Search results for: low temperature synthesis

Authors: Byung hyun Bae

Abstract:

In power transformer, leakage magnetic flux generate temperature rise of inner steel plate. Sometimes, this temperature rise can be serious problem. If temperature of steel plate is over critical point, harmful gas will be generated in the tank. And this gas can be a reason of fire, explosion and life decrease. So, temperature rise forecasting of steel plate is very important at the design stage of power transformer. To improve accuracy of forecasting of temperature rise, comparison between simulation and experiment achieved in this paper.

Keywords: power transformer, steel plate, temperature rise, experiment, simulation

Procedia PDF Downloads 464

Authors: Wanida Wonsawat

Abstract:

Bioreduction of silver nanoparticles (AgNPs) from silver ions (Ag+) using water extract of Thai basil leaf was successfully carried out. The basil leaf extract provided a reducing agent and stabilizing agent for a synthesis of metal nanoparticles. Silver nanoparticles received from cut and uncut basil leaf was compared. The resulting silver nanoparticles are characterized by UV-Vis spectroscopy. The maximum intensities of silver nanoparticle from cut and uncut basil leaf were 410 and 420, respectively. The techniques involved are simple, eco-friendly and rapid.

Keywords: basil leaves, silver nanoparticles, green synthesis, plant extract

Procedia PDF Downloads 549

Authors: Lorenzo Gontrani, Marilena Carbone, Domenica Tommasa Donia, Elvira Maria Bauer, Pietro Tagliatesta

Abstract:

One of the fields where DES shows remarkable added values is the synthesis Of inorganic materials, in particular nanoparticles. In this field, the higher- ent and highly-tunable nano-homogeneities of DES structure give origin to a marked templating effect, a precious role that has led to the recent bloom of a vast number of studies exploiting these new synthesis media to prepare Nanomaterials and composite structures of various kinds. In this contribution, the most recent developments in the field will be reviewed, and some ex-citing examples of novel metal oxide nanoparticles syntheses using non-toxic type-IV Deep Eutectic Solvents will be described. The prepared materials possess nanometric dimensions and show flower-like shapes. The use of the pre- pared nanoparticles as fluorescent materials for the detection of various contaminants is under development.

Keywords: metal deep eutectic solvents, nanoparticles, inorganic synthesis, type IV DES, lamellar

Procedia PDF Downloads 100

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

Abstract:

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

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

Procedia PDF Downloads 276

Authors: Jian Huang, Weixin Qian, Haitao Zhang, Weiyong Ying

Abstract:

Cobalt-gadolinium catalyst for Fischer-Tropsch synthesis was prepared by impregnation method with commercial silica gel, and its texture properties were characterized by BET, XRD, and TPR. The catalytic performance of the catalyst was tested in a fixed bed reactor. The results showed that the addition of gadolinium to the cobalt catalyst might decrease the size of cobalt particles, and increased the dispersion of catalytic active cobalt phases. The carbon number distributions for the catalysts was calculated by ASF equation.

Keywords: Fischer-Tropsch synthesis, cobalt-based catalysts, gadolinium, carbon number distributions

Procedia PDF Downloads 344

Authors: Daniela N. Correa-Llantén, Sebastián A. Muñoz-Ibacache, Mathilde Maire, Jenny M. Blamey

Abstract:

The biosynthesis of nanoparticles by microorganisms, on the contrary to chemical synthesis, is an environmentally-friendly process which has low energy requirements. In this investigation, we used the microorganism Geobacillus wiegelii, strain GWE1, an aerobic thermophile belonging to genus Geobacillus, isolated from a drying oven. This microorganism has the ability to reduce selenite evidenced by the change of color from colorless to red in the culture. Elemental analysis and composition of the particles were verified using transmission electron microscopy and energy-dispersive X-ray analysis. The nanoparticles have a defined spherical shape and a selenium elemental state. Previous experiments showed that the presence of the whole microorganism for the reduction of selenite was not necessary. The results strongly suggested that an intracellular NADPH/NADH-dependent reductase mediates selenium nanoparticles synthesis under aerobic conditions. The enzyme was purified and identified by mass spectroscopy MALDI-TOF TOF technique. The enzyme is a 1-pyrroline-5-carboxylate dehydrogenase. Histograms of nanoparticles sizes were obtained. Size distribution ranged from 40-160 nm, where 70% of nanoparticles have less than 100 nm in size. Spectroscopic analysis showed that the nanoparticles are composed of elemental selenium. To analyse the effect of pH in size and morphology of nanoparticles, the synthesis of them was carried out at different pHs (4.0, 5.0, 6.0, 7.0, 8.0). For thermostability studies samples were incubated at different temperatures (60, 80 and 100 ºC) for 1 h and 3 h. The size of all nanoparticles was less than 100 nm at pH 4.0; over 50% of nanoparticles have less than 100 nm at pH 5.0; at pH 6.0 and 8.0 over 90% of nanoparticles have less than 100 nm in size. At neutral pH (7.0) nanoparticles reach a size around 120 nm and only 20% of them were less than 100 nm. When looking at temperature effect, nanoparticles did not show a significant difference in size when they were incubated between 0 and 3 h at 60 ºC. Meanwhile at 80 °C the nanoparticles suspension lost its homogeneity. A change in size was observed from 0 h of incubation at 80ºC, observing a size range between 40-160 nm, with 20% of them over 100 nm. Meanwhile after 3 h of incubation at size range changed to 60-180 nm with 50% of them over 100 nm. At 100 °C the nanoparticles aggregate forming nanorod structures. In conclusion, these results indicate that is possible to modulate size and shape of biologically synthesized nanoparticles by modulating pH and temperature.

Keywords: genus Geobacillus, NADPH/NADH-dependent reductase, selenium nanoparticles, biosynthesis

Procedia PDF Downloads 286

Authors: Olga Shapovalova, Vladimir Vinogradov

Abstract:

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

Procedia PDF Downloads 240

Authors: H. M. Wang, C. J. Chang

Abstract:

As the threat of global climate change is more seriously, "net zero emissions by 2050" has become a common global goal. In order to reduce the consumption of petrochemical raw materials and reduce carbon emissions, low-carbon fiber materials have become key materials in the future global textile supply chain. This project uses polyolefin raw materials to modify through synthesis and amination to develop low-temperature dyeable polypropylene fibers, endow them with low-temperature dyeability and high color fastness that can be combined with acid dyes, and improve the problem of low coloring strength. The color fastness to washing can reach the requirement of commerce with 3.5 level or more. Therefore, we realize the entry of polypropylene fiber into the clothing textile supply chain, replace existing fiber raw materials, solve the problem of domestic chemical fiber, textile, and clothing industry's plight of no low-carbon alternative new material sources, and provide the textile industry with a solution to achieve the goal of net zero emissions in 2050.

Keywords: acid dyes, dyeing, low-temperature, polypropylene fiber

Procedia PDF Downloads 61

Authors: Mahmoud H. Abu Elella, Riham R. Mohamed, Magdy W. Sabaa

Abstract:

Firstly, synthesis of N-Quaternized Chitosan (NQC), then it was proven by FTIR and 1H-NMR analysis. The degree of quaternization(DQ 35% ) was determined by equation. Secondly, synthesis of cross-linked hydrogels composed of NQC and poly (vinyl alcohol) (PVA) in different weight ratios in presence of glutaraldehyde (GA) as cross-linking agent. Characterization of the prepared hydrogels was done using FTIR, SEM, XRD,and TGA. Swellability in simulated body fluid (SBF) solutions applied on NQC / PVA hydrogels and swelling rate(Wt%) and metal ions uptake was done on it.

Keywords: hydrogel, metal ions uptake, N-quaternized chitosan, poly (vinyl alcohol), swellability

Procedia PDF Downloads 401

Authors: Zehui Du, Chaiwat Prapainainar, Paisan Kongkachuichay, Paweena Prapainainar

Abstract:

The aim of this work was to obtain small crystalline size and high crystallinity of mordenites and analcimes, by modifying the aging time, agitation, water content, crystallization temperature and crystallization time. Two different hydrothermal methods were studied. Both methods used Na2SiO3 as the silica source, NaAlO2 as the aluminum source, and NaOH as the alkali source. The first method used HMI as the template while the second method did not use the template. Mordenite crystals with spherical shape and bimodal in size of about 1 and 5 µm were obtained from the first method using conditions of 24 hr aging time, 170°C and 24 hr crystallization. Modernites with high crystallinity were formed using agitation system in the crystallization process. It was also found that the aging time of 2 hr and 24 hr did not much affect the formation of mordenite crystals. Analcime crystals were formed in spherical shape and facet on surface with the size between 13-15 µm by the second method using the conditions of 30 minutes aging time, 170°C and 24 hr crystallization without calcination. By increasing water content, the crystallization process was slowed down and resulted in smaller analcime crystals. Larger size of analcime crystals were observed when the samples were calcined at 300°C and 580°C. Higher calcination temperature led to higher crystal growth and resulted in larger crystal size. Finally, mordenite and analcime was used as fillers in zeolite/Nafion composite membrane to solve the fuel cross over problem in direct alcohol fuel cell.

Keywords: analcime, hydrothermal synthesis, mordenite, zeolite

Procedia PDF Downloads 236

Authors: Sanjay Upadhyay, Om Prakash Pandey

Abstract:

Hydrogen has been promoted as an alternative source of energy, which is renewable, cost-effective, and nature-friendly. Hydrogen evolution reaction (HER) can be used for mass production of hydrogen at a very low cost through electrochemical water splitting. An active and efficient electrocatalyst is required to perform this reaction. Till date, platinum (Pt) is a stable and efficient electrocatalyst towards HER. But its high cost and low abundance hiders its large scale uses. Molybdenum carbide having a similar electronic structure to platinum can be a great alternative to costly platinum. In this study, pure phase molybdenum carbide (Mo₂C) has been synthesized in a single step. Synthesis temperature and holding time have been optimized to obtain pure phases of Mo₂C. The surface, structural and morphological properties of as-synthesized compounds have been studied. The HER activity of as-synthesized compounds has been explored in detail.

Keywords: capacitance, hydrogen fuel, molybdenum carbide, nanoparticles

Procedia PDF Downloads 169

Authors: Khamael Abualnaja, Hala M. Abo-Dief

Abstract:

Silver nanoparticles (AgNPs) are the subject of important recent interest, present in a large range of applications such as electronics, catalysis, chemistry, energy, and medicine. Metallic nanoparticles are traditionally synthesized by wet chemical techniques, where the chemicals used are quite often toxic and flammable. In this work, we describe an effective and environmental-friendly technique of green synthesis of silver nanoparticles. Silver nanoparticles (AgNPs) synthesized using silver nitrate solution and the extract of mint, basil, orange peel and Tangerines peel which used as reducing agents. Silver Nanoparticles were characterized using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and UV–Vis absorption spectroscopy. SEM analysis showed the average particle size of mint, basil, orange peel, Tangerines peel are 30, 20, 12, 10 nm respectively. This is for the first time that any plant extract was used for the synthesis of nanoparticles.

Keywords: silver nanoparticles, green synthesis, scanning electron microscopy, plants

Procedia PDF Downloads 225

Authors: Houcine Ammar

Abstract:

Chromenederivatives are an important class of heterocycles that are found in a wide range of natural products. Chromenes are commonly used as cosmetics, food additives, and possibly biodegradable agrochemicals. Recently, the synthesis of chromene derivatives has drawn more attention due to their pharmacological and biological applications. In the present work, we are interested in the synthesis and characterization of chromeno [2,3-b] pyridin-4-yl) formimidate, carried out in 4 steps: (i) the synthesis of 3-cyanoiminocoumarins is realized first by Knœvenagel reaction by reacting malonitrile with variously substituted o-phenolic benzaldehydes. In order to undergo reduction by sodium tetraborohydride NaBH4 to lead to new 2-amino-3-cyano-4H-chromenes, these compounds were easily transformed by the action of malonitrile leading to 2,4-diamino-5H-chromeno [2,3-b] pyridine-3-carbonitrile under microwave activation. For the final step, the action of triethylorthoformate on 2,4-diamino-5H-chromeno [2,3-b] pyridine-3-carbonitrile leads to new chromeno [2,3-b] pyridinheterocycles. -4-yl) formimidate. The synthesized compounds have been characterized by different spectroscopic techniques 1 H-NMR, 13 C-NMR, and IRTF.

Keywords: chromene, microwave, knovenagel condensation, chromeno [2, 3-b] pyridine

Procedia PDF Downloads 63

Authors: Nayana T. Nivangune, Vivek V. Ranade, Ashutosh A. Kelkar

Abstract:

Organic carbamates are versatile compounds widely employed as pesticides, fungicides, herbicides, dyes, pharmaceuticals, cosmetics and in the synthesis of polyurethanes. Carbamates can be easily transformed into isocyanates by thermal cracking. Isocyantes are used as precursors for manufacturing agrochemicals, adhesives and polyurethane elastomers. Manufacture of polyurethane foams is a major application of aromatic ioscyanates and in 2007 the global consumption of polyurethane was about 12 million metric tons/year and the average annual growth rate was about 5%. Presently Isocyanates/carbamates are manufactured by phosgene based process. However, because of high toxicity of phoegene and formation of waste products in large quantity; there is a need to develop alternative and safer process for the synthesis of isocyanates/carbamates. Recently many alternative processes have been investigated and carbamate synthesis by methoxycarbonylation of aromatic amines using dimethyl carbonate (DMC) as a green reagent has emerged as promising alternative route. In this reaction methanol is formed as a by-product, which can be converted to DMC either by oxidative carbonylation of methanol or by reacting with urea. Thus, the route based on DMC has a potential to provide atom efficient and safer route for the synthesis of carbamates from DMC and amines. Lot of work is being carried out on the development of catalysts for this reaction and homogeneous zinc salts were found to be good catalysts for the reaction. However, catalyst/product separation is challenging with these catalysts. There are few reports on the use of supported Zn catalysts; however, deactivation of the catalyst is the major problem with these catalysts. We wish to report here methoxycarbonylation of aniline to methylphenylcarbamate (MPC) using amino acid complexes of Zn as highly active and selective catalysts. The catalysts were characterized by XRD, IR, solid state NMR and XPS analysis. Methoxycarbonylation of aniline was carried out at 170 °C using 2.5 wt% of the catalyst to achieve >98% conversion of aniline with 97-99% selectivity to MPC as the product. Formation of N-methylated products in small quantity (1-2%) was also observed. Optimization of the reaction conditions was carried out using zinc-proline complex as the catalyst. Selectivity was strongly dependent on the temperature and aniline:DMC ratio used. At lower aniline:DMC ratio and at higher temperature, selectivity to MPC decreased (85-89% respectively) with the formation of N-methylaniline (NMA), N-methyl methylphenylcarbamate (MMPC) and N,N-dimethyl aniline (NNDMA) as by-products. Best results (98% aniline conversion with 99% selectivity to MPC in 4 h) were observed at 170oC and aniline:DMC ratio of 1:20. Catalyst stability was verified by carrying out recycle experiment. Methoxycarbonylation preceded smoothly with various amine derivatives indicating versatility of the catalyst. The catalyst is inexpensive and can be easily prepared from zinc salt and naturally occurring amino acids. The results are important and provide environmentally benign route for MPC synthesis with high activity and selectivity.

Keywords: aniline, heterogeneous catalyst, methoxycarbonylation, methylphenyl carbamate

Procedia PDF Downloads 250

Authors: S. Sharma, U. Batra, S. Kapoor, A. Dua

Abstract:

In this study, the effects and interactions of reaction time and capping agent assistance during sol-gel synthesis of magnesium substituted hydroxyapatite nanopowder (MgHA) on hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P ratio and mean crystallite size was examined experimentally as well as through statistical analysis. MgHA nanopowders were synthesized by sol-gel technique at room temperature using aqueous solution of calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and potassium dihydrogen phosphate as starting materials. The reaction time for sol-gel synthesis was varied between 15 to 60 minutes. Two process routes were followed with and without addition of triethanolamine (TEA) in the solutions. The elemental compositions of as-synthesized powders were determined using X-ray fluorescence (XRF) spectroscopy. The functional groups present in the as-synthesized MgHA nanopowders were established through Fourier Transform Infrared Spectroscopy (FTIR). The amounts of phases present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders were determined using X-ray diffraction (XRD). The HA content in biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized MgHA nanopowders increased effectively with reaction time of sols (p < 0.0001, two way Anova), however, these were independent of TEA addition (p > 0.15, two way Anova). The MgHA nanopowders synthesized with TEA assistance exhibited 14 nm lower crystallite size (p < 0.018, 2 sample t-test) compared to the powder synthesized without TEA assistance.

Keywords: capping agent, hydroxyapatite, regression analysis, sol-gel, 2- sample t-test, two-way analysis of variance (ANOVA)

Procedia PDF Downloads 340

Authors: Young-Min Kang

Abstract:

M-type Sr-hexaferrites (SrFe12O19) is one of the most utilized materials in permanent magnets due to their low price, outstanding chemical stability, and appropriate hard magnetic properties. For a M-type Sr-hexaferrite with a saturation magnetization (MS) of ~74.0 emu/g the practical limits of remanent flux density (Br) and maximum energy product (BH) max are ~4.6 kG and ~5.3 MGOe. Meanwhile, W-type hexaferrite (SrFe18O27) with higher MS ~81emu/g can be a good candidate for the development of enhanced ferrite magnet. However the W-type hexaferrite is stable at the temperature over 1350 ºC in air, and thus it is hard to control grain size and the coercivity. We report here high-MS M-W composite hexaferrites synthesized at 1250 ºC in air by doping Ca, Co, Mn, and Zn into the hexaferrite structures. The hexaferrites samples of stoichiometric SrFe12O19 (SrM) and Ca-Co-Mn-Zn doped hexaferrite (Sr0.7Ca0.3Fen-0.6Co0.2Mn0.2Zn0.2Oa) were prepared by conventional solid state reaction process with varying Fe content (10 ≤ n ≤ 17). Analysis by x-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM) were performed for phase identification and microstructural observation respectively. Magnetic hysteresis curves were measured using vibrating sample magnetometer (VSM) at room temperature (300 K). Single M-type phase could be obtained in the non-doped SrM sample after calcinations at the range of 1200 ºC ~ 1300 ºC, showing MS in the range of 72 ~ 72.6 emu/g. The Ca-Co-Mn-Zn doped SrM with Fe content, 10 ≤ n ≤ 13, showed both M and W-phases peaks in the XRD after respective calcinations at 1250 ºC. The sample with n=13 showed the MS of 70.7, 75.3, 78.0 emu/g, respectively, after calcination at 1200, 1250, 1300 ºC. The high MS over that of non-doped SrM (~72 emu/g) is attributed to the volume portion of W-phase. It is also revealed that the high MS W-phase could not formed if only one of the Ca, Co, Zn is missed in the substitution. These elements are critical to form the W-phase at the calcinations temperature of 1250 ºC, which is 100 ºC lower than the calcinations temperature for non-doped Sr-hexaferrites.

Keywords: M-type hexaferrite, W-type hexaferrite, saturation magnetization, low-temperature synthesis

Procedia PDF Downloads 143

Authors: Vinaya Kambappa

Abstract:

Propylphosphonic anhydride (T3P®)-DMSO is used as an efficient and mild reagent for the one-pot synthesis of 3,4-dihydropyrimidin-2(1H)-ones/thiones from aromatic alcohols. Alcohols are oxidized in situ to aldehydes under mild conditions, which in turn undergo a three-component reaction with β-ketoester and urea/thiourea to afford 3,4-dihydropyrimidin-2(1H)-ones/thiones. The synthesis of 3,4-dihydropyrimidin-2(1H)-ones/thiones directly from alcohols has been reported for the first time best to our knowledge, under mild reaction conditions in good yield. The easy work-up procedure, low cost and less toxicity of the reagent are the main advantages of this protocol.

Keywords: β-ketoester, propylphosphonic anhydride, three-component reaction, pyrimidine

Procedia PDF Downloads 124

Authors: Hamid Yasinian

Abstract:

Random epistemologies and hash tables have garnered minimal interest from both security experts and experts in the last several years. In fact, few information theorists would disagree with the evaluation of expert systems. In our research, we discover how flip-flop gates can be applied to the study of superpages. Though such a hypothesis at first glance seems perverse, it is derived from known results.

Keywords: synthesis, multi-processors, interactive model, moor’s law

Procedia PDF Downloads 403

Authors: Anita K. Kovacs, Peter Hegyes, Zsolt Bozso, Gabor Toth

Abstract:

Fluorination has been used extensively by the pharmaceutical industry as a strategy to improve the pharmacokinetics of drugs due to its effectiveness in increasing the potency of antimicrobial peptides (AMPs). Multiple-fluorinated indole-ring-containing tryptophan derivatives have the potential of having better antimicrobial activity than the widely used mono-fluorinated indole-ring containing tryptophan derivatives, but they are not available commercially. Therefore, our goal is to synthesize multiple-fluorinated indole-ring containing tryptophan derivatives to incorporate them into AMPs to enhance their antimicrobial activity. During our work, we are trying several methods (classical organic synthesis, enzymic synthesis, and solid phase peptide synthesis) for the synthesis of the said compounds, with mixed results. With classical organic synthesis (four different routes), we did not get the desired results. The reaction of serin with substituted indole in the presence of acetic anhydride led to racemic tryptophane; with the reaction of protected serin with indole in the presence of nickel complex was unsuccessful; the reaction of serin containing protected dipeptide with disuccinimidyl carbonate we achieved a tryptophane containing dipeptide, its chiral purity is being examined; the reaction of alcohol with substituted indole in the presence of copper complex was successful, but it was only a test reaction, we could not reproduce the same result with serine. The undergoing tryptophan-synthase method has shown some potential, but our work has not been finished yet. The successful synthesis of the desired multiple-fluorinated indole-ring-containing tryptophan will be followed by solid phase peptide synthesis in order to incorporate it into AMPs to enhance their antimicrobial activity. The successful completion of these phases will mean the possibility of manufacturing new, effective AMPs.

Keywords: halogenation, fluorination, tryptophan, enhancement of antimicrobial activity

Procedia PDF Downloads 79

Authors: Adrien Cornille, Marine Blain, Bernard Boutevin, Sylvain Caillol

Abstract:

Generally, linear polyurethanes (PUs) are obtained by the reaction between an oligomeric diol, a short diol as chain extender and a diisocyanate. However the use of diisocyanate should be avoided since they are generally very harmful for human health. Therefore the synthesis of NIPUs (non isocyanate PUs) from step growth polymerization of dicyclocarbonates and diamines should be favoured. This method is particularly interesting since no hazardous isocyanates are used. Thus, this reaction, extensively studied by Endo et al. is currently gaining a lot of attention as a substitution route for the synthesis of NIPUs, both from industrial and academic community. However, the reactivity of reaction between amine and cyclic carbonate is a major scientific issue, since cyclic carbonates are poorly reactive. Thus, our team developed several synthetic ways for the synthesis of various di-cyclic carbonates based on C5-, C6- and dithio- cyclic carbonates, from different biobased raw materials (glycerin isosorbide, vegetable oils…). These monomers were used to synthesize NIPUs with various mechanical and thermal properties for various applications. We studied the reactivity of reaction with various catalysts and find optimized conditions for room temperature reaction. We also studied the radical copolymerization of cyclic carbonate monomers in styrene-acrylate copolymers for coating applications. We also succeeded in the elaboration of biobased NIPU flexible foams. To the best of our knowledge, there is no report in literature on the preparation of non-isocyanate polyurethane foams.

Keywords: foam, nonisocyanate polyurethane, cyclic carbonate, blowing agent, scanning electron microscopy

Procedia PDF Downloads 205

Authors: Takeyuki Suzuki, Ismiyarto, Da-Yang Zhou, Kaori Asano, Hiroaki Sasai

Abstract:

The development of catalytic asymmetric reaction is important for the synthesis of natural products. To construct the multiple stereogenic centers, the desymmetrization of meso compounds is powerful strategy for the synthesis of chiral molecules. Oxidative desymmetrization of meso diols using chiral iridium catalyst provides a chiral hydroxyl ketone. The reaction is practical and an environmentally benign method which does not require the use of stoichiometric amount of heavy metals. This time we report here catalytic asymmetric synthesis of catalponol based on tandem coupling of meso-diols and an aldehyde. The tandem reaction includes oxidative desymmetrization of meso-diols, aldol condensation with an aldehyde. The reaction of meso-diol, benzaldehyde in the presence of a catalytic amount of chiral Ir complex and CsOH in tetrahydrofuran afforded the desired benzylidene ketone in 82% yield with 96% ee (enantiomeric excess). Next, we applied this benzylidene ketone derivative to the synthesis of catalponol. The corresponding benzylidene ketone was obtained in 87% yield with 99% ee. Finally, catalponol was synthesized by the regio- and stereo-selective reduction of dienone moiety in good yield.

Keywords: catalponol, desymmetrization, iridium, oxidation

Procedia PDF Downloads 145

Authors: Sze Shin Low, Michelle T. T. Tan, Poi Sim Khiew, Hwei-San Loh

Abstract:

An efficient graphene/zinc oxide (PSE-G/ZnO) platform based on pi-pi stacking, non-covalent interactions for the development of aptamer-based biosensor was presented in this study. As a proof of concept, the DNA recognition capability of the as-developed PSE-G/ZnO enhanced aptamer-based biosensor was evaluated using Coconut Cadang-cadang viroid disease (CCCVd). The G/ZnO nanocomposite was synthesised via a simple, green and efficient approach. The pristine graphene was produced through a single step exfoliation of graphite in sonochemical alcohol-water treatment while the zinc nitrate hexahydrate was mixed with the graphene and subjected to low temperature hydrothermal growth. The developed facile, environmental friendly method provided safer synthesis procedure by eliminating the need of harsh reducing chemicals and high temperature. The as-prepared nanocomposite was characterised by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) to evaluate its crystallinity, morphology and purity. Electrochemical impedance spectroscopy (EIS) was employed for the detection of CCCVd sequence with the use of potassium ferricyanide (K3[Fe(CN)6]). Recognition of the RNA analytes was achieved via the significant increase in resistivity for the double stranded DNA, as compared to single-stranded DNA. The PSE-G/ZnO enhanced aptamer-based biosensor exhibited higher sensitivity than the bare biosensor, attributing to the synergistic effect of high electrical conductivity of graphene and good electroactive property of ZnO.

Keywords: aptamer-based biosensor, graphene/zinc oxide nanocomposite, green synthesis, screen printed carbon electrode

Procedia PDF Downloads 328

Authors: Masoumeh Moghbel

Abstract:

Nowadays, carbon dioxide which is produced by human activities is considered as the main effective factor in the global warming occurrence. Regarding to the role of CO2 and its ability in trapping the heat, the main objective of this research is study the effect of atmospheric CO2 (which is recorded in Manaloa) on variations of temperature parameters (daily mean temperature, minimum temperature and maximum temperature) in 5 meteorological stations in Iran which were selected according to the latitude and altitude in 40 years statistical period. Firstly, the trend of temperature parameters was studied by Regression and none-graphical Man-Kendal methods. Then, relation between temperature variations and CO2 were studied by Correlation technique. Also, the impact of CO2 amount on temperature in different atmospheric levels (850 and 500 hpa) was analyzed. The results illustrated that correlation coefficient between temperature variations and CO2 in low latitudes and high altitudes is more significant rather than other regions. it is important to note that altitude as the one of the main geographic factor has limitation in affecting the temperature variations, so that correlation coefficient between these two parameters in 850 hpa (r=0.86) is more significant than 500 hpa (r = 0.62).

Keywords: altitude, atmospheric carbon dioxide, latitude, temperature variations

Procedia PDF Downloads 377

Authors: I. Grigoraviciute-Puroniene, K. Tsuru, E. Garskaite, Z. Stankeviciute, A. Beganskiene, K. Ishikawa, A. Kareiva

Abstract:

Tricalcium phosphate (β-Ca₃(PO₄)₂, β-TCP) powders were synthesized using wet polymeric precipitation method for the first time to our best knowledge. The results of X-ray diffraction analysis showed the formation of almost single a Ca-deficient hydroxyapatite (CDHA) phase of a poor crystallinity already at room temperature. With continuously increasing the calcination temperature up to 800 °C, the crystalline β-TCP was obtained as the main phase. It was demonstrated that infrared spectroscopy is very effective method to characterize the formation of β-TCP. The SEM results showed that β-TCP solids were homogeneous having a small particle size distribution. The β-TCP powders consisted of spherical particles varying in size from 100 to 300 nm. Fabricated β-TCP specimens were placed to the bones of the rats and maintained for 1-2 months.

Keywords: Tricalcium phosphate (β-Ca3(PO4)2, bone regeneration, wet chemical processing, polymeric precipitation

Procedia PDF Downloads 272

Authors: Afrah E. Mohammed, Mudawi M. Nour

Abstract:

Environmentally friendly green synthesis of nanomaterial has a very significant part in nanotechnology. In the present research, the synthesis of silver nanoparticles (AgNPs) was established by treating silver ions with the aqueous extract of Calligonum comosum green shoots at room temperature. AgNPs formation was firstly detected by the colour change of mixed extract (plant extract and AgNO3). Further characterization was done by ultraviolet (UV)-Vis spectrophotometer, transmission electron microscopy (TEM), scanning electron microscopy (SEM), zeta potential and fourier transform infrared spectroscopy (FTIR). The peak values for UV-VIS- spectroscopy were in the range of 440 nm, TEM micrograph showed a spherical shape for the particles and zeta potential showed the formation of negative charged nanoparticles with an average size of about 105.8 nm. 1635.41 and 3249.83 cm−1 are the peaks detected from the FTIR analysis. In this study, biosynthesized silver nanoparticles mediated by C. comosum were tested for their antimycotic activity using a well diffusion method against fungal species; Aspergillus flavus, Penicillium sp, Fusarium oxysporum. Our findings indicated that biosynthesized AgNPs showed an efficient antimycotic activity against tested species. The antimycotic action of AgNPs varied according to different fungal species. Results confirmed the ability of C. comosum green shoot extract to act as an reducing and stabilizing agent during the synthesis of AgNPs.

Keywords: AGNPS, zeta potential, TEM, SEM

Procedia PDF Downloads 49

Authors: Aleksander Ejsmont, Stefan Wuttke, Joanna Goscianska

Abstract:

Gaining control over particle shape, size and crystallinity is an ongoing challenge for many materials. Especially metalorganic frameworks (MOFs) are recently widely studied. Besides their remarkable porosity and interesting topologies, morphology has proven to be a significant feature. It can affect the further material application. Thus seeking new approaches that enable MOF morphology modulation is important. MOFs are reticular structures, where building blocks are made up of organic linkers and metallic nodes. The most common strategy of ensuring metal source is using salts, which usually exhibit high solubility and hinder morphology control. However, there has been a growing interest in using metal oxides as structure-directing agents towards MOFs due to their very low solubility and shape preservation. Metal oxides can be treated as a metal reservoir during MOF synthesis. Up to now, reports in which receiving MOFs from metal oxides mostly present ZnO conversion to ZIF-8. However, there are other oxides, for instance, Co₃O₄, which often is overlooked due to their structural stability and insolubility in aqueous solutions. Cobalt-based materials are famed for catalytic activity. Therefore the development of their efficient synthesis is worth attention. In the presented work, an optimized Co₃O₄transition to Co-MOFviaa solvothermal approach was proposed. The starting point of the research was the synthesis of Co₃O₄ flower petals and needles under hydrothermal conditions using different cobalt salts (e.g., cobalt(II) chloride and cobalt(II) nitrate), in the presence of urea, and hexadecyltrimethylammonium bromide (CTAB) surfactant as a capping agent. After receiving cobalt hydroxide, the calcination process was performed at various temperatures (300–500 °C). Then cobalt oxides as a source of cobalt cations were subjected to reaction with trimesic acid in solvothermal environment and temperature of 120 °C leading to Co-MOF fabrication. The solution maintained in the system was a mixture of water, dimethylformamide, and ethanol, with the addition of strong acids (HF and HNO₃). To establish how solvents affect metal oxide conversion, several different solvent ratios were also applied. The materials received were characterized with analytical techniques, including X-ray powder diffraction, energy dispersive spectroscopy,low-temperature nitrogen adsorption/desorption, scanning, and transmission electron microscopy. It was confirmed that the synthetic routes have led to the formation of Co₃O₄ and Co-based MOF varied in shape and size of particles. The diffractograms showed receiving crystalline phase for Co₃O₄, and also for Co-MOF. The Co₃O₄ obtained from nitrates and with using low-temperature calcination resulted in smaller particles. The study indicated that cobalt oxide particles of different size influence the efficiency of conversion and morphology of Co-MOF. The highest conversion was achieved using metal oxides with small crystallites.

Keywords: Co-MOF, solvothermal synthesis, morphology control, core-shell

Procedia PDF Downloads 125

Authors: Azizi Cherifa, O. Benzaoui

Abstract:

The thermal aspects in the design of power circuits often deserve as much attention as pure electric components aspects as the operating temperature has a direct influence on their static and dynamic characteristics. MOSFET is fundamental in the circuits, it is the most widely used device in the current production of semiconductor components using their honorable performance. The aim of this contribution is devoted to the effect of the temperature on the properties of MOSFETs. The study enables us to calculate the drain current as function of bias in both linear and saturated modes. The effect of temperature is evaluated using a numerical simulation, using the laws of mobility and saturation velocity of carriers as a function of temperature.

Keywords: temperature, MOSFET, mobility, transistor

Procedia PDF Downloads 322

Authors: Gülşah Çelik Gül, Figen Kurtuluş

Abstract:

The first laboratory synthesis of hard materials such as diamond proceeded to attack of developing materials with high hardness to compete diamond. Boron rich solids are good candidates owing to their short interatomic bond lengths and strong covalent character. Boron containing hard material was synthesized by modified-microwave method under nitrogen atmosphere by using a fuel (glycine or urea), amorphous boron and/or boric acid in appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differantial thermal analysis (TG/DTA).

Keywords: boron containing materials, hard materials, microwave synthesis, powder X-ray diffraction

Procedia PDF Downloads 569

Authors: O. Abusaeeda, J. P. O. Evans, D. Downes

Abstract:

We demonstrate the synthesis of intermediary views within a sequence of X-ray images that exhibit depth from motion or kinetic depth effect in a visual display. Each synthetic image replaces the requirement for a linear X-ray detector array during the image acquisition process. Scale invariant feature transform, SIFT, in combination with epipolar morphing is employed to produce synthetic imagery. Comparison between synthetic and ground truth images is reported to quantify the performance of the approach. Our work is a key aspect in the development of a 3D imaging modality for the screening of luggage at airport checkpoints. This programme of research is in collaboration with the UK Home Office and the US Dept. of Homeland Security.

Keywords: X-ray, kinetic depth, KDE, view synthesis

Procedia PDF Downloads 231

Authors: Devender Mandala, Paul Watts

Abstract:

Cis-Nucleosides mainly lamivudine (3TC) and emtricitabine (FTC) are an important tool in the treatment of Human immune deficiency virus (HIV), Hepatitis B virus (HBV) and Human T-Lymotropoic virus (HTLV). Lamivudine and emtricitabine are potent nucleoside analog reverse transcriptase inhibitors (nRTI). These two drugs are synthesized by a four-stage process from the starting materials: menthyl glyoxylate hydrate and 1,4-dithane-2,5-diol to produce the 5-hydroxy oxathiolane which upon acetylation with acetic anhydride to yield 5-acetoxy oxathiolane. Then glycosylation of this acetyl product with silyl protected nucleoside to produce the intermediate. The reduction of this intermediates can provide the final targets. Although there are several different methods reported for the synthesis of lamivudine and emtricitabine as a single enantiomer, we required an efficient route, which was suitable for large-scale synthesis to support the development of these compounds. In this process, we successfully prepared the intermediates of lamivudine and emtricitabine without using any solvents and catalyst, thus promoting the green synthesis. All the synthesized compound were confirmed by TLC, GC, Mass, NMR and 13C NMR spectroscopy.

Keywords: emtricitabine, green synthesis, lamivudine, nucleoside

Procedia PDF Downloads 202