Search results for: inorganic synthesis

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

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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

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Authors: Talat Baran

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The Suzuki C(sp2)-C(sp2) coupling reaction is considered to be one of the best ways for the synthesis of biaryl compounds. There are many studies reporting the catalytic performance of palladium catalyst in Suzuki coupling reactions. Natural biopolymer (such as zeolite, carbon, silica, and chitosan) supporting catalysts have been lately attracted interest because of their low-cost, nontoxicity, and eco-friendliness. One of the most important natural biopolymer is cellulose, which is widely considered as an eco-friendly biopolymer due to its biodegradable, non-toxic and renewable nature. In this study, (1) cellulose supported Pd(II) catalyst was synthesized (2) its chemical structure was characterized by FT-IR, SEM/EDAX, XRD, TG-DTG, ICP-OES techniques (3) to investigate the performance of the catalyst in Suzuki coupling reactions by using microwave irradiation technique (4) reusability of the catalyst was done under optimum conditions. This cellulose supported Pd(II) catalyst exhibited high selectivity and efficiency in Suzuki coupling reactions under mild conditions (50°C). High TON and TOF values were recorded for the catalyst. Also, the reusability tests showed the catalysts could be used for several times in consequence of reusability tests.

Keywords: palladium, cellulose, Schiff base, reusability

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Authors: Opeyemi A. Oyewo, Seshibe Makgato

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This paper presents the synthesis, characterization, and application of pelletized chitosan immobilized sawdust cellulose nanocrystals (PCCN) in a fixed-bed column for the continuous adsorption of methyl blue (MB) from water. The product was characterized using FT-IR, XRD, and SEM analysis. Microstructural examination revealed that the pellets are porous and spherical. XRD examination revealed phases that can be attributed to the presence of chitosan in PCCN. The effects of starting concentration, bed depth, and flow rate on synthetic water were explored. To identify MB breakthrough behaviour, performance indices such as bed volume, adsorbent exhaustion rate, and service time were investigated. Furthermore, the breakthrough data were incorporated into both the Thomas and Bohart-Adams models. The Thomas model was suitable for describing MB breakthrough curves. However, more research with diverse water matrices may be required to assess the resilience of PCCN.

Keywords: adsorption, dynamic, methyl blue, pelletization

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Authors: Cristina Lavilla, Andreas Heise

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The synthesis of sequence-controlled polymers has received increasing attention in the last years. Well-defined polyacrylates, polyacrylamides and styrene-maleimide copolymers have been synthesized by sequential or kinetic addition of comonomers. However this approach has not yet been introduced to the synthesis of polypeptides, which are in fact polymers developed by nature in a sequence-controlled way. Polypeptides are natural materials that possess the ability to self-assemble into complex and highly ordered structures. Their folding and properties arise from precisely controlled sequences and compositions in their constituent amino acid monomers. So far, solid-phase peptide synthesis is the only technique that allows preparing short peptide sequences with excellent sequence control, but also requires extensive protection/deprotection steps and it is a difficult technique to scale-up. A new strategy towards sequence control in the synthesis of polypeptides is introduced, based on the sequential addition of α-amino acid-N-carboxyanhydrides (NCAs). The living ring-opening process is conducted to full conversion and no purification or deprotection is needed before addition of a new amino acid. The length of every block is predefined by the NCA:initiator ratio in every step. This method yields polypeptides with a specific sequence and controlled molecular weights. A series of polypeptides with varying block sequences have been synthesized with the aim to identify structure-property relationships. All of them are able to adopt secondary structures similar to natural polypeptides, and display properties in the solid state and in solution that are characteristic of the primary structure. By design the prepared polypeptides allow selective modification of individual block sequences, which has been exploited to introduce functionalities in defined positions along the polypeptide chain. Poly(ethylene glycol)(PEG) was the functionality chosen, as it is known to favor hydrophilicity and also yield thermoresponsive materials. After PEGylation, hydrophilicity of the polypeptides is enhanced, and their thermal response in H2O has been studied. Noteworthy differences in the behavior of the polypeptides having different sequences have been found. Circular dichroism measurements confirmed that the α-helical conformation is stable over the examined temperature range (5-90 °C). It is concluded that PEG units are the main responsible of the changes in H-bonding interactions with H2O upon variation of temperature, and the position of these functional units along the backbone is a factor of utmost importance in the resulting properties of the α-helical polypeptides.

Keywords: α-amino acid N-carboxyanhydrides, multiblock copolymers, poly(ethylene glycol), polypeptides, ring-opening polymerization, sequence control

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Authors: Todd R. Walton

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Social media would seem to be an ideal mechanism for crisis communication, yet it has been met with varied results. Natural disasters, such as hurricanes, provide a slow moving view of how social media can be leveraged to guide stakeholders and the public through a crisis. Crisis communication managers have struggled to reach target audiences with credible messaging. This Qualitative Evidence Synthesis (QES) analyzed the findings of eight studies published in the last year to determine how organizations effectively utilize social media for crisis communication. Additionally, the evidence was analyzed to note strategies for establishing credibility in a medium fraught with misinformation. Studies indicated wide agreement on the use of multiple social media channels in addition to frequent accurate messaging in order to establish credibility. Studies indicated mixed agreement on the use of text based emergency notification systems. The findings in this QES will help crisis communication professionals plan for social media use for crisis communication.

Keywords: crisis communication, crisis management, emergency response, social media

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Authors: Preeti Makkar, R. C. Agarwala, Vijaya Agarwala

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The present study focuses on the preparation of Al2O3 nanoparticles by top down approach i.e. mechanical milling using high energy planetary ball mill at 250 rpm for 40h. The milled Al2O3 nanoparticles are then used as the second phase to develop electroless (EL) Ni-P- Al2O3 nanocomposite coatings on mild steel substrate. An alkaline bath was used with a suspension of Al2O3 particles (4 g/L) for the synthesis of Ni-P-Al2O3 nanocomposite coating. The surface morphology, size range and phase analysis of as-prepared Al2O3 particles and the coatings were characterized using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The coatings were heat treated at 400°C for 1h in argon atmosphere and the hardness of the nanocomposite coatings was investigated with respect to Ni-P before and after heat treatment. The results showed that as milled Al2O3 nanoparticles exhibit irregular shaped and size ranges around 40-45 nm. The Al2O3 particles are uniformly distributed in Ni-P matrix. The microhardness of the coatings is found to be significantly improved after heat treatment (1126 VHN).

Keywords: Electroless (EL), Ni-P-Al2O3, nanocomposite, mechanical milling, microhardness

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Authors: M. S. M. Yusof, R. Ramli, S. K. C. Soh, N. Ismail, N. Ngah

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This study presents the synthesis of a series of methoxybenzoylthiourea amino acid derivatives. The compounds were obtained from the reactions between 2/3/4-methoxybenzoyl isothiocyanate with threonine. All of the compounds were characterized via mass spectrometry, ¹H and ¹³C NMR spectrometry, UV-Vis spectrophotometer and FT-IR spectroscopy. Mass spectra for all of the compounds showed the presence of molecular ion [M]⁺ peaks at m/z 312, which are in agreement to the calculated molecular weight. For ¹H NMR spectra, the presence of OCH₃, C=S-NH and C=O-NH protons were observed within range of δ_H 3.8-4.0 ppm, 11.1-11.5 ppm and 10.0-11.5 ppm, respectively. ¹³C NMR spectra in all compounds displayed the presence of OCH₃, C=O-NH, C=O-OH and C=S carbon resonances within range of δ_C 55.0-57.0 ppm, 165.0-168.0 ppm, 170.0-171.0 ppm and 180.0-182.0 ppm, respectively. In UV spectra, two absorption bands have been observed and both were assigned to the n-π* and π-π* transitions. Six vibrational modes of v(N-H), v(O-H), v(C=O-OH), v(C=O-NH), v(C=C) aromatic and v(C=S) appeared in the FT-IR spectra within the range of 3241-3467 cm^-1, 2976-3302 cm^-1, 1720-1768 cm^-1, 1655-1672 cm^-1, 1519-1525 cm^-1 and 754-763 cm^-1, respectively. The antibacterial activity for all of the compounds was screened against Staphylococcus aureus, Staphylococcus epidermidis, Salmonella typhimurium and Escherichia coli. However, no activity was observed.

Keywords: methoxybenzoyl isothiocyanate, amino acid, threonine, antibacterial

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Authors: Dorith Tavor, Adi Wolfson

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In the past two decades a variety of green solvents have been proposed, including water, ionic liquids, fluorous solvents, and supercritical fluids. However, their implementation in industrial processes is still limited due to their tedious and non-sustainable synthesis, lack of experimental data and familiarity, as well as operational restrictions and high cost. Several years ago we presented, for the first time, the use of glycerol-based solvents as alternative sustainable reaction mediums in both catalytic and non-catalytic organic synthesis. Glycerol is the main by-product from the conversion of oils and fats in oleochemical production. Moreover, in the past decade, its price has substantially decreased due to an increase in supply from the production and use of fatty acid derivatives in the food, cosmetics, and drugs industries and in biofuel synthesis, i.e., biodiesel. The renewable origin, beneficial physicochemical properties and reusability of glycerol-based solvents, enabled improved product yield and selectivity as well as easy product separation and catalyst recycling. Furthermore, their high boiling point and polarity make them perfect candidates for non-conventional heating and mixing techniques such as ultrasound- and microwave-assisted reactions. Finally, in some reactions, such as catalytic transfer-hydrogenation or transesterification, they can also be used simultaneously as both solvent and reactant. In our ongoing efforts to design a viable protocol that will facilitate the acceptance of glycerol and its derivatives as sustainable solvents, pure glycerol and glycerol triacetate (triacetin) as well as various glycerol-triacetin mixtures were tested as sustainable solvents in several representative organic reactions, such as nucleophilic substitution of benzyl chloride to benzyl acetate, Suzuki-Miyaura cross-coupling of iodobenzene and phenylboronic acid, baker’s yeast reduction of ketones, and transfer hydrogenation of olefins. It was found that reaction performance was affected by the glycerol to triacetin ratio, as the solubility of the substrates in the solvent determined product yield. Thereby, employing optimal glycerol to triacetin ratio resulted in maximum product yield. In addition, using glycerol-based solvents enabled easy and successful separation of the products and recycling of the catalysts.

Keywords: glycerol, green chemistry, sustainability, catalysis

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Authors: Charmaine Lamiel, Van Hoa Nguyen, Jae-Jin Shim

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Supercapacitors are energy storage devices capable of storing more energy than conventional capacitors and have higher power density than batteries. The advantages of this method include the non-use of reducing agents and acidic medium, and no further use of a post-heat treatment unlike the conventional processes, in which calcination is generally employed after obtaining the initial product. Furthermore, it also offers a shorter reaction time at low temperatures and low power requirements, which allows low fabrication and energy cost. In this study, microwave irradiation was used for the facile and rapid synthesis of mesoporous RGO@(Co,Mn)3O4 nanosheets as an electrode material. The as-prepared electrode exhibited a high capacitance of 953 F•g^−1 at 1 A•g^−1 in a 6 M KOH electrolyte solution. Moreover, the electrode exhibited a high energy density of 76.2 Wh•kg^−1 at a power density of 720 W•kg^−1, and a high power density of 7200 W•kg^−1 at an energy density of 38 Wh•kg^−1. The successful methodology was considered to be efficient and cost-effective, thereby providing an active electrode material with very promising electrochemical performance.

Keywords: cobalt-manganese oxide, electrochemical, graphene, microwave synthesis, supercapacitor

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Authors: Nidhi Gupta, Omita Nanda, Rakhi Grover, Kanchan Saxena

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Hybrid perovskite is new class of material which has gained much attention due to their different crystal structure and interesting optical and electrical properties. Easy fabrication, high absorption coefficient, and photoluminescence properties make them a strong candidate for various applications such as sensors, photovoltaics, photodetectors, etc. In perovskites, ions arrange themselves in a special type of crystal structure with chemical formula ABX3, where A is organic species like CH3NH3+, B is metal ion (e.g., Pb, Sn, etc.) and X is halide (Cl-, Br-, I-). In crystal structure, A is present at corner position, B at center of the crystal lattice and halide ions at the face centers. High stability and sensitivity of nanostructured perovskite make them suitable for chemical sensors. Researchers have studied sensing properties of perovskites for number of analytes such as 2,4,6-trinitrophenol, ethanol and other hazardous chemical compounds. Ammonia being highly toxic agent makes it a reason of concern for the environment. Thus the detection of ammonia is extremely important. Our present investigation deals with organic inorganic hybrid perovskite based ammonia sensor. Various methods like sol-gel, solid state synthesis, thermal vapor deposition etc can be used to synthesize Different hybrid perovskites. In the present work, a novel hybrid perovskite has been synthesized by a single step method. Ethylenediammnedihalide and lead halide were used as precursor. Formation of hybrid perovskite was confirmed by FT-IR and XRD. Morphological characterization of the synthesized material was performed using scanning electron microscopy (SEM). SEM analysis revealed the formation of one dimensional nanowire perovskite with mean diameter of 200 nm. Measurements for sensing properties of halide perovskite for ammonia vapor were carried out. Perovskite thin films showed a color change from yellow to orange on exposure of ammonia vapor. Electro-optical measurements show that sensor based on lead halide perovskite has high sensitivity towards ammonia with effective selectivity and reversibility. Sensor exhibited rapid response time of less than 20 seconds.

Keywords: hybrid perovskite, ammonia, sensor, nanostructure, thin film

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Authors: Angel Mauricio Castillo

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The background to the way theatrical performances and music dramas- as they were known in the mid-nineteenth century, provided the audience with a complete immersion into the feelings of the characters through poetry, music and other artistic representations which create a false sense of reality. However, a novel representation on stage some eighty years later, which is non-cathartic, is significant because it represents the antithesis to the common creations of the period and is originated by the separation of the elements as a dominant. A succinct description of the basic methodologies includes the sense of defamiliarization that results as a near translation of the German word Verfremdung will be referred to along this work as the V-effect (also known as the ‘alienation effect’) and will embody the representation of the performing techniques that enables the audience to watch a play being fully aware of its nature. A play might sometimes present the audience with a constant reminder that it is only a play; therefore, all elements will be introduced to provoke dissimilar reactions and opinions. A clear indication of the major findings of the study is that there is a strong correlation between Hegel, Marx and Brecht as it is disclosed how the didactics of Literature have been influencing not only Brecht’s productions but also every educational context in which these ideas are intertwined. The result is a new dialectical process that is to say, a new thesis that creates independent thinking skills on the part of the audience. Therefore, this model opposes to the Hegelian formula thesis-antithesis-synthesis in that the synthesis in the Brechtian theatre will inevitably fall into the category of a different thesis within an enlightening type of discourse. The confronting ideas of illusion versus reality will create a new dialectical thesis instead of resulting into a synthesis.

Keywords: Brechtian theatre, didactics, literature, education

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

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

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

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Authors: Meral Tuncbilek, Duygu Sac, Irem Durmaz, Rengul Cetin Atalay

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Nucleoside analogs are a pharmacologically diverse family that includes cytotoxic compounds, antiviral agents, and immunosuppressive molecules. Purine nucleoside derivatives such as fludarabine, cladribine, and pentostatin are significant drugs used in chemotherapy for the treatment of solid tumors and hematological malignancies. In this study, we synthesized novel purine ribonucleoside analogs containing a 4-(4-substituted phenylsulfonyl) piperazine in the substituent at N6- and O-substituted sulfonyl group at 5’-position as putative cytotoxic agents. The newly obtained compounds were then characterized for their cytotoxicity in human cancer cell lines. The 5’, 6-disubstituted 9-(β-D-ribofuranosyl)purine derivatives (44-67) were readily obtained from commercially available inosine in seven steps in very cost effective synthesis approach. The newly synthesized compounds were first evaluated for their anti-tumor activities against human liver (Huh7), colon (HCT116) and breast (MCF7) carcinoma cell lines. The IC50 values were in micromolar concentrations with 5’, 6-disubstituted purine nucleoside derivatives. Time-dependent IC50 values for each molecule were also calculated in comparison with known cytotoxic agents Camptothecin (CPT), 5-Fluorouracil (5-FU), Cladribine, Pentostatine and Fludarabine. N6-(4-trifluoromethyl phenyl) / N6-(4-bromophenyl) and 5’-O-(4-methoxybenzene sulfonyl) / 5’-O-(benzenesulfonyl) derivatives 54, 64 displayed the best cytotoxic activity with IC50 values of 8.8, 7 µM against MCF7 cell line. The N6-(4-methylphenyl) analog 50 was also very active (IC50= 10.7 μM) against HCT116 cell line. Furthermore, compound 64 had a better cytotoxic activity than the known cell growth inhibitors 5-FU and Fludarabine on Huh7 (1.5 vs 30.7, 29.9 μM for 5-FU and Fludarabine).

Keywords: cytotoxic activity, Huh7, HCT116, MCF7, nucleoside, synthesis

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Authors: Titus Y. Ngmenzuma, Cherian. Mathews, Feilx D. Dakora

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In Africa, poor nutrient availability, particularly N and P, coupled with low soil moisture due to erratic rainfall, constitutes the major crop production constraints. Although inorganic fertilizers are an option for meeting crop nutrient requirements for increased grain yield, the high cost and scarcity of inorganic inputs make them inaccessible to resource-poor farmers in Africa. Because crops grown on such nutrient-poor soils are micronutrient deficient, incorporating N₂-fixing legumes into cropping systems can sustainably improve crop yield and nutrient accumulation in the grain. In Africa, groundnut can easily form an effective symbiosis with native soil rhizobia, leading to marked N contribution in cropping systems. In this study, field experiments were conducted at Blesbokfontein in Mpumalanga Province to assess N₂ fixation and N contribution by 30 groundnut varieties during the 2018/2019 planting season using the ¹⁵N natural abundance technique. The results revealed marked differences in shoot dry matter yield, symbiotic N contribution, soil N uptake and grain yield among the groundnut varieties. The percent N derived from fixation ranged from 37 to 44% for varieties ICGV131051 and ICGV13984. The amount of N-fixed ranged from 21 to 58 kg/ha for varieties Chinese and IS-07273, soil N uptake from 31 to 80 kg/ha for varieties IS-07947 and IS-07273, and grain yield from 193 to 393 kg/ha for varieties ICGV15033 and ICGV131096, respectively. Compared to earlier studies on groundnut in South Africa, this study has shown low N₂ fixation and N contribution to the cropping systems, possibly due to environmental factors such as low soil moisture. Because the groundnut varieties differed in their growth, symbiotic performance and grain yield, more field testing is required over a range of differing agro-ecologies to identify genotypes suitable for different cropping environments

Keywords: ¹⁵N natural abundance, percent N derived from fixation, amount of N-fixed, grain yield

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Authors: Francisco Vidal Vázquez, Pekka Simell, Christian Frilund, Matti Reinikainen, Ilkka Hiltunen, Tim Böltken, Benjamin Andris, Paolo Piermartini

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Carbon capture and utilization (CCU) are one of the key topics in mitigation of CO2 emissions. There are many different technologies that are applied for the production of diverse chemicals from CO2 such as synthetic natural gas, Fischer-Tropsch products, methanol and polymers. Power-to-Gas and Power-to-Liquids concepts arise as a synergetic solution for storing energy and producing value added products from the intermittent renewable energy sources and CCU. VTT is a research and technology development company having energy in transition as one of the key focus areas. VTT has extensive experience in piloting and upscaling of new energy and chemical processes. Recently, VTT has developed and commissioned a Mobile Synthesis Unit (MOBSU) in close collaboration with INERATEC, a spin-off company of Karlsruhe Institute of Technology (KIT, Germany). The MOBSU is a multipurpose synthesis unit for CO2 upgrading to energy carriers and chemicals, which can be transported on-site where CO2 emission and renewable energy are available. The MOBSU is initially used for production of fuel compounds and chemical intermediates by combination of two consecutive processes: reverse Water-Gas Shift (rWGS) and Fischer-Tropsch synthesis (FT). First, CO2 is converted to CO by high-pressure rWGS and then, the CO and H2 rich effluent is used as feed for FT using an intensified reactor technology developed and designed by INERATEC. Chemical equilibrium of rWGS reaction is not affected by pressure. Nevertheless, compression would be required in between rWGS and FT in the case when rWGS is operated at atmospheric pressure. This would also require cooling of rWGS effluent, water removal and reheating. For that reason, rWGS is operated using precious metal catalyst in the MOBSU at similar pressure as FT to simplify the process. However, operating rWGS at high pressures has also some disadvantages such as methane and carbon formation, and more demanding specifications for materials. The main parts of FT module are an intensified reactor, a hot trap to condense the FT wax products, and a cold trap to condense the FT liquid products. The FT synthesis is performed using cobalt catalyst in a novel compact reactor technology with integrated highly-efficient water evaporation cooling cycle. The MOBSU started operation in November 2016. First, the FT module is tested using as feedstock H2 and CO. Subsequently, rWGS and FT modules are operated together using CO2 and H2 as feedstock of ca. 5 Nm3/hr total flowrate. On spring 2017, The MOBSU unit will be integrated together with a direct air capture (DAC) of CO2 unit, and a PEM electrolyser unit at Lappeenranta University of Technology (LUT) premises for demonstration of the SoletAir concept. This would be the first time when synthetic fuels are produced by combination of DAC unit and electrolyser unit which uses solar power for H2 production.

Keywords: CO2 utilization, demonstration, Fischer-Tropsch synthesis, intensified reactors, reverse water-gas shift

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Authors: Hoang Thi Quynh, Shima Kazuto

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Organic farming is gaining interest in Vietnam. However, organic fertilizer production is not sufficiently regulated, resulting in unknown quality. This study investigated characteristics of so-called organic fertilizers in the Vietnam’s market and their mineralization in soil-plant system. We collected 15 commercial products (11 domestic and 4 imported) which labelled 'organic fertilizer' in the market to analyze nutrients composition. A 20 day-incubation experiment was carried on with 80 g sandy-textured soil, amended with the fertilizer at a rate of 109.4 mgN.kg⁻¹soil in 150 mL glass bottle at 25℃. We categorized them according to nutrients content and mineralization rate, and then selected 8 samples for cultivation experiment. The experiment was conducted by growing Komatsuna (Brassica campestris) in sandy-textured soil using an automatic watering apparatus in a greenhouse. The fertilizers were applied to the top one-third of the soil stratum at a rate of 200 mgN.kg⁻¹ soil. Our study also analyzed material flow of coffee husk compost in Central Highland of Vietnam. Total N, P, K, Ca, Mg and C: N ratio varied greatly cross the domestic products, whereas they were quite similar among the imported materials. The proportion of inorganic-N to T-N of domestic products was higher than 25% in 8 of 11 samples. These indicate that N concentration increased dramatically in most domestic products compared with their raw materials. Additionally, most domestic products contained less P, and their proportions of Truog-P to T-P were greatly different. These imply that some manufactures were interested in adjusting P concentration, but some ones were not. Furthermore, the compost was made by mixing with chemical substances to increase nutrients content (N, P), and also added construction surplus soil to gain weight before packing product to sell in the market as 'organic fertilizer'. There was a negative correlation between C:N ratio and mineralization rate of the fertilizers. There was a significant difference in N efficiency among the fertilizer treatments. N efficiency of most domestic products was higher than chemical fertilizer and imported organic fertilizers. These results suggest regulations on organic fertilizers production needed to support organic farming that is based on internationally accepted standards in Vietnam.

Keywords: inorganic N, mineralization, N efficiency, so-called organic fertilizers, Vietnam’s market

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Authors: Ming Su, Ziqiang Mu

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This paper proposes a synthesis method for nonuniform linear antenna arrays that combine Gaussian process regression (GPR) and genetic algorithm (GA). In this method, the GPR model can be used to calculate the array radiation pattern in the presence of mutual coupling effects, and then the GA is used to optimize the excitations and locations of the elements so as to generate the desired radiation pattern. In this paper, taking a 9-element nonuniform linear array as an example and the desired radiation pattern corresponding to a Chebyshev distribution as the optimization objective, optimize the excitations and locations of the elements. Finally, the optimization results are verified by electromagnetic simulation software CST, which shows that the method is effective.

Keywords: nonuniform linear antenna arrays, GPR, GA, mutual coupling effects, active element pattern

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Authors: Satyendra P. Chaurasia, Aditi Sharma, Ajay K. Dalai

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The esterification of Docosahexaenoic acid (DHA) with glycerol using immobilized Mucor mie-hei lipase (MML) and Rhizopus oryzae lipase (ROL) have been studied in the present paper to synthesize triglycerides (TG) rich in DHA. Both immobilized lipases (MML and ROL), and their support materials (immobead-150 and ion-exchange resin) were characterized and compared for surface properties with BET, for chemical functional groups with FT-IR, and for particle size distribution with particle size analyzer. The most suitable reaction conditions for synthesis of DHA rich TG in biphasic solvent system were found as 1:3 (wt/wt) glycerol to DHA ratio, 1:1 (wt/wt) buffer to DHA ratio, 1:1 (wt/wt) solvent to DHA ratio at 50 ºC temperature, and 600 rpm speed of agitation with 100 mg of immobilized lipases. Maximum 95.9 % esterification was obtained with immobilized MML in 14 days reaction with formation of 65.7 wt% DHA rich TG. Whereas, immobilized ROL has shown formation of only 23.8 wt% DHA rich TG with total 78.9 % esterification in 15 days. Additionally, repeated use of both immobilized lipases was con-ducted up to five cycles, indicated 50.4% and 41.2 % activity retention after fifth repeated use of immobilized MML and ROL, respectively.

Keywords: DHA, immobilized Mucor miehei lipase, Rhizopus oryzae lipase, esterification

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Authors: W. Mazari, K. Boucherit, Z. Boucherit-Otmani, M. N. Rahmoun, M. Benabdallah

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The hospital or any other establishment of care can be considered as an ecosystem where the patient comes into contact with a frightening microbial universe and a risk to contract infection that is referred to as nosocomial or health care-associated. In these last years, the incidence of these infections has risen sharply. Several microorganisms are the cause of these nosocomial infections and the emergence of resistance of the microbial strains against antibiotics creates a danger to public health. The search for new antimicrobial agents to overcome this problem has produced interesting compounds through chemical synthesis, which plays a very important role in the research and discovery of new drugs. It is in this framework that our study was conducted at our laboratory and it involves evaluating the antibacterial activity of thirteen 2-pyridone derivatives synthesized by two methods, the diffusion disc method and the dilution method against eight Gram negative bacterial strains. The results seem interesting especially for two products that have shown the best activities against Escherichia coli ATCC 25922 and Enterobacter cloacae ATCC 13047 with CMI of 512µg/ml.

Keywords: heterocyclic derivatives, chemical synthesis, antimicrobial activity, biotechnology

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Authors: B.Benalioua, I.Benyamina, A.Bentouami, B.Boury

Abstract:

The objective of this study is based on the synthesis of a new photocatalyst based on TiO2 and its application in the photo-degradation of an acid dye under the visible light. The material obtained was characterized by different techniques like diffuse reflectance UV–Vis spectroscopy (DRS), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic efficiency of the Bi, Zn co-doped TiO2 treated at 670°C for 2 h was tested on the Indigo Carmine under the irradiation of visible light and compared with that of the commercial titanium oxide TiO2-P25 (Degussa). The XRD characterization of the material Bi-Zn-TiO2 (670°C) revealed the presence of the anatase phase and the absence of the rutile phase in comparison of the TiO2 P25 diffractogram. Characterization by UV- visible diffuse reflection (DRS) material showed that the Bi-Zn-TiO2 exhibits redshift (move visible) relative to commercial titanium oxide TiO2-P25, this property promises a photocatalytic activity of Bi-Zn-TiO2 under visible light. Indeed, the efficiency of photocatalytic Bi-Zn-TiO2 as a visible light is shown by a complete discoloration of indigo carmine solution of 16 mg/L after 70 minutes, whereas with the P25-TiO2 discoloration is achieved after 120 minutes.

Keywords: POA, heterogeneous photocatalysis, TiO2, co-doping

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Authors: B. Benalioua, I. Benyamina, A. Bentouami, B. Boury

Abstract:

The objective of this study is based on the synthesis of a new photocatalyst based on TiO2 and its application in the photo-degradation of an acid dye under the visible light. The material obtained was characterized by different techniques like diffuse reflectance UV–Vis spectroscopy (DRS), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic efficiency of the S, N co-doped TiO2 treated at 600°C for 1 h was tested on the Indigo Carmine under the irradiation of visible light and compared with that of the commercial titanium oxide TiO2-P25 (Degussa). The XRD characterization of the material S-N-TiO2 (600°C) revealed the presence of the anatase phase and the absence of the rutile phase in comparison of the TiO2 P25 diffractogram. Characterization by UV- visible diffuse reflection (DRS) material showed that the S-N-TiO2 exhibits redshift (move visible) relative to commercial titanium oxide TiO2-P25, this property promises a photocatalytic activity of S-N-TiO2 under visible light. Indeed, the efficiency of photocatalytic S-N-TiO2 as a visible light is shown by a complete discoloration of indigo carmine solution of 16 mg/L after 40 minutes, whereas with the P25-TiO2 discoloration is achieved after 90 minutes.

Keywords: POA, heterogeneous photocatalysis, TiO2, co-doping

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Authors: Hummera Rafique, Aamer Saeed

Abstract:

Synthesis of structural analogues of various well known bioactive natural 3,4-dihydroisocoumarins viz. Scorzocreticin, Annulatomarin, Montroumarin, and Thunberginol B, have been carried out starting from 3,5-dimethoxy-4-methylphenyl acetic acid. 3,5-Dimethoxy-4-methylphenyl acetic acid was then condensed with various aryl acid chlorides (a-e) to afford the corresponding 6,8-dimethoxy-7-methyl-3-aryl isocoumarins (5a-e). The alkaline hydrolysis of isocoumarins yields keto-acids (3a-e), which were then reduced to hydroxyacids, followed by cyclodehydration with acetic anhydride furnish corresponding 3,4-dihydroisocoumarins (7a-e). Finally, demethylation of 3,4-dihydroisocoumarins was carried out to afford 6,8-dihydroxy-7-methyl-3-aryl-3,4-dihydroisocoumarins (7a-e). Antibacterial evaluation of all the synthesized compounds were carried out against ten bacterial strains, it was concluded that isocoumarins (5a-e) and 3,4-dihydroisocoumarins (7a-e) are more active against gram positive bacteria then gram negative. However, the 6,8-dihydroxy-3,4-dihydroisocoumarin derivatives (8a-e) are more active against gram negative then gram positive.

Keywords: 3, 5-Dimethoxy-4-methylhomophthalic acid, natural 3, 4-Dihydroisocoumarin analogues, antibacterial activity, isocoumarins, demethylation

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Authors: Suneeta Kumari, Abanti Sahoo

Abstract:

Industrial effluents treatment is a major problem in the world. All wastewater treatment methods have some problems in the environment. Due to this reason, today many natural biopolymers are being used in the waste water treatment because those are safe for our environment. In this study, synthesis and characterization of polyethersulfone/chitosan membranes (Thin film composite membrane) are carried out. Fish scales are used as raw materials. Different characterization techniques such as Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), scanning electron microscope (SEM) and Thermal gravimetric analysis (TGA) are analysed for the synthesized membrane. The performance of membranes such as flux, rejection, and pore size are also checked. The synthesized membrane is used for the treatment of steel industry waste water where Biochemical oxygen demand (BOD), Chemical Oxygen Demand (COD), pH, colour, Total dissolved solids (TDS), Total suspended solids (TSS), Electrical conductivity (EC) and Turbidity aspects are analysed.

Keywords: fish scale, membrane synthesis, treatment of industrial effluents, chitosan

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

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Polyaniline/gold (PANI/Au) nanocomposite was prepared by in-situ chemical oxidation polymerization method. The synthesis involved the formation of polyaniline-gold nanocomposite, by in-situ redox reaction and the dispersion of gold nano particles throughout the polyaniline matrix. The nanocomposites were characterized by XRD, FTIR, TEM and UV-visible spectroscopy. The characteristic peaks in FTIR and UV-visible spectra confirmed the expected structure of polymer as reported in the literature. Further, transmission electron microscopy (TEM) confirmed the formation of gold nano particles. The crystallite size of 30 nm for nanoAu was supported by the XRD pattern. Further, the A.C. conductivity, dielectric constant (€’(w)) and dielectric loss (€’’(w)) of PANI/Au nano composite was measured using impedance analyzer. The effect of doping on the conductivity was investigated. The antibacterial activity was examined for this nano composite and it was observed that PANI/Au nanocomposite could be used as an antibacterial agent.

Keywords: AC-conductivity, anti-microbial activity, dielectric constant, dielectric loss, polyaniline/gold (PANI/AU) nanocomposite

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Authors: Mahmoud Elrouby

Abstract:

Metal chalcogenide materials have wide spectrum of properties, for that these materials can be used in electronics, optics, magnetics, solar energy conversion, catalysis, passivation, ion sensing, batteries, and fuel cells. This work aims to, how can obtain these materials via electrochemical methods simply for further applications. The work regards in particular the systems relevant to the sulphur sub-group elements, i.e., sulphur, selenium, and tellurium. The role of electrochemistry in synthesis, development, and characterization of the metal chalcogenide materials and related devices is vital and important. Electrochemical methods as preparation tool offer the advantages of soft chemistry to access bulk, thin, nano film and epitaxial growth of a wide range of alloys and compounds, while as a characterization tool provides exceptional assistance in specifying the physicochemical properties of materials. Moreover, quite important applications and modern devices base their operation on electrochemical principles. Thereupon, our scope in the first place was to organize existing facts on the electrochemistry of metal chalcogenides regarding their synthesis, properties, and applications.

Keywords: electrodeposition, metal chacogenides, semiconductors, applications

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Authors: Efrain Rodriguez, Cristhian Riano, Alberto Alvares

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In recent years, robots manipulators with parallel architectures are used in additive manufacturing processes – 3D printing. These robots have advantages such as speed and lightness that make them suitable to help with the efficiency and productivity of these processes. Consequently, the interest for the development of parallel robots for additive manufacturing applications has increased. This article deals with the conceptual design and dimensional synthesis of the linear delta robot for additive manufacturing. Firstly, a methodology based on structured processes for the development of products through the phases of informational design, conceptual design and detailed design is adopted: a) In the informational design phase the Mudge diagram and the QFD matrix are used to aid a set of technical requirements, to define the form, functions and features of the robot. b) In the conceptual design phase, the functional modeling of the system through of an IDEF0 diagram is performed, and the solution principles for the requirements are formulated using a morphological matrix. This phase includes the description of the mechanical, electro-electronic and computational subsystems that constitute the general architecture of the robot. c) In the detailed design phase, a digital model of the robot is drawn on CAD software. A list of commercial and manufactured parts is detailed. Tolerances and adjustments are defined for some parts of the robot structure. The necessary manufacturing processes and tools are also listed, including: milling, turning and 3D printing. Secondly, a dimensional synthesis method applied on design of the linear delta robot is presented. One of the most important key factors in the design of a parallel robot is the useful workspace, which strongly depends on the joint space, the dimensions of the mechanism bodies and the possible interferences between these bodies. The objective function is based on the verification of the kinematic model for a prescribed cylindrical workspace, considering geometric constraints that possibly lead to singularities of the mechanism. The aim is to determine the minimum dimensional parameters of the mechanism bodies for the proposed workspace. A method based on genetic algorithms was used to solve this problem. The method uses a cloud of points with the cylindrical shape of the workspace and checks the kinematic model for each of the points within the cloud. The evolution of the population (point cloud) provides the optimal parameters for the design of the delta robot. The development process of the linear delta robot with optimal dimensions for additive manufacture is presented. The dimensional synthesis enabled to design the mechanism of the delta robot in function of the prescribed workspace. Finally, the implementation of the robotic platform developed based on a linear delta robot in an additive manufacturing application using the Fused Deposition Modeling (FDM) technique is presented.

Keywords: additive manufacturing, delta parallel robot, dimensional synthesis, genetic algorithms

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Authors: Abdullah Alsehaimi

Abstract:

Over decades, there have been many studies of delay in construction, and this type of study continues to be popular in construction management research. A synthesis and critical evaluation of delay studies in developing countries reveals that poor project management is cited as one of the main causes of delay. However, despite such consensus, most of the previous studies fall short in providing clear recommendations demonstrating how project management practice could be improved. Moreover, the majority of recommendations are general and not devoted to solving the difficulties associated with particular delay causes. This paper aims to demonstrate that the root cause of this state of affairs is that typical research into delay tends to be descriptive and explanatory, making it inadequate for solving persistent managerial problems in construction. It is contended that many problems in construction could be mitigated via alternative research approaches, i.e. action and constructive research. Such prescriptive research methods can assist in the development and implementation of innovative tools tackling managerial problems of construction, including that of delay. In so doing, those methods will better connect research and practice, and thus strengthen the relevance of academic construction management.

Keywords: construction delay, action research, constructive research, industrial engineering

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Authors: D. A. S. Gamage, B. F. A Basnayake, W. A. J. M. de Costa

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Rice is one of the world’s most important cereals. Increasing food production both to meet in-country requirements and to help overcome food crises is one of the major issues facing Sri Lanka today. However, productive land is limited and has mostly been utilized either for food crop production or other uses. Agriculture plays an important and strategic role in the performance of Sri Lankan national economy. A variety of modern agricultural inputs have been introduced, namely ploughs and harvesters, pesticides, fertilizers and lime. Besides, there are several agricultural institutions developing and updating the management of agricultural sector. Modern agricultural inputs cooperate as a catalyst in raising the productivity. However, in the eagerness of gaining profits from the efficient and productive techniques, this modern agricultural input has affected the environment and living things especially those which have been blended from various chemical substance. The increased pressure to maintain a high level of rice output for consumption has resulted in increased use of pesticides and inorganic fertilizer on rice fields in Sri Lanka. The application of inorganic fertilizer has become a burdened to the country in many ways. The excessive reuse of the ground water resources with a considerable application of organic and chemical fertilizers will lead to a deterioration of the quality and quantity of water. Biochar is a form of charcoal produced through the heating of natural organic materials. It has received significant attention recently for its potential as a soil conditioner, a fertilizer and as a means of storing carbon in a sustainable manner. It is the best solution for managing the agricultural wastes while providing a useful product for increasing agricultural productivity and protecting the environment. The objective of this study was to evaluate rice husk charcoal coated urea as a slow releasing fertilizer and compare the total N, P, K, organic matter in soil and yield of rice production.

Keywords: biochar, paddy husk, soil conditioner, rice straw compost

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Authors: Mohamedou El Boukhary, Farba Bouyagui Tamboura, A. Hamady Barry, T. Moussa Seck, Mohamed L. Gaye

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Nowadays, low-schiff acyl-hydrazone ligands are highly sought after due to their wide applications in various fields of biology, coordination chemistry, and catalysis. They are studied for their antioxidant, antibacterial and antiviral properties. The complexes of transition metals and the lanthanide they derive are well known for their magnetic, optical, and catalytic properties. In this work, we present the synthesis of an acyl-hydrazone (H2L) schiff base and their 3d transition complexes. The ligand (H2L) is characterized by IR, NMR (1H; 13C) spectroscopy. The complexes are characterized by different physic-chemical techniques such as IR, UV-visible, conductivity, measurement of magnetic susceptibility. The study of XRD allowed us to elucidate the crystalline structure of the manganese (Mn) complex. The asymmetric unit of the complex is composed of two molecules of the ligand, one manganese (II) ion, and two coordinate chloride ions; the environment around Mn is described as a pentagonal base bipyramid. In the crystal lattice, the asymmetric unit is bound by hydrogen bonds.

Keywords: synthene, acyl-hydrazone, 3D transition metal complex, application

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Authors: Krishnakant Bhole, Neerakallu D. Shivakumar, Shakti Singh Chauhan, Sanketh Tonannavar, Rajath S

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Synthesis of natural-based composite materials is state of the art. This work discusses the preparation and characterization of cellulose nanofibers (CNF) extracted from the bamboo pulp using TEMPO-oxidization and high-pressure homogenization methods. Bio-composites are prepared using synthesized CNF and bamboo particles. Nanocellulose prepared is characterized using SEM and XRD for morphological and crystallinity analysis, and the formation of fibers at the nano level is ensured. Composite specimens are fabricated using these natural sources and subjected to tensile and flexural tests to characterize the mechanical properties such as modulus of elasticity (MOE), modulus of rupture (MOR), and interfacial strength. Further, synthesized nanocellulose is used as a binding agent to prepare particleboards using various natural sources like bamboo, areca nut, and banana in the form of fibers. From the results, it can be inferred that nanocellulose prepared from bamboo pulp acts as a binding agent for making bio-composites. Hence, the concept of using matrix and reinforcement derived from natural sources can be used to prepare green composites that are highly degradable.

Keywords: nanocellulose, biocomposite, CNF, bamboo

Procedia PDF Downloads 87