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.     

Comparison of Canola and Soy Flour with Added Isocyanate as Wood Adhesives

Canola is widely grown in the northern latitudes for its vegetable oil, generating large quantities of residual, low value canola flour used as animal feed. The common wood adhesive poly(diphenylmethylene diisocyanate) (pMDI) should react with the wide variety of functional groups in proteins. Therefore, it would seem that canola flour with added pMDI could be an effective adhesive. Two main questions are addressed in this study: How do the wood adhesive properties of canola flour compare to the better-studied soy flour? How well do proteins, which contain an abundance of functional groups, cure with the very reactive pMDI? These questions were addressed using the small-scale adhesive strength test ASTM D-7998, with various adhesive formulations and bonding conditions for canola flour plus pMDI compared to soy adhesives. The more challenging wet cohesive bond strength was emphasized because the dry strengths were usually very good. Generally, soy adhesives were better than canola ones, as was the polyamidoamine-epichlorohydrin cross-linker compared to pMDI, but these generalizations can be altered by the conditions selected. Three-ply plywood tests supported the small-scale test results.     

Dynamically vulcanized thermoplastic elastomer nanocomposites based on linear low-density polyethylene/styrene-butadiene rubber/nanoclay/bitumen: morphology and rheological behavior

Dynamically crosslinked thermoplastic elastomer nanocomposites were synthesized as modifier for the bitumen binder-based asphalts. Linear low-density polyethylene (LLDPE) and styrene-butadiene rubber (SBR), with the ratio of 80/20, bitumen, and organically modified clay (OC) were all melt mixed in the presence of the sulfur curing system. The proposed mixing was carried out in an internal mixer at 160 °C with a rotor speed of 120 rpm. To enhance the molecular interactions between the polymer phases and the clay silicate layers, maleic anhydride-grafted LLDPE (PE-g-MA) with the maleiation degree of 50% was also incorporated into the mixture. Observation of the composite samples, using the scanning electron microscopy (SEM), revealed the matrix dispersed type of morphology for all dynamically vulcanized samples. X-ray diffraction (XRD) and transmission electron microscopy (TEM) examinations evidenced the exfoliation of the clay silicate layers with good dispersion. Rheomechanical spectrometry (RMS) was performed on the prepared nanocomposites. All dynamically vulcanized nanocomposites comprising 2.5% of OC exhibited shear-thinning behavior and non-terminal characteristics with a low frequency range. These indicate the formation of three-dimensional physical networks by the clay nanolayers throughout the LLDPE matrix. The presence of the bitumen in the composition of the prepared nanocomposites improved the flowability of the samples. This is a promising feature of the prepared nanocomposites to be used as an elastic and resistant modifier in the composition of the bitumen-based asphalts.

     

Effect of various efficient vulcanization cure systems on the compression set of a nitrile rubber filled with different fillers

Effect of various efficient vulcanization (EV) sulfur cure systems on the compression set of a nitrile rubber filled with carbon black and silica/silane fillers was examined. The cure systems had different amounts of thiuram and sulfenamide accelerators and elemental sulfur, whilst the loading of zinc oxide and stearic acid activators was kept constant. The fillers had surface areas from 35 to 175 m²/g. In this study, the lowest compression set was measured for the rubber filled with carbon black with 78 m²/g surface area, which was cured with an EV cure system made of a small amount of elemental sulfur and large amounts of the two accelerators. Interestingly, a small change in the amount of elemental sulfur had a bigger effect on the compression set than did large changes in the loading of the accelerators in the cure system. Among the fillers, carbon black caused less compression set of the rubber vulcanizate than the silica/silane system did. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41512.     

First-principles DFT study of SO2 and SO3 adsorption on 2PANI: a model for polyaniline response

Interaction of SO_x (x?=?2,3) molecules on active sites of dianiline (as a model for polyaniline, denoted here as 2PANI) was studied using density functional theory at the BLYP-D/6-31+G(d) level of theory. Natural population analysis was used to find out the charge distribution as well as the net transferred charge of SO_x upon adsorption on 2PANI and the result has been compared with Mulliken charge analysis to evaluate the sensing ability of 2PANI. The computed density of states point to the remarkable orbital hybridization between SO_x and 2PANI during the adsorption process. As a consequence, the results of UV–VIS confirm the sensing ability of 2PANI toward SO₂ and SO₃. Based on our results, it can be found that at proper configuration the SO₂ and SO₃ molecules can be adsorbed on 2PANI with adsorption energies (E_ads) of ?18.2 and ?62.9?kJ/mol (BSSE), respectively.     

Comprehensive and Facile Synthesis of Some Functionalized Bis-Heterocyclic Compounds Containing a Thieno[2,3-b]thiophene Motif

A comprehensive and facile method for the synthesis of new functionalized bis-heterocyclic compounds containing a thieno[2,3-b]thiophene motif is described. The hitherto unknown bis-pyrazolothieno[2,3-b]thiophene derivatives 2a-c, bis-pyridazin othieno[2,3-b]thiophene derivatives 4, bis-pyridinothieno[2,3-b]thiophene derivatives 6a,b, and to an analogous bis-pyridinothieno[2,3-b]thiophene nitrile derivatives 7 are obtained. Additionally, the novel bis-pyradazinonothieno[2,3-b]thiophene derivatives 9, and nicotinic acid derivatives 10, 11 are obtained via bis-dienamide 8. The structures of all newly synthesized compounds have been elucidated by (1)H, (13)C NMR, GCMS, and IR spectrometry. These compounds represent a new class of sulfur and Nitrogen containing heterocycles that should also be of interest as new materials.     

Utilization of ZSM-5/MCM-41 composite as FCC catalyst additive for enhancing propylene yield from VGO cracking

A micro-mesoporous ZSM-5/MCM-41 composite molecular sieve (ZM13) was synthesized and tested as an FCC catalyst additive to enhance the yield of propylene from catalytic cracking of vacuum gas oil (VGO). The catalytic performance of the additive was assessed using a commercial equilibrium USY FCC catalyst (E-Cat) in a fixed-bed micro-activity test unit (MAT) at 520?°C and various catalyst/oil ratios. MCM-41, ZSM-5 and two ZSM-5/MCM-41 composites were systematically characterized by complementary techniques such as XRD, BET, FTIR and SEM. The characterization results showed that the composites contained secondary building unit with different textural properties compared to pure ZSM-5 and MCM-41. MAT results showed that the VGO cracking activity of E-Cat did not decrease by using these additives. The highest propylene yield of 12.2 wt% was achieved over steamed ZSM-5/MCM-41 composite additive (ZM13) compared with 8.6 wt% over conventional ZSM-5 additive at similar gasoline yield penalty. The enhanced production of propylene over composite additive was attributed to its mesopores that suppressed secondary and hydrogen transfer reactions and offered easier transport and accessibility to active sites. Gasoline quality was improved by the use of all additives except MCM-41, as octane rating increased by 6?C12 numbers.     

Physical and mechanical properties of a poly-3-hydroxybutyrate-coated nanocrystalline hydroxyapatite scaffold for bone tissue engineering

A major challenge for tissue engineers is the design of scaffolds with appropriate physical and mechanical properties. The present research discusses the formation of ceramic scaffolding in tissue engineering. Hydroxyapatite (HAp) powder was made from bovine bone by thermal treatment at 900?°C; 40, 50 and 60%wt porous HAp was then produced using the polyurethane sponge replication method. Scaffolds were coated with poly-3-hydroxybutyrate (P3HB) for 30?s and 1?min in order to increase the scaffold??s mechanical properties. XRD, SEM and FT-IR were used to study phase structure, morphology and agent groups, respectively. In XRD and FT-IR data, established hydrogen bands between polymer and ceramic matrix confirm that the scaffold is formed as a composite. The scaffold obtained with 50%wt HAp and a 30?s coating was 90% porous, with an average diameter of 100?C400???m, and demonstrated a compressive strength and modulus of 1.46 and 21.27?MPa, respectively. Based on these results, this scaffold is optimised for the aforementioned properties and can be utilised in bone tissue engineering.     

Optical Spectroscopic Analysis of High Density Lead Borosilicate Glasses

Lead borosilicate glasses, of chemical composition 20SiO₂-xPbO-(15 + x)B₂O₃-5WO₂-10ZnO-(50-2x) Na₂O (where x = 5, 10, 15, 20, 25) were prepared using the normal melt-quenching technique. The samples were examined using a Philips Analytical X-ray diffraction system in order to check their amorphous nature. The effect of increasing B₂O₃ and PbO content on glass transition temperature was examined using Differential Thermal Analysis measurements (DTA). The results of DTA showed that both melting and glass transition temperatures decrease with increase of lead and boron oxides. Density and its related parameters have been determined to study the effect of lead-boron content on the structural properties of the prepared samples. Based on the density and DTA results, the network forming role of Pb and B ions was proved. The optical properties of the glass samples have been obtained using UV-VIS measurements. The optical parameters, such as optical band gap, Urbach energy, refractive index, and electronic polarizability were deduced based on the optical data. The observed increase in optical band gap and decrease in Urbach energy as well as the red shift in the absorption spectra arise due to the formation of non-bridging oxygen.