Taguchi Optimization of Solvent-Antisolvent Crystallization to Prepare Ammonium Perchlorate Particles

The sphericity and size of ammonium perchlorate (AP) particles significantly influence the properties of composite propellants. As the AP particles become more spherical, the accumulation coefficient increases, the viscosity during casting decreases, and the particle loading and burning rate increase. Hence, the production of micronized AP particles with an average size between 1 and 20 μm is important to increase the loading percentage of AP in the composite propellant. Here, the Taguchi experimental design was used to optimize the solvent-antisolvent crystallization (SAC) process for the preparation of micronized AP particles with higher sphericity. SAC parameters such as the type of antisolvent, the solvent-to-antisolvent ratio, the antisolvent temperature, the stirring speed, and the retention time were investigated at four levels. The type of antisolvent and the solvent-to-antisolvent ratio were found to mainly contribute to improving the sphericity and size of the AP particles, respectively.     

Developing electrochemical measurements in order to assess anti-corrosive coatings more effectively

The aim of this project was to check reproducibility of results obtained using NOCS (no connection to the substrate) arrangement of the electrochemical noise method (ENM). NOCS involves taking measurements from three nominally identical areas on the coated surface. Thus, no electrical connection to substrate is required. In practice the areas are not identical and various arrangements for connection of the three cells were tried to see if the individual areas could be separated out and whether the individual resistances could be computed. Also different ways of calculating the R_n (noise resistance) and R_sn (spectral noise resistance) parameters were attempted to see which one gave the best comparison with the more standard EIS measurements. The maximum entropy method was recognized to be the most useful for comparison with EIS, as well as for graphic evaluation of results. Regarding distinguishing three areas using different connection arrangements, it was possible to identify the situation when one of the three values was different to the other two. However further experiments are needed before it will be possible to confidently assign an R_n value to each individual area.     

Properties of PET/clay nanocomposite films

Polyethylene terephthalate (PET) nanocomposite films were prepared by cast extrusion followed by uniaxial stretching, using chill rolls. Transmission electron microscopy (TEM) and wide angle X‐ray diffraction (WAXD) showed that the clay layers were aligned in the machine direction (MD) in the PET/clay nanocomposite (PCN) films. Differential scanning calorimetry (DSC) showed that PCN films have higher crystallinity than the neat PET films, possibly due to the nucleating role of the silicate layers. The PCN films became hazier as the clay content increased, but the film transparency remained in the acceptable range. Oxygen permeability of the PCN films decreased by 23% compared to the neat PET film. This is comparable with predictions of models proposed in the literature. Silicate incorporation brought about 20% increase in the tensile modulus, while the puncture and tear propagation resistance were reduced, due to brittleness of the PCN films. The measured modulus (1.7 GPa) was somewhat smaller than the values predicted using the Pseudoinclusion model (2.1 GPa). POLYM. ENG. SCI., 2012. © 2011 Society of Plastics Engineers     

Synthesis of water dispersible reduced graphene oxide via supramolecular complexation with modified β-cyclodextrin

A noncovalent functionalization of the edges of reduced graphene oxide (RGO) with β-cyclodextrin-graft-hyperbranched polyglycerol (β-CD-g-HPG) was successfully performed via a host-guest interaction. The results showed that β-CD-g-HPG disperses the graphene sheets better than pure β-CD or HPG. The resulted supramolecular structure is stable in neutral water medium more than one week. However, in acidic medium the host-guest interaction is collapsed and graphene nanosheets precipitate.     

Sonochemical Synthesis of a Nanocrystalline Tin(IV) Complex based on a Bulky Anthracene Carboxylate Ligand: Spectroscopic and Photophysical Properties

In order systematically investigate the effect of ligand with a large conjugated π-system on the structure and optical properties of tin complex, anthracene-9-carboxylic acid (L¹) is selected as a primary ligand, and quinoline-2-carboxylic acid (L²) used as second ligand to incorporate with anthracene-9-carboxylic acid to construct a new tin(IV)-carboxylate coordination complex under thermal gradient condition. Prepared complex was fully characterized based on its ¹H and ¹³C NMR, IR and UV spectra and elemental analysis. The molecular structure of complex was determined by single-crystal X-ray analysis. The nanocrystalline complexes of the prepared complex were successfully obtained at 30, 50 and 60 °C by a facile sonochemical route. The new nanocrystalline complexes were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analysis. The photoluminescence properties of the nanocrystalline complexes and crystalline bulk complex in the solid-state indicated that the size of the complex particles has a remarkable effect on the optical properties of it. Absorption and emission peaks of the nanocrystalline complexes blue shifted significantly in comparison with those of in the single-crystal form. Application of the prepared complex in fabrication of an organic light-emitting diode has been demonstrated. The current–voltage (I–V) characteristics and the electroluminescence (EL) properties of the complex have been investigated. The EL of the compound exhibits green emission at 552 nm.     

Mass Transfer in Molybdenum Extraction from Aqueous Solutions Using Nanoporous Membranes

Modeling of non‐disperse solvent extraction of molybdenum(VI) with PC‐88A as extractant and a nanoporous hollow‐fiber membrane contactor as extractor was performed. Computational fluid dynamics was applied for modeling and simulation of molybdenum extraction. Concentration, pressure, and velocity distributions for molybdenum were determined. The extraction of Mo⁶⁺ was greatly influenced by the flow rate of feed solution. The extraction efficiency was reduced with higher feed flow rate and increased with the molybdenum content in the feed. The pressure drop along the shell side of the membrane extractor was found to be not significant, being one of the advantages of membrane extractors which assist in reducing the operational costs. The proposed simulation method is capable to prognosticate the performance of solvent extraction of molybdenum in membrane extractors.     

Polybutadiene/polyhedral oligomeric silsesquioxane nanohybrid: investigation of various reactants in polyesterification reaction

Nano‐sized polyhedral oligomeric silsesquioxane (POSS) diol or ethylene glycol (EG) as diol monomer was incorporated into hydroxyl‐terminated polybutadiene (HTPBD) chain in the presence of fumaryl or thionyl chloride as extenders. Using these polyesterification reactions, two fumarate‐based polyesters and two polyester sulfites were synthesized. Each couple of polyesters and polyester sulfites includes a linear (diol:EG) and a nanohybrid macromer (diol:POSS). Full structural characterization was performed using Fourier transform infrared, ¹H NMR and ¹³C NMR spectroscopies. Gel permeation chromatography was undertaken to study polyesterification mechanisms by deconvolution of the obtained traces. Finally, differential scanning calorimetry, thermogravimetric analysis and cell culture were performed to evaluate the structure–property relationship for the synthesized macromers in comparison with unreacted HTPBD. © 2016 Society of Chemical Industry     

Effect of pulsed ultrasound treatment compared to continuous mode on microbiological and quality of Mirabelle plum during postharvest storage

The effects of pulsed and continuous ultrasound treatment on microbiological and physiological quality of Mirabelle plum fruit were investigated. Freshly harvested Mirabelle plum was treated with 30‐kHz pulsed and continuous ultrasound at 20 °C for 0, 15, 30, 45 and 60 min and subsequently stored at 4 °C for 10 days. The total count of bacteria, total fungi, decay index, titratable acidity (TA), total soluble solids (TSS), colour, texture, ascorbic acid content and total phenolics was measured. The results showed that pulsed and continuous ultrasonic treatment significantly (P < 0.05) reduced the number of microorganisms and improved the quality of Mirabelle plums during storage. Increasing pretreatment time enhanced the positive effects of pulsed and continuous ultrasound. Also, in terms of the total count of bacteria, total fungi, titratable acidity and total phenolics, the pulsed and continuous ultrasound did not show a significant difference (P < 0.05). However, pulsed ultrasound was better compared to continuous mode in preservation of TSS, colour, texture and ascorbic acid content of the fruit during storage. Our results demonstrated that pulsed ultrasound is an appropriate method for improving safety and maintaining the quality of Mirabelle plum fruit.