Simultaneous control of rod length and pore diameter of SBA-15 for PPL loading

Mesoporous silica materials are attractive materials for immobilizing enzymes because of their well-ordered structures, large surface area are pore volume. Diffusion of large enzyme molecules such as porcine pancreatic lipase (PPL) through the lengthy channels of MPS takes place too slowly. Therefore, the squat of the enzyme at the pore mouth entrance, actually makes the rest of the channel useless. In this study, to overcome this problem, synthesis parameters of SBA-15 were changed, since along with pore diameter increasing, the mesochannel length becomes shorter. The main point to obtain a well-ordered 2D hexagonal pore structure was the pre-hydrolysis of tetraethyl orthosilicate (TEOS) before the addition of 1,3,5-trimethyl benzene as a micelle swelling agent. Due to the strong effect of zirconium in changing the morphology of SBA-15 particles, we modified SBA-15 in the presence of a small amount of ZrOCl₂ in the synthesis solution under acidic conditions. As a result, mesochannel length of SBA-15-Zr was shortened from 600 to <200 nm. The morphology of mesoporous silica was also changed from rod-like to platelet, because of the accelerating effect of Zr(IV) on the self-assembly rate of P123 and TEOS condensation. Characteristic results conducted by low angle XRD, high resolution transmission electron microscopy and nitrogen adsorption, confirmed tuning effect of Zr(IV) in SBA-15. Furthermore, it was shown that the number of pore entrances increases with decreasing the length of SBA-15 mesochannels, leading to obvious improvement of enzyme uptake. PPL has been successfully immobilized in the mesoporous channels of SBA-15-Zr. The total amount of lipase adsorbed on the mesoporous SBA-15-Zr was measured by thermal gravimetric analysis. The largest PPL adsorption capacity was 784 mg/g belonging to the SBA-15-Zr with the length of 150 nm and the mean pore size diameter of 9.22 nm.     

Nonisothermal suspension polymerization of vinyl chloride for enhanced productivity

In the present study, a mathematical model is developed to numerically predict nonisothermal batch suspension polymerization of vinyl chloride. Free volume theory was used to consider diffusion‐controlled reactions. Model predictions were validated against field data obtained in a pilot scale stirred tank reactor. Variable temperature trajectory was considered during the course of the reaction to improve productivity by reducing the polymerization time for a certain conversion. Variable temperature during the course of the polymerization was successfully implemented by considering the predefined K value. By using variable temperatures during the course of the reaction, the density of the short branches per 1,000 monomer units as a criterion for structure defect remained relatively unchanged. Maximum reduction in reaction time relative to the isothermal case with the same K value and final conversion was 44% for the best temperature trajectory. J. VINYL ADDIT. TECHNOL., 22:470–478, 2016. © 2015 Society of Plastics Engineers     

Optimization of a Three-Component Green Corrosion Inhibitor Mixture for Using in Cooling Water by Experimental Design

Factors such as inhibitor concentration, solution hydrodynamics, and temperature influence the performance of corrosion inhibitor mixtures. The simultaneous studying of the impact of different factors is a time- and cost-consuming process. The use of experimental design methods can be useful in minimizing the number of experiments and finding local optimized conditions for factors under the investigation. In the present work, the inhibition performance of a three-component inhibitor mixture against corrosion of St37 steel rotating disk electrode, RDE, was studied. The mixture was composed of citric acid, lanthanum(III) nitrate, and tetrabutylammonium perchlorate. In order to decrease the number of experiments, the L16 Taguchi orthogonal array was used. The “control factors” were the concentration of each component and the rotation rate of RDE and the “response factor” was the inhibition efficiency. The scanning electron microscopy and energy dispersive x-ray spectroscopy techniques verified the formation of islands of adsorbed citrate complexes with lanthanum ions and insoluble lanthanum(III) hydroxide. From the Taguchi analysis results the mixture of 0.50 mM lanthanum(III) nitrate, 0.50 mM citric acid, and 2.0 mM tetrabutylammonium perchlorate under the electrode rotation rate of 1000 rpm was found as optimum conditions.     

Tartaric Acid as a Non-toxic and Environmentally-Friendly Anti-scaling Material for Using in Cooling Water Systems: Electrochemical and Surface Studies

Because of the major limitations in drinking water resources, the industries need to use unprocessed water sources for their cooling systems; these water resources contain major amount of hardening cations. So, mineral scales are formed in cooling water systems during the time and cause major problems. The use of green anti-scaling materials such as carboxylic acids is considered due to their low risks of environmental pollution. In the present work, the scale inhibition performance of tartaric acid as a green organic material was evaluated. Chemical screening tests, cathodic and anodic voltammetry measurements and electrochemical impedance spectroscopy (EIS), field emission scanning electron microscopy (FESEM), energy-dispersive x-ray and x-ray diffraction, were used for the evaluation of the scale inhibition performance. The results showed that tartaric acid can prevent calcium carbonate precipitation significantly. The hard water solution with 2.0 mM of tartaric acid indicated the highest scale inhibition efficiency (ca. 68%). The voltammetry, EIS and FESEM results verified that tartaric acid can form smooth and homogeneous film on steel surface through formation of Fe(III)-tartrate complexes and retard the local precipitation of calcium carbonate deposits.     

Corrosion and time dependent passivation of Al 5052 in the presence of H<Subscript>2</Subscript>O<Subscript>2</Subscript>

Corrosion and time–dependent oxide film growth on AA5052 Aluminum alloy in 0.25M Na₂SO₄ solution containing H₂O₂ was studied using electrochemical impedance spectroscopy, potentiodynamic polarization, chronoamperometric and open circuit potential monitoring. It was found that sequential addition of H₂O₂ provokes passivation of AA5052 which ultimately thickens the oxide film and brings slower corrosion rates for AA5052. H2O2 facilitates kinetics of oxide film growth on AA 5052 at 25° and 60 °C which is indicative of formation of a thick barrier film that leads to an increment in the charge transfer resistance. Pitting incubation time increases by introduction of H₂O₂ accompanied by lower pitting and smoother surface morphologies. At short exposure (up to 8 h) to H₂O₂–containing solution, the inductive response at low frequencies predominantly determined the corrosion mechanism of AA5052. On the other hand, at prolonged exposure times (more than 24 h) to 0.25M Na₂SO₄+1vol% H₂O₂ solution, thicker oxide layers resulted in the mixed inductive–Warburg elements in the spectra.     

CuI Immobilized on Tricationic Ionic Liquid Anchored on Functionalized Magnetic Hydrotalcite (Fe3O4/HT-TIL-CuI) as a Novel,Magnetic and Efficient Nanocatalyst for Ullmann-Type C–N Coupling Reaction

One of the most important reactions in organic synthesis is Ullmann-type C–N coupling reaction which has been used for preparation of numerous biologically active compounds. In this work, CuI immobilized on tricationic ionic liquid anchored on functionalized magnetic hydrotalcite (Fe₃O₄/HT-TIL-CuI) has been successfully prepared and fully characterized by different techniques, including fourier-transform infrared spectroscopy, vibrating sample magnetometer, thermo gravimetric analysis, transmission electron microscopy, field-emission scanning electron microscopy, energy dispersive X-ray spectroscopy, elemental mapping, zeta potential, X-ray diffraction, temperature programmed desorption of ammonia (NH₃-TPD), temperature-programmed reduction and inductively coupled plasma. The results showed that the as-prepared nanocatalyst possesses plate-like morphology with approximate size of 50 nm and superparamagnetic behavior. Also, total acidity and total hydrogen consumption of the nanocatalyst were measured to be 8.5 and 1.41 mmol g^?1, respectively. This nanocatalyst exhibited favorable performance for C–N coupling reaction among a variety of aryl halides and N(H)-heterocycles (benzimidazoles, pyrazoles and triazoles) in the presence of 2.5 mol% of nanocatalyst without any additives under air atmosphere revealing high yields in all cases. Besides, it is noted that in the present system the desired product can be easily and quickly isolated and nanocatalyst also recovered magnetically from the reaction mixture employing a permanent magnet for at least six consecutive trials without a discernible decrease in catalytic activity which makes the proposed methodology appropriate for industrial. The findings demonstrated the advantages of the present method as no need for neutral atmosphere, appropriate times, recyclability of the catalyst, broad substrate scope, minimization of chemical waste, simple purification of products, easy workup process, and high yields.

     

The effect of substrate surface integrity on the surface properties of TiCrN coating applied via the CAE-PVD method

This study aims to investigate how the predeposition machining processes such as magnetic grinding, turning machining, and wire electrical discharge machining can influence the surface properties including electrochemical and tribological behavior of TiCrN nanostructured coating applied on Mo40 steel substrate. A physical vapor deposition technique using cathodic arc evaporation was used to apply the coating. The crystallographic phases and the microstructure of the coating were studied by X-ray diffraction and scanning electron microscope, respectively. Rockwell-C, electrochemical impedance spectroscopy and potentiodynamic polarization, and pin-on-disk wear tests were employed to evaluate the adhesion strength, corrosion behavior, and tribological property of specimens, respectively. The electrochemical results after 24 h of exposure to 3.5 wt% NaCl solution showed that TiCrN coating pretreated with a turning process with polarization resistance of about 3525.32 Ω.cm² had the best corrosion resistance among all specimens. This was because of the improvement of the smoothness, surface quality, and adhesion after the turning process. On the other, the friction coefficient of the grounded sample is less than that of other ones. This is probably due to its higher adhesion strength and higher surface smoothness.     

Fault diagnosis of an automobile cylinder head using low frequency vibrational data

This paper proposes a vibration-based fault-diagnosis method for mechanical parts. This method, after algorithm development, only requires a single inexpensive test to inspect the part which could take as short as half a second. The algorithm is developed in three major stages, (i) exciting specimens without or with known faults using a controlled force and recording acceleration of a single point for a short time (ii) finding a signature for each faulty specimen, using Fourier transform and statistical analysis. (iii) Developing a multi-layer perceptron, as a mathematical model, using the results of stage (ii). The elements of a part signature are the inputs to the model. The location (and possibly size and shape factor) of the fault is model output. Stage (i) can be performed experimentally or alternatively with a validated FEM, one experiment or simulation per specimen. The proposed technique was examined to locate (isolate) a fault on an automobile cylinder head. The presented accuracy is considerable, and the data collected at fairly low frequency range (below 1200 Hz) were found to be sufficient for this technique. In the case study of this paper, possible fault locations are on a line; as a result, fault location has one dimension. It is shown that the technique can be extended to higher dimensions.     

Flammability and thermal properties of epoxy/glass/MWNT Composites

The aim f this work is to study the effect of nanotubes on flammability properties of epoxy/glass composites. Multiwalled carbon nanotubes (MWNT) and its functionalized derivative (amino functionalized nanotubes) were incorporated into epoxy resin. To disperse MWNTs in the epoxy resin, different ways were employed. Microscopic observations showed that, the best dispersion state was gained by using ultrasonication method and high shear flow simultaneously. Thermal resistance of cured epoxy resins containing various amounts of nanotubes (0.25–0.7 wt %), was investigated by thermo gravimetric analysis (TGA). Introducing MWNTs and amino‐MWNTs to samples increased the initial thermal decomposition temperature for about 32 and 37°C, respectively. LOI measurements of composite samples showed an increase up to 32. Cone calorimetry test was carried out on epoxy/glass and epoxy/glass containing 0.5% MWNT. The results showed that, introducing 0.5% MWNTs decreases maximum average rate of heat emission for about 26%. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 39849.     

Protective properties of PPy‐Au nanocomposite coatings prepared by sonoelectrochemisty and optimized by the Taguchi method

The polypyrrole (PPy) and polypyrrole‐Au (PPy‐Au) nanocomposite films have been sonoelectrochemically synthesized on St‐12 steel electrodes using the galvanostatic technique. Experimental design according to the Taguchi method has been applied to optimize the factors on the synthesis of PPy‐Au nanocomposite coating. Three factors were used to design an orthogonal array L9: Synthesis time (t), Current density (I), and Concentration of HAuCl₄ (C). The synthesized Au nanoparticles during polymerization were characterized by Ultraviolet–visible (UV‐visible) spectroscopy. Characterization of the surfaces was done by scanning electron microscope (SEM), energy dispersive X‐ray spectrum (EDX), and atomic force microscope (AFM). The scanning electron microscopy (SEM) image of PPy shows a smooth surface while PPy‐Au nanocomposite film has a compact morphology. Moreover, energy dispersive X‐ray spectrum (EDX) is evidence for the incorporation of Au nanoparticles. The corrosion protection of coatings was investigated by open circuit potential (OCP) time trends, potentiodynamic polarization technique, and electrochemical impedance spectroscopy (EIS) in a NaCl 3.5% solution. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 41087.