Search results for: synthesis process

Authors: Jessica Carolina Hernandez Galeano, Juan Carlos Moreno Pirajan, Liliana Giraldo

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Carbon gels are materials whose structure and porous texture can be designed and controlled on a nanoscale. Among their characteristics it is found their low density, large surface area and high degree of porosity. These materials are produced by a sol-gel polymerization of organic monomers using basic or acid catalysts, followed by drying and controlled carbonization. In this work, the synthesis and characterization of carbon aerogels from resorcinol, phenol and formaldehyde in ethanol is described. The aim of this study is obtaining different carbonaceous materials in the form of spheres using the Stöber method to perform a further evaluation of CO₂ adsorption of each material. In general, the synthesis consisted of a sol-gel polymerization process that generates a cluster (cross-linked organic monomers) from the precursors in the presence of NH₃ as a catalyst. This cluster was subjected to specific conditions of gelling and curing (30°C for 24 hours and 100°C for 24 hours, respectively) and CO₂ supercritical drying. Finally, the dry material was subjected to a process of carbonization or pyrolysis, in N₂ atmosphere at 350°C (1° C / min) for 2 h and 600°C (1°C / min) for 4 hours, to obtain porous solids that retain the structure initially desired. For this work, both the concentrations of the precursors and the proportion of ammonia in the medium where modify to describe the effect of the use of phenol and the amount of catalyst in the resulting material. Carbon aerogels were characterized by Scanning Electron Microscope (SEM), N₂ isotherms, infrared spectroscopy (IR) and X-ray Powder Diffraction (XRD) showing the obtention of carbon spheres in the nanometric scale with BET areas around 500 m2g-1.

Keywords: carbon aerogels, carbon spheres, CO₂ adsorption, Stöber method

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Authors: Pervaiz Ahmad, Mayeen Uddin Khandaker, Yusoff Mohd Amin

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A unique cone-like morphologies of boron nitride microtubes with larger internal space and thin walls structure are synthesized in a dual zone quartz tube furnace at 1200 ° C with ammonia as a reaction atmosphere. The synthesized microtubes are found to have diameter in the range of 1 to ̴ 2 μm with walls thickness estimated from 10 – 100 nm. XPS survey shows N 1s and B 1s peaks at 398.7 eV and 191 eV that represent h-BN in the sample. Raman spectroscopy indicates a high intensity peak at 1372.53 (cm-1) that corresponds to the E2g mode of h-BN.

Keywords: BNMTs, synthesis, reaction atmosphere, growth

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Authors: Reza Behtash, Enayat Enayati

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The pool condenser is in principal a horizontal reactor, containing a bundle of U-tubes for heat exchange, coupling to low pressure steam drum. Condensation of gas takes place in a condensed pool around the tubes of the condenser. The heat of condensation is removed by the generation of low pressure steam on the inner tube side of the bundle. A circulation pump transfers ample boiler feed water to these tubes. The pressure of the steam generated influenced the heat flux. Changing the steam pressure means changing the steam condensate temperature and therefore the temperature difference between the tube side and the shell side. 2NH3 + CO2 ↔ NH2COONH4 + Heat. This reaction is exothermic and according to Le Chatelier's Principle if the heat is not removed enough, it will come back to left side and generate of the gas and so the Urea synthesis pressure will rise. The most principal reasons for high Urea synthesis pressure are non proportional of Ammonia/Dioxide Carbon ratio and too high a pressure in low pressure steam drum. Proportional of Ammonia/Dioxide Carbon ratio is 3.0 and normal pressure for low pressure steam drum is 4.5 bar. As regards these conditions were proportional but we could not control the synthesis pressure the plant endangered, therefore we had to control the steam drum pressure at about 3.5 bar. While we opened the pool condenser, we found the partition plate used to divide inlet and outlet boiler feed water to tubes, was broken partially and so amount of boiler feed water bypass the tubes and the heat was not removed totally and it resulted in the generation of gases and high pressure in synthesis.

Keywords: boiler, pressure, pool condenser, partition plate

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Authors: Adel S. El-Azab, Alaa A. M. Abdel-Aziz, Ibrahim A. Al-Suwaidan, Amer M. Alanazi

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A novel series of 2,3,6-trisubstitute quinazolinone were designed, synthesized, and evaluated for their in-vitro antitumor activity. 3 (Benzylideneamino)-6-chloro-2-p-tolylquinazolin-4(3H)-One, 2-[(4-oxo-3-phenethyl-3,4-dihydroquinazolin-2-yl)thio]-N-(3,4;5-trimethoxyphenyl) acetamide and 3-(3-benzyl-6-methyl-4-oxo-3, 4-dihydroquinazolin-2-ylthio)-N-(3,4,5-trimethoxyphenyl) propanamide have shown amazing broad spectrum antitumor activity with mean GI50; 15.8, 3.16, and 7.4 μM respectively compared to known Quinazoline Derivatives antitumor drug 5-FU mean GI50=22.6 μM.

Keywords: quinazoline derivatives, in vitro antitumor, synthesis, 5-FU, NCI

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Authors: Pauline Bredy, Yves Schuurman, David Farrusseng

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To fulfill climate objectives, the production of synthetic e-fuels using CO₂ as a raw material appears as part of the solution. In particular, Power-to-Liquid (PtL) concept combines CO₂ with hydrogen supplied from water electrolysis, powered by renewable sources, which is currently gaining interest as it allows the production of sustainable fossil-free liquid fuels. The proposed process discussed here is an upgrading of the well-known Fischer-Tropsch synthesis. The concept deals with two cascade reactions in one pot, with first the conversion of CO₂ into CO via the reverse water gas shift (RWGS) reaction, which is then followed by the Fischer-Tropsch Synthesis (FTS). Instead of using a Fe-based catalyst, which can carry out both reactions, we have chosen the strategy to decouple the two functions (RWGS and FT) on two different catalysts within the same reactor. The FTS shall shift the equilibrium of the RWGS reaction (which alone would be limited to 15-20% of conversion at 250°C) by converting the CO into hydrocarbons. This strategy shall enable optimization of the catalyst pair and thus lower the temperature of the reaction thanks to the equilibrium shift to gain selectivity in the liquid fraction. The challenge lies in maximizing the activity of the RWGS catalyst but also in the ability of the FT catalyst to be highly selective. Methane production is the main concern as the energetic barrier of CH₄ formation is generally lower than that of the RWGS reaction, so the goal will be to minimize methane selectivity. Here we report the study of different combinations of copper-based RWGS catalysts with different cobalt-based FTS catalysts. We investigated their behaviors under mild process conditions by the use of high-throughput experimentation. Our results show that at 250°C and 20 bars, Cobalt catalysts mainly act as methanation catalysts. Indeed, CH₄ selectivity never drops under 80% despite the addition of various protomers (Nb, K, Pt, Cu) on the catalyst and its coupling with active RWGS catalysts. However, we show that the activity of the RWGS catalyst has an impact and can lead to longer hydrocarbons chains selectivities (C₂⁺) of about 10%. We studied the influence of the reduction temperature on the activity and selectivity of the tandem catalyst system. Similar selectivity and conversion were obtained at reduction temperatures between 250-400°C. This leads to the question of the active phase of the cobalt catalysts, which is currently investigated by magnetic measurements and DRIFTS. Thus, in coupling it with a more selective FT catalyst, better results are expected. This was achieved using a cobalt/iron FTS catalyst. The CH₄ selectivity dropped to 62% at 265°C, 20 bars, and a GHSV of 2500ml/h/gcat. We propose that the conditions used for the cobalt catalysts could have generated this methanation because these catalysts are known to have their best performance around 210°C in classical FTS, whereas the iron catalysts are more flexible but are also known to have an RWGS activity.

Keywords: cobalt-copper catalytic systems, CO₂-hydrogenation, Fischer-Tropsch synthesis, hydrocarbons, low-temperature process

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Authors: Mohamed Hassan Abdullahi

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Decomposition is used as a synthesis tool in several physical systems. It can also be used for tearing and restructuring, which is large-scale system analysis. On the other hand, the commutativity of series-connected systems has fascinated the interest of researchers, and its advantages have been emphasized in the literature. The presentation looks into the necessary conditions for decomposing any third-order discrete-time linear time-varying system into a commutative pair of first- and second-order systems. Additional requirements are derived in the case of nonzero initial conditions. MATLAB simulations are used to verify the findings. The work is unique and is being published for the first time. It is critical from the standpoints of synthesis and/or design. Because many design techniques in engineering systems rely on tearing and reconstruction, this is the process of putting together simple components to create a finished product. Furthermore, it is demonstrated that regarding sensitivity to initial conditions, some combinations may be better than others. The results of this work can be extended for the decomposition of fourth-order discrete-time linear time-varying systems into lower-order commutative pairs, as two second-order commutative subsystems or one first-order and one third-order commutative subsystems.

Keywords: commutativity, decomposition, discrete time-varying systems, systems

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Authors: Juan C. Duran-Alvarez, Daniel Mejia, Rodolfo Zanella

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Heterogeneous photocatalysis is a promising method to achieve the complete degradation and mineralization of organic pollutants in water via their exhaustive oxidation. In order to take this advanced oxidation process towards sustainability, it is necessary to reduce the energy consumption, referred as the light sources and the post-treatment operations. For this, the synthesis of new nanostructures of low band gap semiconductors in the form of thin films is in continuous development. In this work, thin films of the low band gap semiconductor bismuth oxyiodide (BiOI) were synthesized via the Successive Ionic Layer Adsorption and Reaction (SILAR) method. For this, Bi(NO3)3 and KI solutions were prepared, and glass supports were immersed in each solution under strict rate and time immersion conditions. Synthesis was performed at room temperature and a washing step was set prior to each immersion. Thin films with an average thickness below 100 nm were obtained upon a cycle of 30 immersions, as determined by AFM and profilometry measurements. Cubic BiOI nanocrystals with average size of 17 nm and a high orientation to the 001 plane were observed by XRD. In order to optimize the synthesis method, several Bi/I ratios were tested, namely 1/1, 1/5, 1/10, 1/20 and 1/50. The highest crystallinity of the BiOI films was observed when the 1/5 ratio was used in the synthesis. Non-stoichiometric conditions also resulted in the highest uniformity of the thin layers. PVP was used as an additive to improve the adherence of the BiOI thin films to the support. The addition of 0.1 mg/mL of PVP during the washing step resulted in the highest adherence of the thin films. In photocatalysis tests, degradation rate of the antibiotic ciprofloxacin as high as 75% was achieved using visible light (380 to 700 nm) irradiation for 5 h in batch tests. Mineralization of the antibiotic was also observed, although in a lower extent; ~ 30% of the total organic carbon was removed upon 5 h of visible light irradiation. Some ciprofloxacin by-products were identified throughout the reaction; and some of these molecules displayed residual antibiotic activity. In conclusion, it is possible to obtain highly oriented BiOI thin films under ambient conditions via the SILAR method. Non-stoichiometric conditions using PVP additive are necessary to increase the crystallinity and adherence of the films, which are photocatalytically active to remove recalcitrant organic pollutants under visible light irradiation.

Keywords: bismuth oxyhalides, photocatalysis, thin films, water treatment

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Authors: Özlen Altun, Zeliha Yoruç

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In the present study, the reactions involving 4-Bromo-2,6-bis-hydroxymethyl-phenol (BBHMP) and nikotinamide (NA) in the presence Pd (II) ion were investigated. Optimum conditions for the reactions were established as pH 7 and λ = 450 nm. According to absorbance measurements, the mole ratio of BBHMP : NA : Pd2+ was found as 1 : 2 : 2. As a result of physico-chemical, spectrophotometric and thermal analysis results, the reactions of BBHMP and NA with Pd (II) is complexation reactions and one molecule BBHMP and two molecules of NA react with two molecules of metal (II) ion.

Keywords: 4-Bromo-2, 6-bis-hydroxymethyl-phenol, nicotinamide, Pd(II), spectral analysis, synthesis

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Authors: Shringika Soni, Utkarsh Jain, Nidhi Chauhan

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Aptamers are recently discovered ~80-100 bp long artificial oligonucleotides that not only demonstrated their applications in therapeutics; it is tremendously used in diagnostic and sensing application to detect different biomarkers and drugs. Synthesizing aptamers for proteins or genomic template is comparatively feasible in laboratory, but drugs or other chemical target based aptamers require major specification and proper optimization and validation. One has to optimize all selection, amplification, and characterization steps of the end product, which is extremely time-consuming. Therefore, we performed asymmetric PCR (polymerase chain reaction) for random oligonucleotides pool synthesis, and further use them in Systematic evolution of ligands by exponential enrichment (SELEX) for anti-psychotic drugs based aptamers synthesis. Anti-psychotic drugs are major tranquilizers to control psychosis for proper cognitive functions. Though their low medical use, their misuse may lead to severe medical condition as addiction and can promote crime in social and economical impact. In this work, we have approached the in-vitro SELEX method for ssDNA synthesis for anti-psychotic drugs (in this case ‘target’) based aptamer synthesis. The study was performed in three stages, where first stage included synthesis of random oligonucleotides pool via asymmetric PCR where end product was analyzed with electrophoresis and purified for further stages. The purified oligonucleotide pool was incubated in SELEX buffer, and further partition was performed in the next stage to obtain target specific aptamers. The isolated oligonucleotides are characterized and quantified after each round of partition, and significant results were obtained. After the repetitive partition and amplification steps of target-specific oligonucleotides, final stage included sequencing of end product. We can confirm the specific sequence for anti-psychoactive drugs, which will be further used in diagnostic application in clinical and forensic set-up.

Keywords: anti-psychotic drugs, aptamer, biosensor, ssDNA, SELEX

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Authors: Mohamed El Moctar Abeidi

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The indazole derivatives exhibit a wide spectrum of biological activities. They are known for their anti-tumor, antiplatelet, anti-viral, anti-microbial, anti-inflammatory, anti-leishmania and even anti-spermatogen. As part of our research on the synthesis of a number of heterocycles capable of exhibiting a biological and pharmacological property, due to our ongoing interest in the development of a simple and low-cost procedure for obtaining heterocyclic compounds that may have an interest for medicinal purposes. We present in this work the synthesis of 6-nitro-indazoles derivatives, using two different methods. the first method is the alkylation of Nitroindazole by two different alkylating agents under the conditions of solid/liquid phase transfer catalysis in N, N-dimethylformamide (DMF) in the presence of potassium carbonate (K₂CO₃) as a base, and tetra-n-butylammonium bromide (BTBA) as a catalyst. While the other method is the 1,3-dipolar cycloaddition, in this case, we have undertaken the preparation of bi-heterocyclic containing the 6-nitroindazole associate with group of isoxazoline, isoxazole or 1,2,3-Triazole under normal conditions and, under the catalytic conditions of the click chemistry we were also able to determine the structures without any ambiguity by the ¹H and ¹³C NMR.

Keywords: indazole, 6-nitroindazole, isoxazole, 1, 2, 3-Triazole

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Authors: Elham Zarenezhad, Ali Zarenezhad, Mehdi Mardkhoshnood

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We described the synthesis and biological study of O-oxime ethers having a-amino acid residues as new analogs of IPS-339. In this synthesis, the reaction of fluorene O-oxime with epichlorohydrin or epibromohydrin afforded the corresponding O-oxime ether adducts. The N-alkylation of valine amino acid with O-oxime ether adducts led to the synthesis of new analogs of IPS-339. The cardiovascular properties of the compound have been studied. In this regard, six clinically healthy same sex mongrel dogs were examined. The dogs were randomly divided into 3 groups of two members. 1 groups received 2 mg kg-1 body weight of compound (2-(3-(9H-fluoren-9-ylideneaminooxy)-2- hydroxypropylamino)-3-methylbutanoic acid) intravenously, whereas group 2 and 3 received only DMSO–water (distil.) and propranolol (Inderal) (2 mg kg-1), respectively. The electrocardiograph (ECG) was recorded with lead II. The recording was run successively by 5 min time interval on each dog before, simultaneously, and after compound infusion. Data after administration were taken from normal sinus beats that were closely related to the arrhythmias whenever they occurred. In general, no detectable arrhythmia was observed in all ECG records regardless of increasing the heart rate that likely caused by stress origin from invasive procedure just after infusion. Compound diminished the heart rate during study especially at 20th minute compared to propranolol as a reference drug. Compound (2-(3-(9H-fluoren-9-ylideneaminooxy)-2- hydroxypropylamino)-3-methylbutanoic acid) was the most effective compound with remarkable ability in declining of the heart rate.

Keywords: electrocardiograph (ECG), cardiovascular, IPS-339, dogs

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Authors: Seyed Mahdi Rafiaei

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In this investigation, red emitting Eu³⁺ doped YVO₄ nano-phosphors have been synthesized via the facile combustion method using isobutyl nitrite and urea fuels, individually. Field-emission scanning electron microscope (FE-SEM) images, high resolution transmission electron microscope (TEM) images and X-ray diffraction (XRD) spectra reveal that the mentioned fuels can be used successfully to synthesis YVO₄: Eu³⁺ nano-particles. Interestingly, the fuels have a large effect on the size and morphology of nano-phosphors as well as luminescence properties. Noteworthy the use of isobutyl nitrite provides an average particle size of 65 nm, while the employment of urea, results in the formation of larger particles and also provides higher photoluminescence emission intensity. The improved luminescence performance is attributed to the condition of chemical reaction via the combustion synthesis and the size of synthesized phosphors.

Keywords: phosphors, combustion, fuels, luminescence, nanostructure

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Authors: Saeed Khodabakhshi, Alimorad Rashidi, Ziba Tavakoli, Sajad Kiani, Sadegh Dastkhoon

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Alumina nanoparticles (γ-Al2O3 NPs) were prepared via a new and simple synthetic route and characterized by field emission scanning electron microscope, X-ray diffraction, and Fourier transform infrared spectroscopy. The catalytic activity of prepared γ-Al2O3 NPs was investigated for the one-pot, four-component synthesis of fused tri-heterocyclic compounds containing pyrazole, pyran, and pyrimidine. This procedure has some advantages such as high efficiency, simplicity, high rate and environmental safety.

Keywords: alumina nanoparticles, one-pot, fused tri-heterocyclic compounds, pyran

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Authors: Juan Patricio Ibáñez, Exequiel López

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A method for synthesizing copper nanoparticles through an electrochemical approach is proposed, employing surfactants to stabilize the size of the newly formed nanoparticles. The electrolyte was made up of a matrix of H₂SO₄ (190 g/L) having Cu²⁺ (from 3.2 to 9.5 g/L), sodium dodecyl sulfate -SDS- (from 0.5 to 1.0 g/L) and Tween 80 (from 0 to 7.5 mL/L). Tween 80 was used in a molar relation of 1 to 1 with SDS. A glass cell was used, which was in a thermostatic water bath to keep the system temperature, and the electrodes were cathodic copper as an anode and stainless steel 316-L as a cathode. This process was influenced by the control exerted through the initial copper concentration in the electrolyte and the applied current density. Copper nanoparticles of electrolytic purity, exhibiting a spherical morphology of varying sizes with low dispersion, were successfully produced, contingent upon the chemical composition of the electrolyte and current density. The minimum size achieved was 3.0 nm ± 0.9 nm, with an average standard deviation of 2.2 nm throughout the entire process. The deposited copper mass ranged from 0.394 g to 1.848 g per hour (over an area of 25 cm²), accompanied by an average Faradaic efficiency of 30.8% and an average specific energy consumption of 4.4 kWh/kg. The chemical analysis of the product employed X-ray powder diffraction (XRD), while physical characteristics such as size and morphology were assessed using atomic force microscopy (AFM). It was identified that the initial concentration of copper and the current density are the variables defining the size and dispersion of the nanoparticles, as they serve as reactants in the cathodic half-reaction. The presence of surfactants stabilizes the nanoparticle size as their molecules adsorb onto the nanoparticle surface, forming a thick barrier that prevents mass transfer with the exterior and halts further growth.

Keywords: copper nanopowder, electrochemical synthesis, current density, surfactant stabilizer

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Authors: Ratthiwa Deewan, Visanu Tanboonchuy

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The optimal conditions for green synthesis of zero-valent (G-NZVI) synthesis are investigated in this study using a Box Behnken design. The factors that were used in the study consisted of 3 factors as follows: the iron solution to mango peel extract ratio (1:1-1:3), feeding rate of mango peel extracts (1-5 mL/min), and agitation speed (300-30 rpm). The results showed that the optimization of conditions using the regression model was appropriate. The optimal conditions of the synthesis of G-NZVI for arsenate removal are the iron solution to mango peel extract ratio of 1:1, the feeding rate of mango peel extract at 5 mL/min, and the agitation speed rate of 300 rpm, which was able to arsenate removal of 100%.

Keywords: Box Behnken design, arsenate removal, green nano zero valent iron, arsenic

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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: Messai Amel, Badis Zakaria, Benali-Cherif Nourredine, Dominique Luneaub

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We are interested in molecular polymetallic species having high spin and nuclearities in relation to the field of so call single-molecule magnets (SMMs). The goal is to find a way to synthesis metal clusters which may have application in magnetism and nano sciences. With this purpose, we decided to investigate the coordination chemistry of the Schiff base. Along this way we were able to create cubane-like complexes and elaborate new Single Molecule-Magnets. The idea was to use Schiff base ligands and different metals to generate high nuclear complexes. Complexation of Shiff base with copper (II) has been investigated. Tetra nuclear complex with a cubane like core have been synthesized with (Sciff base), with the same base and cobalt (II) we obtain an other single magnetic complex completely different. In this presentation, we report the synthesis, crystal structure and magnetic properties of the tetranuclear compound (Cu4 L4), and the tetranuclear compound. (Co4L4)

Keywords: cluster-assembled materials, magnetic compounds, Sciff base, cupper, cobalt

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Authors: Erico R. Carmona, Lucas Hernandez-Saravia, Aliro Villacorta, Felipe Carevic

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Tailings and electronic waste (e-waste) are an important source of global contamination. Chile is one of Organisation for Economic Co-operation and Development (OECD) member countries that least recycled this kind of industrial waste, reaching only 3% of the total. Tailings and e-waste recycling offers a valuable tool to minimize the increasing accumulation of waste, supplement the scarcity of some raw materials and to obtain economic benefits through the commercialization of these. It should be noted that this type of industrial waste is an important source of valuable metals, such as copper, which allow generating new business and added value through its transformation into new materials with advanced physical and biological properties. In this sense, the development of nanotechnology has led to the creation of nanomaterials with multiple applications given their unique physicochemical properties. Among others, copper nanoparticles (CuNPs) have gained great interest due to their optical, catalytic, conductive properties, and particularly because of their broad-spectrum antimicrobial activity. There are different synthesis methods of copper nanoparticles; however, green synthesis is one of the most promising methodologies, since it is simple, low-cost, ecological, and generates stable nanoparticles, which makes it a promising methodology for scaling up. Currently, there are few initiatives that involve the development of methods for the recovery and transformation of copper from waste to produce nanoparticles with new properties and better technological benefits. Thus, the objective of this work is to show preliminary data about the develop a sustainable transformation process of tailings and e-waste that allows obtaining a copper-based nanotechnological product with potential antimicrobial applications. For this, samples of tailings and e-waste collected from Tarapacá and Antofagasta region of northern Chile were used to recover copper through efficient, ecological, and low-cost alkaline hydrometallurgical treatments, which to allow obtaining copper with a high degree of purity. On the other hand, the transformation process from recycled copper to a nanomaterial was carried out through a green synthesis approach by using vegetal organic residue extracts that allows obtaining CuNPs following methodologies previously reported by authors. Initial physical characterization with UV-Vis, FTIR, AFM, and TEM methodologies will be reported for CuNPs synthesized.

Keywords: nanomaterials, industrial waste, chile, recycling

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Authors: Otilia R. Vasile, Florina C. Ilie, Irina F. Nicoara, Cristina D. Ghitulica, Roxana Trusca, Ovidiu Oprea, Vasile A. Surdu, Bogdan S. Vasile, Ecaterina Adronescu

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In this work ZnO nanostructures (nanopowders and nanostars) have been synthesized via a simple sol-gel method. The used methods for synthesizing the nanostructures involve two steps as follows: (1) precipitation of zinc acetate precursor for the synthesis of ZnO nanopowders and zinc chloride precursor for the synthesis of ZnO nanostars and (2) addition of Eu2O3 in different concentrations (1%, 3%, and 5%) using europium acetate as precursor. Detailed crystalline parameters for each of the synthetized species were analysed using X-ray diffraction. Structural transitions were also discussed. The structure and morphology of the as-prepared ZnO nanopowders and nanostars were investigated by electron microscopy. TEM investigations have shown an average particle size range from 23 to 29 nm and polyhedral and spherical morphology with tendency to form aggregates for nanopowders. For nanostars structures, a star-like morphology could be observed. Cytotoxicity tests on MG-63 cell lines were also performed. Photocatalytic activity of ZnO nanopowders have reached higher values compared to ZnO nanostars.

Keywords: cytotoxicity, photocatalytic activity, TEM, ZnO

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Authors: Mahsa Kangazian Kangazi, Ali Akbar Ghareh Aghaji, Majid Montazer

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Nowadays, silica nanofibers are highly regarded among the inorganic nanofibers due to the high reactivity and availability of silicon compounds in nature. Sol-gel process is required for electrospinning of silica nanofibers in which a metal alkoxide is hydrolyzed, and the viscosity is increased. In this study, silica nanofibers containing silver nanoparticles were synthesized and electrospun from a mixture of silica sol with an easy spinnable polymer (PVA) as an additive. The silica sol contains tetraethyl orthosilicate (TEOS), silver nitrate, distilled water, nitric acid, and ethanol. Nanofibers were formed through electrospinning setup. The nanofibers were calcinated to remove the solvent and additive polymer. Consequently, pure silica nanofibers were produced. FTIR analysis indicated entire removal of polyvinyl alcohol from the structure and formation of silan groups. The presence of silver, silica and oxygen was confirmed by EDX. Also, XRD patterns revealed the presence of silver nanoparticles with a mean crystal size of 18 nm. FESEM images showed that adding silver nitrate into the sol-gel, resulted in lower nanofibers diameter from 286 to 136 nm. Furthermore, the electrospun nanofibers were more resistance in acidic media than alkaline media.

Keywords: in situ synthesis of silver nanoparticles, silica nanofibers, sol-gel, tetraethyl orthosilicate

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Authors: Mahmoud H. Aboul-Ela, Riham R. Mohamed, Magdy W. Sabaa

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Synthesis of cross-linked hydrogels composed of trimethyl chitosan (TMC) and poly(vinyl alcohol) (PVA) in different weight ratios in presence of glutaraldehyde as cross-linking agent. Characterization of the prepared hydrogels was done using FTIR, XRD, SEM and TGA. The prepared hydrogels were investigated as adsorbent materials for some transition metal ions from their aqueous solutions. Moreover, the swell ability of the prepared hydrogels was also investigated in both acidic and alkaline pHs, as well as in simulated body fluid (SBF).

Keywords: trimethyl chitosan, hydrogels, metal uptake, superabsorbent materials

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Authors: Kai-Sheng Ji, Yi-Feng Lin

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The pervaporation process for solvent and water separation has attracted research attention due to its lower energy consumption compared with conventional distillation processes. The membranes used for the pervaporation approach should exhibit high flux and separation factors. In this study, the ZIF-7 crystal particles were successfully incorporated into chitosan (CS) membranes to form ZIF-7/CS mixed-matrix membranes. The as-prepared ZIF-7/CS mixed-matrix membranes were used to separate mixtures of water/ethanol at 25℃ in the pervaporation process. The mixed-matrix membranes with different ZIF-7 wt% incorporation showed better separation efficiency than the pristine CS membranes because of the smaller pore size of the mixed-matrix membranes. The separation factor and the flux of the ZIF-7/CS membranes clearly exceed the upper limit of the previously reported CS-based and mixed-matrix membranes.

Keywords: pervaporation, chitosan, ZIF-7, memberane separation

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Authors: Yousef Bakhbakhi

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Crystallization with supercritical fluids (SCFs), as a developed technology to produce particles of micron and sub-micron size with narrow size distribution, has found appreciable importance as an environmentally friendly technology. Particle synthesis using SCFs can be achieved employing a number of special processes involving solvent and antisolvent mechanisms. In this study, the compressed antisolvent (PCA) process is utilized as a model to analyze the theoretical complexity of crystallization with supercritical fluids. The population balance approach has proven to be an effectual technique to simulate and predict the particle size and size distribution. The nucleation and growth mechanisms of the particles formation in the PCA process is investigated using the population balance equation, which describes the evolution of the particle through coalescence and breakup levels with time. The employed mathematical population balance model contains a set of the partial differential equation with algebraic constraints, which demands a rigorous numerical approach. The combined Collocation and Galerkin finite element method are proposed as a high-resolution technique to solve the dynamics of the PCA process.

Keywords: particle formation, particle size and size distribution, PCA, supercritical carbon dioxide

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Authors: Farzaneh Ziaee, Mohammad Ziaee

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N-acetyl-L-cysteine (NAC) is a well-known mucolytic agent, and recently its efficacy has been examined for the prevention and remediation of several diseases such as lung infections caused by Coronavirus. Also, it is administrated as the main antidote in paracetamol overdose and is effective for the treatment of idiopathic pulmonary fibrosis (IPF), chronic obstructive pulmonary disease (COPD). This medicine is used as an antioxidant to prevent diabetic kidney disease (nephropathy). In this study, a method for the acylation of amino acids is employed to manufacture this drug in a height yield. Regarding this patented path, NAC can be made in a single batch step at ambient pressure and temperature. Moreover, this study offers a technique to make peptide bonds which is of interest for pharmaceutical and medicinal industries. The separation process was undertaken using appropriate solvents to achieve an excellent purification level. The synthesized drug was characterized via proton nuclear magnetic resonance (1H NMR), high-performance liquid chromatography (HPLC), Fourier transform infrared spectroscopy (FT-IR), elemental analysis, and melting point.

Keywords: N-acetylcysteine, synthesis, mucolytic medication, lung anti-inflammatory, COVID-19, antioxidant, pharmaceutical supplement, characterization

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Authors: B. M. Vishal, Monamie Basu, Gopinath M., Rose Havilah Pulla

Abstract:

Though there are several methods of synthesizing silver nano particles, Green synthesis always has its own dignity. Ranging from the cost-effectiveness to the ease of synthesis, the process is simplified in the best possible way and is one of the most explored topics. This study of extracting secondary metabolites from Perilla frutescens and using them for therapeutic additives has its own significance. Unlike the other researches that have been done so far, this study aims to synthesize Silver nano particles from Perilla frutescens using three available forms of the plant: leaves, seed, and commercial leaf extract powder. Perilla frutescens, commonly known as 'Beefsteak Plant', is a perennial plant and belongs to the mint family. The plant has two varieties classed within itself. They are frutescens crispa and frutescens frutescens. The species, frutescens crispa (commonly known as 'Shisho' in Japanese), is generally used for edible purposes. Its leaves occur in two forms, varying on the colors. It is found in two different colors of red with purple streaks and green with crinkly pattern on it. This species is aromatic due to the presence of two major compounds: polyphenols and perillaldehyde. The red (purple streak) variety of this plant is due to the presence of a pigment, Perilla anthocyanin. The species, frutescens frutescens (commonly known as 'Egoma' in Japanese), is the main source for perilla oil. This species is also aromatic, but in this case, the major compound which gives the aroma is Perilla ketone or egoma ketone. Shisho grows short as compared with Wild Sesame and both produce seeds. The seeds of Wild Sesame are large and soft whereas that of Shisho is small and hard. The seeds have a large proportion of lipids, ranging about 38-45 percent. Excluding those, the seeds have a large quantity of Omega-3 fatty acids, linoleic acid, and an Omega-6 fatty acid. Other than these, Perilla leaf extract has gold and silver nano particles in it. The yield comparison in all the cases have been done, and the process’ optimal conditions were modified, keeping in mind the efficiencies. The characterization of secondary metabolites includes GC-MS and FTIR which can be used to identify the components of purpose that actually helps in synthesizing silver nano particles. The analysis of silver was done through a series of characterization tests that include XRD, UV-Vis, EDAX, and SEM. After the synthesis, for being used as therapeutic additives, the toxin analysis was done, and the results were tabulated. The synthesis of silver nano particles was done in a series of multiple cycles of extraction from leaves, seeds and commercially purchased leaf extract. The yield and efficiency comparison were done to bring out the best and the cheapest possible way of synthesizing silver nano particles using Perilla frutescens. The synthesized nano particles can be used in therapeutic drugs, which has a wide range of application from burn treatment to cancer treatment. This will, in turn, replace the traditional processes of synthesizing nano particles, as this method will prove effective in terms of cost and the environmental implications.

Keywords: nanoparticles, green synthesis, Perilla frutescens, characterisation, toxin analysis

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Authors: G. N. Maheshika, J. A. R. H. Wijerathna, S. H. P. Gunawardena

Abstract:

Feedstock with high free fatty acids (FFAs) content can be successfully employed for biodiesel synthesis once the high FFA content is reduced to the desired levels. In the present study, the applicability of ferric sulphate as the solid acid catalyst for esterification of FFA in used coconut oil was evaluated at varying catalyst concentration and methanol:oil molar ratios. 1.25, 2.5, 3.75 and 5.0% w/w Fe2(SO4)3 on oil basis was used at methanol:oil ratios of 3:1, 4.5:1, and 6:1 and at the reaction temperature of 60 0C. The FFA reduction increased with the increase in catalyst and methanol:oil molar ratios while the time requirement to reach the esterification equilibrium reduced. Satisfactory results for esterification could be obtained within a small reaction period in the presence of only a small amount of Fe2(SO4)3 catalyst concentration and at low reaction temperature, which then can be subjected for trans-esterification process. At the end of the considering reaction period the solid Fe2(SO4)3 catalyst could be separated from the reaction system. The economics of the Fe2(SO4)3 catalyzed esterification of high FFA content used coconut oil for biodiesel is at favorable conditions.

Keywords: biodiesel, esterification, ferric sulphate, Free fatty acids, used coconut oil

Procedia PDF Downloads 548

Authors: D. Wattanasiriwech, S. Wattanasiriwech

Abstract:

In this paper, attempt to synthesize designed cordierite-mullite system with various ratios was performed using a solid-state method. Alumina, quartz, magnesia, and talc were used as starting materials for the synthesis. Talc was added for two purposes; to assist the reaction progress and to be the Mg source. The raw materials were mixed and fired at 1350°C for 2 h and 1400°C for 2 and 4 h. The resulting phase compositions were analysed using the Reference Intensity Ratio (RIR) semi-quantitative analysis method. The highest amount of cordierite up to Cordierite phase 96% could be obtained at the firing scheme of 1400°C for 4 h in the C100-M0. Mullite could not be formed at the selected scheme if talc did not present so no pure mullite was observed in the selected firing regime. The highest amount of mullite co-existed with cordierite and other phases were 74%.

Keywords: RIR semi-quantitative analysis, cordierite-mullite system, solid state synthesis, X-Ray diffraction

Procedia PDF Downloads 168

Authors: Prasanta Sutradhar, Mitali Saha

Abstract:

With an increasing awareness of green and clean energy, zinc oxide based solar cells were found to be suitable candidates for cost-effective and environmentally friendly energy conversion devices. In this work, we have reported the green synthesis of zinc oxide nanoparticles (ZnO) by thermal method and under microwave irradiation using the aqueous extract of tomatoes as non-toxic and ecofriendly reducing material. The synthesized ZnO nanoparticles were characterised by UV-Visible spectroscopy (UV-Vis), infra-red spectroscopy (IR), particle size analyser (DLS), scanning electron microscopy (SEM), atomic force microscopy (AFM), and X- ray diffraction study (XRD). A series of ZnO nanocomposites with titanium dioxide nanoparticles (TiO2) and graphene oxide (GO) were prepared for photovoltaic application. Structural and morphological studies of these nanocomposites were carried out using UV-vis, SEM, XRD, and AFM. The current-voltage measurements of the nanocomposites demonstrated enhanced power conversion efficiency of 6.18% in case of ZnO/GO/TiO2 nanocomposite.

Keywords: ZnO, green synthesis, microwave, nanocomposites, I-V characteristics

Procedia PDF Downloads 402

Authors: Shalini Rajput, Dinesh Mohan

Abstract:

Water is the most important and essential resources for existing of life on the earth. Water quality is gradually decreasing due to increasing urbanization and industrialization and various other developmental activities. It can pose a threat to the environment and public health therefore it is necessary to remove hazardous contaminants from wastewater prior to its discharge to the environment. Recently, magnetic iron oxide nanoparticles have been arise as significant materials due to its distinct properties. This article focuses on the synthesis method with a possible mechanism, structure and application of magnetic iron oxide nanoparticles. The various characterization techniques including X-ray diffraction, transmission electron microscopy, scanning electron microscopy with energy dispersive X-ray, Fourier transform infrared spectroscopy and vibrating sample magnetometer are useful to describe the physico-chemical properties of nanoparticles. Nanosized iron oxide particles utilized for remediation of contaminants from aqueous medium through adsorption process. Due to magnetic properties, nanoparticles can be easily separate from aqueous media. Considering the importance and emerging trend of nanotechnology, iron oxide nanoparticles as nano-adsorbent can be of great importance in the field of wastewater treatment.

Keywords: nanoparticles, adsorption, iron oxide, nanotechnology

Procedia PDF Downloads 556

Authors: Rungsinee Sothornvit, Pattrathip Rodsamran

Abstract:

Rice stubble consists of a high content of cellulose and can be synthesized as a cellulose derivative such as carboxymethyl cellulose (CMC) to value added products from agricultural waste. Therefore, the synthesis conditions and characterization the properties of CMC from rice stubble (CMCr) were investigated. Hemicellulose and lignin were first removed from the rice stubble using 10% NaOH at 55 C for 3 h and 5% NaOCl at 75 C for 15 min, respectively. Rice stubble cellulose was swollen in 30% NaOH and isopropanol as a solvent. The content of chloroacetic acid (5–7 g in 5 g of alkali cellulose), reaction temperature (50 and 70 C) and time (180, 270 and 360 min) were explored to obtain CMC. It was found that synthesis conditions did not affect significantly on moisture content and pH of CMCr. The best quality of CMCr was synthesized by using 7 g of chloroacetic acid and reacted at 50 C for 180 min based on 5 g of rice stubble cellulose. Degree of substitution (DS), viscosity and purity of CMCr were 0.64, 36.03 cP and 90.18 %, respectively. Furthermore, Fourier transform infrared (FT–IR) spectroscopy confirmed the presence of carboxymethyl substituents. CMCr was categorized in commercial scale as a low viscosity material and it can be used as film forming packaging materials for food and pharmaceutical product applications.

Keywords: rice stubble, cellulose, carboxymethyl cellulose, degree of substitution, purity

Procedia PDF Downloads 393