain 3 (GFP-LC3B) foci by confocal microscopy, transfection of pBABE-puro mCherry-EGFP-LC3B plasmid and western blotting of autophagy marker proteins LC3B, beclin1, and ATG5. Further, inhibition of autophagy by 3-Methyladenine (3-MA) decreased LD50 doses of CuO NPs. Such cell death was associated with the induction of apoptosis as revealed by FACS analysis, cleavage of PARP, dephosphorylation of Bad and increased cleavage product of caspase3. siRNA-mediated inhibition of autophagy-related gene beclin1 also demonstrated similar results. Finally, induction of apoptosis by 3-MA in CuO NPs treated cells were observed by TEM. This study indicates that CuO NPs are a potent inducer of autophagy which may be a cellular defense against the CuO NPs mediated toxicity and inhibition of autophagy switches the cellular response into apoptosis. A combination of CuO NPs with the autophagy inhibitor is essential to induce apoptosis in breast cancer cells. Acknowledgments: The authors would like to acknowledge for financial support for this research work to the Department of Biotechnology (No. BT/PR14661/NNT/28/494/2010), Government of India.

Keywords: nanoparticle, autophagy, apoptosis, siRNA-mediated inhibition

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Authors: Abdelkader Hadjoudja, Hajar Bouazza

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The PLD/CPLD devices are widely used for logic synthesis since several decades. Based on sum of product terms (PTs) architecture, the PLD/CPLD offer a high degree of flexibility to support various application requirements. They are suitable for large combinational logic, finite state machines as well as intensive I/O designs. CPLDs offer very predictable timing characteristics and are therefore ideal for critical control applications. This paper describes how the logic synthesis techniques, such as 1) XOR detection, 2) logic doubling, 3) complement of a Boolean function are combined, applied and used to optimize the CPLDs devices architecture that is based on PAL-like macrocells. Our goal is to use these techniques for minimizing the number of macrocells required to implement a circuit and minimize the delay of mapped circuit.

Keywords: CPLD, doubling, optimization, XOR

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Authors: S. Aouabdi, M. Taibi

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The supervision of chemical processes is the subject of increased development because of the increasing demands on reliability and safety. An important aspect of the safe operation of chemical process is the earlier detection of (process faults or other special events) and the location and removal of the factors causing such events, than is possible by conventional limit and trend checks. With the aid of process models, estimation and decision methods it is possible to also monitor hundreds of variables in a single operating unit, and these variables may be recorded hundreds or thousands of times per day. In the absence of appropriate processing method, only limited information can be extracted from these data. Hence, a tool is required that can project the high-dimensional process space into a low-dimensional space amenable to direct visualization, and that can also identify key variables and important features of the data. Our contribution based on powerful techniques for development of a new monitoring method based on multi-scale entropy MSE in order to characterize the behaviour of the concentrations of different gases present in synthesis and soft sensor based on PCA is applied to estimate these variables.

Keywords: ammonia synthesis, concentrations of different gases, soft sensor, multi-scale entropy, multivarite statistics

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Authors: Rafat M. Mohareb

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Several D-ring alkylated estrone analogues display exceptionally high affinity for estrogen receptors. In particular, compounds in which an E-ring is formed are known to be involved in the inhibition of steroidogenic enzymes. Such compounds also have an effect on steroid dehydrogenase activity and the ability to inhibit the detrimental action of the steroid sulfatase enzyme. Generally, E-ring extended steroids have been accessed by modification of the C17-ketone in the D-ring by either arylimine or oximino formation, addition of a carbon nucleophile or hydrazone formation. Other approaches have included ketone reduction, silyl enol ether formation or ring-closing metathesis (giving five- or six-membered E-rings). Chemical modification of the steroid D-ring provides a way to alter the functional groups, sizes and stereochemistry of the D-ring, and numerous structure-activity relationships have been established by such synthetic alterations. Steroids bearing heterocycles fused to the D-ring of the steroid nucleus have been of pharmaceutical interest. In the present paper, we report on the efficient synthesis of estrone possessing pyran, pyrimidine and thiazole ring systems. This study focused on the synthesis and biochemical evaluation of newly synthesized heterocyclic compounds which were then subjected through inhibitory evaluations towards human cancer and normal cell lines.

Keywords: estrone, heterocyclization, cytotoxicity, biomedicine

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Authors: Khamis Al Kalbani

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The effects of a uniform heat source position on the heat transfer flow inside an inclined square enclosure filled with different types of nanofluids having various shapes of the nanoparticles are investigated numerically following one component thermal equilibrium model. The effects of the Brownian diffusion of the nanoparticles, magnetic field intensity and orientation are taken into consideration in nanofluid modeling. The heat source is placed in the middle of a wall of the enclosure while the opposite wall of it is kept at different temperature. The other walls of the enclosure are kept insulated. The results indicate that the heat source position significantly controls the heat transfer rates of the nanofluids. The distributions of the average heat transfer rates varying the position of the heat source with respect to the geometry inclination angle are calculated for the first time. The outcomes of the present research may be helpful for designing solar thermal collectors, radiators, building insulators and advanced cooling of a nuclear system.

Keywords: heat source, inclined, square enclosure, nanofluids

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Authors: L. N. Shubha, P. Madhusudana Rao

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The Polyaniline / Copper Oxide(PANI / CuO) nanocomposite was prepared by solution mixing of prepared Polyaniline and copper Oxide in Dimethyl sulfoxide (DMSO). The synthesis involved the formation of dark green colored Polyaniline-Copper Oxide nanocomposite. The synthesized polymer nano composites were characterized by XRD, FTIR, SEM and UV-Visible Spectroscopy. The characteristic peaks in XRD, FTIR and UV-Visible spectra confirmed the presence of CuO in the polymer structure. SEM analysis revealed formation of PANI/CuO nano composite The D.C. conductivity measurements were performed using two probe method for various temperatures.

Keywords: polyaniline/copper oxide (PANI/CuO) nanocomposite, XRD, SEM, FTIRand DC- conductivity, UV-visible spectra

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Authors: Gyati Shilakari Asthana, Abhay Asthana

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Purpose: The therapeutic potential of oligonucleotide (ODN) is primarily dependent upon its safe and efficient delivery to specific cells overcoming degradation and maximizing cellular uptake in vivo. The present study is focused to design low molecular weight chitosan nanoconstructs to meet the requirements of safe and effectual delivery of ODNs. LMW-chitosan is a biodegradable, water soluble, biocompatible polymer and is useful as a non-viral vector for gene delivery due to its better stability in water. Methods: LMW chitosan ODN nanoparticles (CHODN NPs) were formulated by self assembled method using various N/P ratios (moles ratio of amine groups of CH to phosphate moieties of ODNs; 0.5:1, 1:1, 3:1, 5:1 and 7:1) of CH to ODN. The developed CHODN NPs were evaluated with respect to gel retardation assay, particle size, zeta potential and cytotoxicity and transfection efficiency. Results: Complete complexation of CH/ODN was achieved at the charge ratio of 0.5:1 or above and CHODN NPs displayed resistance against DNase I. On increasing the N/P ratio of CH/ODN, particle size of the NPs decreased whereas zeta potential (ZV) value increased. No significant toxicity was observed at all CH concentrations. The transfection efficiency was increased on increasing N/P ratio from 1:1 to 3:1, whereas it was decreased with further increment in N/P ratio upto 7:1. Maximum transfection of CHODN NPs with both the cell lines (Raw 267.4 cells and Hela cells) was achieved at N/P ratio of 3:1. The results suggest that transfection efficiency of CHODN NPs is dependent on N/P ratio. Conclusion: Thus the present study states that LMW chitosan nanoparticulate carriers would be acceptable choice to improve transfection efficiency in vitro as well as in vivo delivery of oligonucleotide.

Keywords: LMW-chitosan, chitosan nanoparticles, biocompatibility, cytotoxicity study, transfection efficiency, oligonucleotide

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Authors: Hossein Tavallali, Mohammad Ali Karimi, Gohar Deilamy-Rad

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The proposed method for speciation, preconcentration and determination of Fe(II) and Fe(III) in pharmaceutical products was developed using of alumina-coated magnetite nanoparticles (Fe₃O₄/Al₂O₃ NPs) as solid phase extraction (SPE) sorbent in magnetic mixed hemimicell solid phase extraction (MMHSPE) technique followed by flame atomic absorption spectrometry analysis. The procedure is based on complexation of Fe(II) with 1, 10-phenanthroline (OP) as complexing reagent for Fe(II) that immobilized on the modified Fe₃O₄/Al₂O₃ NPs. The extraction and concentration process for pharmaceutical sample was carried out in a single step by mixing the extraction solvent, magnetic adsorbents under ultrasonic action. Then, the adsorbents were isolated from the complicated matrix easily with an external magnetic field. Fe(III) ions determined after facility reduced to Fe(II) by added a proper reduction agent to sample solutions. Compared with traditional methods, the MMHSPE method simplified the operation procedure and reduced the analysis time. Various influencing parameters on the speciation and preconcentration of trace iron, such as pH, sample volume, amount of sorbent, type and concentration of eluent, were studied. Under the optimized operating conditions, the preconcentration factor of the modified nano magnetite for Fe(II) 167 sample was obtained. The detection limits and linear range of this method for iron were 1.0 and 9.0 - 175 ng.mL⁻¹, respectively. Also the relative standard deviation for five replicate determinations of 30.00 ng.mL^-1 Fe²⁺ was 2.3%.

Keywords: Alumina-Coated magnetite nanoparticles, Magnetic Mixed Hemimicell Solid-Phase Extraction, Fe(ΙΙ) and Fe(ΙΙΙ), pharmaceutical sample

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Authors: Olga Shapovalova, Vladimir Vinogradov

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Among many different sol – gel matrices only alumina can be successfully parenteral injected in the human body. And this is not surprising, because boehmite (aluminium oxyhydroxide) is the metal oxide approved by FDA and EMA for intravenous and intramuscular administrations, and also has been using for a longtime as adjuvant for producing of many modern vaccines. In our earlier study, it has been shown, that denaturation temperature of enzymes entrapped in sol-gel boehmite matrix increases for 30 – 60 °С with preserving of initial activity. It makes such matrices more attractive for long-term storage of non-stable drugs. In current work we present ultrasound-assisted sol-gel synthesis of nano-boehmite. This method provides bio-friendly, very stable, highly homogeneous alumina sol with using only water and aluminium isopropoxide as a precursor. Many parameters of the synthesis were studied in details: time of ultrasound treatment, US frequency, surface area, pore and nanoparticle size, zeta potential and others. Here we investigated the dependence of stability of colloidal sols and textural properties of the final composites as a function of the time of ultrasonic treatment. Chosen ultrasonic treatment time was between 30 and 180 minutes. Surface area, average pore diameter and total pore volume of the final composites were measured by surface and pore size analyzer Nova 1200 Quntachrome. It was shown that the matrices with ultrasonic treatment time equal to 90 minutes have the biggest surface area 431 ± 24 m2/g. On the other had such matrices have a smaller stability in comparison with the samples with ultrasonic treatment time equal to 120 minutes that have the surface area 390 ± 21 m2/g. It was shown that the stable sols could be formed only after 120 minutes of ultrasonic treatment, otherwise the white precipitate of boehmite is formed. We conclude that the optimal ultrasonic treatment time is 120 minutes.

Keywords: boehmite matrix, stabilisation, ultrasound-assisted sol-gel synthesis

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Authors: Koilpitchai Sivamuthuraman, Venkitasamy Kesavan

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3-substituted 3-amino-2-oxindole skeleton bearing adjacent tetrasubstituted stereogenic centers is of great importance because of these heterocyclic motifs possess a wide range of pharmacological activity. The catalytic asymmetric construction of multi functionalised heterocyclic compound with adjacent tetrasubstituted stereocenters is one of the most difficult tasks in organic synthesis. To date, the most straightforward methodologies have been developed for synthesis of chiral 3-substituted 3-amino-2-oxindoles through the addition of carbon nucleophiles to isatin-derived ketimines. However, only a few successful examples have been described for the assembly of vicinal tetrasubstituted stereocenters using isatin derived ketimines as electrophiles. On the other hand, 2,2-Disubstituted benzofuran-3(2H)-ones and related frameworks are characteristic of a quaternary stereogenic center at C2 position present in quite a number of natural products and bioactive Molecules.Despite the intensive efforts devoted for the construction of 2,2-Disubstituted Benzofuran-3[2H]-one, there are only a few asymmetric methods such as organocatalytic Michael addition and enantioselective halogenations were reported till now. Due to the biological importance of oxindole and benzofuran-3-one, it is proposed here with the synthesis of hybrid molecule containing tetrasubstituted stereo centers through asymmetric organocatalysis. The addition of 2-substituted Benzofuran-3-one(1a) to isatin-derived ketimines(2a) using a bifunctional organocatalyst(catalyst IV or V), leading to chiral heterocyclic compounds containing both 3-amino 2-oxindole and benzofurn-3-one bearing vicinal quaternary stereocenters with good yields and excellent enantioselectivity. The present study extends the scope of the catalytic asymmetric Mannich reaction with isatin-derived ketimines, providing a new class of amino oxindole derivatives having benzofuran-3-one.

Keywords: asymmetric synthesis, benzofuran-3-one, isatin-derived ketimines, quaternary stereocenters

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Authors: Jing Lin, Zou Yiming, Goei Ronn, Li Yun, Amanda Ong Jiamin, Alfred Tok Iing Yoong

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High-entropy alloy (HEA) coatings comprise multiple (five or more) principal elements that give superior mechanical, electrical, and thermal properties. However, the current synthesis methods of HEA coating still face huge challenges in facile and controllable preparation, as well as conformal integration, which seriously restricts their potential applications. Herein, we report a controllable synthesis of conformal quinary HEA coating consisting of noble metals (Rh, Ru, Ir, Pt, and Pd) by using the atomic layer deposition (ALD) with a post-annealing approach. This approach realizes low temperature (below 200 °C), precise control (nanoscale), and conformal synthesis (over complex substrates) of HEA coating. Furthermore, the resulting quinary HEA coating shows promising potential as a platform for catalysis, exhibiting substantially enhanced electrocatalytic hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) performances as compared to other noble metal-based structures such as single metal coating or multi-layered metal composites.

Keywords: high-entropy alloy, thin-film, catalysis, water splitting, atomic layer deposition

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Authors: Rama Bhargava, Surabhi Nishad

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The infusion of nanofluids has dramatically enhanced the heat-carrying capacity of the fluids, applicable to many engineering and medical process where the temperature below freezing is required. Cryosurgery is an efficient therapy for the treatment of cancer, but sometimes the excessive cooling may harm the nearby healthy cells. Efforts are therefore done to develop a model which can cause to generate the low temperature as required. In the present study, a mathematical model is developed based on the bioheat transfer equation to simulate the heat transfer from the probe on a tumor (with irregular domain) using the hybrid technique consisting of element free Galerkin method with αα-family of approximation. The probe is loaded will nano-particles. The effects of different nanoparticles, namely Al₂O₃, Fe₃O₄, Au on the heat-producing rate, is obtained. It is observed that the temperature can be brought to (60°C)-(-30°C) at a faster freezing rate on the infusion of different nanoparticles. Besides increasing the freezing rate, the volume of the nanoparticle can also control the size and growth of ice crystals formed during the freezing process. The study is also made to find the time required to achieve the desired temperature. The problem is further extended for multi tumors of different shapes and sizes. The irregular shape of the frozen domain and the direction of ice growth are very sensitive issues, posing a challenge for simulation. The Meshfree method has been one of the accurate methods in such problems as a domain is naturally irregular. The discretization is done using the nodes only. MLS approximation is taken in order to generate the shape functions. Sufficiently accurate results are obtained.

Keywords: cryosurgery, EFGM, hybrid, nanoparticles

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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: H. Aldewachi, M. Hines, M. McCulloch, N. Woodroofe, P. Gardiner

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DPP-IV is an enzyme whose expression is affected in a variety of diseases, therefore, has been identified as possible diagnostic or prognostic marker for various tumours, immunological, inflammatory, neuroendocrine, and viral diseases. Recently, DPP-IV enzyme has been identified as a novel target for type II diabetes treatment where the enzyme is involved. There is, therefore, a need to develop sensitive and specific methods that can be easily deployed for the screening of the enzyme either as a tool for drug screening or disease marker in biological samples. A variety of assays have been introduced for the determination of DPP-IV enzyme activity using chromogenic and fluorogenic substrates, nevertheless these assays either lack the required sensitivity especially in inhibited enzyme samples or displays low water solubility implying difficulty for use in vivo samples in addition to labour and time-consuming sample preparation. In this study, novel strategies based on exploiting the high extinction coefficient of gold nanoparticles (GNPs) are investigated in order to develop fast, specific and reliable enzymatic assay by investigating synthetic peptide sequences containing a DPP IV cleavage site and coupling them to GNPs. The DPP IV could be detected by colorimetric response of peptide capped GNPs (P-GNPS) that could be monitored by a UV-visible spectrophotometer or even naked eyes, and the detection limit could reach 0.01 unit/ml. The P-GNPs, when subjected to DPP IV, showed excellent selectivity compared to other proteins (thrombin and human serum albumin) , which led to prominent colour change. This provided a simple and effective colorimetric sensor for on-site and real-time detection of DPP IV.

Keywords: gold nanoparticles, synthetic peptides, colorimetric detection, DPP-IV enzyme

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Authors: Mohamed Amine Ben Abdallah, Imed Khemili, Nizar Aifaoui

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This work denotes an insight into dynamic synthesis of multibody systems. A set of mechanism parameters design variable are synthetized based on a desired mechanism response, such as, velocity, acceleration and bodies deformations. Moreover, knowing the work space, for a robot, and mechanism response allow defining optimal parameters mechanism handling with the desired target response. To this end, evolutionary genetic algorithm has been deployed. A demonstrative example for imperfect mechanism has been treated, mainly, a slider crank mechanism with a flexible connecting rod. The transversal deflection of the connecting rod has been chosen as response to identify the mechanism design parameters.

Keywords: dynamic response, evolutionary genetic algorithm, flexible bodies, optimization

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Authors: Najla M. Salkho, Vinod Paul, Pierre Kawak, Rute F. Vitor, Ana M. Martin, Nahid Awad, Mohammad Al Sayah, Ghaleb A. Husseini

Abstract:

Liposomes are popular lipid bilayer nanoparticles that are highly efficient in encapsulating both hydrophilic and hydrophobic therapeutic drugs. Liposomes promote a low risk controlled release of the drug avoiding the side effects of the conventional chemotherapy. One of the great potentials of liposomes is the ability to attach a wide range of ligands to their surface producing ligand-mediated active targeting of cancer tumour with limited adverse off-target effects. Ultrasound can also aid in the controlled and specified release of the drug from the liposomes by breaking it apart and releasing the drug in the specific location where the ultrasound is applied. Our research focuses on the synthesis of PEGylated liposomes (contain poly-ethylene glycol) encapsulated with the model drug calcein and studying the effect of low frequency ultrasound applied at different power densities on calcein release. In addition, moieties are attached to the surface of the liposomes for specific targeting of the cancerous cells which over-express the receptors of these moieties, ultrasound is then applied and the release results are compared with the moiety free liposomes. The results showed that attaching these moieties to the surface of the PEGylated liposomes not only enhance their active targeting but also stimulate calcein release from these liposomes.

Keywords: active targeting, liposomes, moieties, ultrasound

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Authors: Xuan Li, Weian Huang, Jinsheng Sun, Fuhao Zhao, Zhiyuan Wang, Jintang Wang

Abstract:

Natural gas hydrates (NGHs) as promising alternative energy sources have gained increasing attention. Hydrate-bearing formation in marine areas is highly unconsolidated formation and is fragile, which is composed of weakly cemented sand-clay and silty sediments. During the drilling process, the invasion of drilling fluid can easily lead to excessive water content in the formation. It will change the soil liquid plastic limit index, which significantly affects the formation quality, leading to wellbore instability due to the metastable character of hydrate-bearing sediments. Therefore, controlling the filtrate loss into the formation in the drilling process has to be highly regarded for protecting the stability of the wellbore. In this study, the temperature-sensitive nanogel of P(NIPAM-co-AMPS-co-tBA) was prepared by soap-free emulsion polymerization, and the temperature-sensitive behavior was employed to achieve self-adaptive plugging in hydrate sediments. First, the effects of additional amounts of AMPS, tBA, and cross-linker MBA on the microgel synthesis process and temperature-sensitive behaviors were investigated. Results showed that, as a reactive emulsifier, AMPS can not only participate in the polymerization reaction but also act as an emulsifier to stabilize micelles and enhance the stability of nanoparticles. The volume phase transition temperature (VPTT) of nanogels gradually decreased with the increase of the contents of hydrophobic monomer tBA. An increase in the content of the cross-linking agent MBA can lead to a rise in the coagulum content and instability of the emulsion. The plugging performance of nanogel was evaluated in a core sample with a pore size distribution range of 100-1000nm. The temperature-sensitive nanogel can effectively improve the microfiltration performance of drilling fluid. Since a combination of a series of nanogels could have a wide particle size distribution at any temperature, around 200nm to 800nm, the self-adaptive plugging capacity of nanogels for the hydrate sediments was revealed. Thermosensitive nanogel is a potential intelligent plugging material for drilling operations in natural gas hydrate-bearing sediments.

Keywords: temperature-sensitive nanogel, NIPAM, self-adaptive plugging performance, drilling operations, hydrate-bearing sediments

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Authors: M. A. Akhavan-Behabadi, M. Najafi, A. Abbasi

Abstract:

An empirical investigation was performed in order to study the heat transfer characteristics of R600a flow boiling inside horizontal flattened tubes and the simultaneous effect of nanoparticles on boiling heat transfer in flattened channel. Round copper tubes of 8.7 mm I.D. were deformed into flattened shapes with different inside heights of 6.9, 5.5, and 3.4 mm as test areas. The effect of different parameters such as mass flux, vapor quality and inside height on heat transfer coefficient was studied. Flattening the tube caused significant enhancement in heat transfer performance so that the maximum augmentation ratio of 163% was obtained in flattened channel with lowest internal height. A new correlation was developed based on the present experimental data to predict the heat transfer coefficient in flattened tubes. This correlation estimated 90% of the entire database within ±20%.

Keywords: nano particles, flattend tube, R600a, CuO

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Authors: Allah Bakhsh Javid, Ali Mashayekh-Salehi, Fatemeh Davardoost

Abstract:

This study presents the preparation, characterization and catalytic activity of a novel natural mineral-based catalyst for destructive adsorption of tetracycline (TTC) as water emerging compounds. Degradation potential of raw and calcined magnetite catalyst was evaluated at different experiments situations such as pH, catalyst dose, reaction time and pollutant concentration. Calcined magnetite attained greater catalytic potential than the raw ore in the degradation of tetracycline, around 69% versus 3% at reaction time of 30 min and TTC aqueous solution of 50 mg/L, respectively. Complete removal of TTC could be obtained using 2 g/L calcined nanoparticles at reaction time of 60 min. The removal of TTC increased with the increase in solution temperature. Accordingly, considering its abundance in nature together with its very high catalytic potential, calcined pyrite is a promising and reliable catalytic material for destructive decomposition for catalytic decomposition and mineralization of such pharmaceutical compounds as TTC in water and wastewater.

Keywords: catalytic degradation, tetracycline, pyrite, emerging pollutants

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Authors: Jasneet Kaur, Swapandeep Singh Chimni

Abstract:

The unfavorable use of metal-based catalysts that are often extortionate and toxic can be overcome by using small organic molecules known as organocatalysts. A variety of small organic molecules, including Brønsted/Lewis bases and acids, based on sulfonic acids, phosphoric acids, amines, phosphines or carbenes, Cinchona alkaloids, have been used as organocatalysts. One of the key reasons for using organocatalysis is their ability to be effectively removed from the final product in comparison to the metallic counterparts, which are exceedingly difficult to remove. The present investigation seeks to explore the catalytic nature of Cinchona alkaloids as an organocatalyst for enantioselective synthesis of 3-substituted-3-aminooxindole, which is known to exhibit a variety of biological activities and pharmacological activities. In this context, an organocatalytic asymmetric route for the synthesis of 3-aminooxindoles via reaction of isatin imine with α-acetoxy-β-ketoesters has been developed. The bifunctional Cinchona derived thiourea catalyzed the reaction of α-acetoxy-β-ketoesters derivatives with isatin imine to afford 3-substituted-aminooxindole derivatives in up to 93% yield, 95% enantiomeric excess and >20:1 diastereomeric ratio. The reaction was performed at room temperature for two hours using 10 mol% of catalyst, in the presence of 4Å molecular sieves in tetrahydrofuran as a solvent at ambient temperature. After the completion of the reaction, the pure product could be easily separated by using column chromatography using hexane and ethyl acetate as solvents. In conclusion, the catalytic potential of Cinchona derived chiral thiourea-tertiary amine catalyst was explored for an organocatalytic enantioselective Mannich reaction of β-ketoester derivatives with various isatin imine derivatives under mild conditions.

Keywords: asymmetric synthesis, aminooxindoles, enantioselective, isatin imine

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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: A. Esra Pişkin, L. Yusuf Yivlik

Abstract:

Polyurethane consumption in the world increases every year. Polyetherpolyol, which is the main raw material of polyurethane, is produced from petroleum, and bioresources are needed in polyol production due to the damage it causes to the environment and the consumption of too much energy during the production phase. In this present work, bio polyol was synthesized with castor oil and soybean oil, and its use in rigid polyurethane systems was investigated. Transesterification and ring opening methods were applied for polyol synthesis, and the obtained bio polyols were compared with polyols derived petroleum. The goal of the present study was to synthesize biopolyols and to investigate the mechanical, thermal, and chemical properties of the synthesized polyurethane in terms of bio polyols.

Keywords: polyurethane, polyol, biopolyol, vegetable oil, foam, rigid polyurethane foam, ring opening, transesterification

Procedia PDF Downloads 445