Copper(I) selenophene-2-carboxylate (CuSC) promoted C–S cross-coupling reaction of thiols with aryl iodides

We reported the synthesis of copper (I)-selenophene-2-carboxylate (CuSC) and application as new catalyst in the cross-coupling reactions of thiols with aryl iodide to afford the corresponding unsymmetrical thioethers. The optimized reaction conditions were applied to thiols and aryl iodides having a wide range of functional groups, including electron rich and electron poor substrates. The chemoselectivity of the reaction with 4-iodobromobenzene and 2-aminothiophenol derivatives was briefly examined through the competitive iodine versus bromine and thiol versus nitrogen cross-coupling.     

High surface area LaNiO<Subscript>3</Subscript> electrodes for oxygen electrocatalysis in alkaline media

LaNiO₃ coatings on nickel-foam supports were prepared by brush painting. The electrochemical properties were investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Comparative studies were performed with LaNiO₃-pelleted electrodes. The roughness factors were determined by CV and found to be 5,208 ± 350 and 4,037 ± 250 for the pelleted and coated electrodes, respectively. EIS measurements confirm the results obtained by CV. Values lower than 0.3 were calculated for the morphology factors for both electrodes, indicating low electrochemical porosity. The experimental method used in this work to synthesise the oxide coupled with the use of Ni foam as support has proved to be very effective in producing oxide electrodes with surface areas higher than those referred to in relevant literature.     

Application of Multivariate Analysis in Mid-Infrared Spectroscopy as a Tool for the Evaluation of Waste Frying Oil Blends

Mid-infrared spectroscopy, in association with multivariate chemometric techniques, was employed for pattern recognition and the determination of the composition of waste frying oils (WFO); data are presented in terms of the percentage of soybean oil, palm oil and hydrogenated vegetable fat in frying oil blends. Principal component analysis (PCA) was performed using spectral data (3,000–600 cm⁻¹) to discriminate between the samples containing 100% soybean oil, 100% palm oil, 100% hydrogenated vegetable fat groups and their blends. Additionally, the results indicated that partial least squares (PLS) models based on mid-infrared spectra were suitable as practical analytical methods for predicting the oil contents in WFO blends. PLS models were validated by a representative prediction set, and the root mean square errors of prediction (RMSEP) were 2.8, 4.7 and 5.5% for palm oil, soybean oil and hydrogenated vegetable fat, respectively. The proposed methodology can be very useful for the rapid and low cost determination of waste frying oil composition while also aiding in decisions regarding the management of oil pretreatment and production routes for biodiesel production.     

Water soluble polymeric nanofibres for rapid flocculation and enhanced dewatering of mature fine tailings

Water-soluble polymer flocculants have been used to efficiently release entrapped water in oil sands tailings by bridging fine particles to create large heavier flocs which can then settle faster and release water more efficiently. Due to their initial interaction with the fine particles suspended in tailings, polymer nanofibres may perform better than their parent polymers because of the entire surface of the nanofibres being fully accessible to the fine particles. In this work, commercially available poly(acrylamide-co-diallyl dimethylammonium chloride) was chosen as a basis for this study. Initial settling rate, supernatant turbidity, water recovery, capillary suction time, and solids content were measured to determine the effect of polymer nanofibres on solid-liquid separation. The solid forms of the polymer (either as nanofibre or powder) perform better than the polymer solution in each test, with optimum dosages of 5 wt% mature fine tailings (MFT) loading. Nanofibres could achieve settling rates of 60 m/h, while the other forms were only able to achieve 42 m/h. Additionally, the turbidity of the supernatant obtained after flocculation with nanofibres was 15 nephelometric turbidity units (NTU), while the polymer solution and powder produced turbidites of 162 NTU and 70 NTU, respectively. In addition, polymer nanofibres and powders generated larger flocs compared to the polymer solution, which produced small, homogenized flocs.     

Niobium and tantalum recovery from the primary source and from tin slag,an industrial challenge: A review

Niobium (Nb) and Tantalum (Ta) are used to increase materials' mechanical resistance and produce lighter alloys. Worldwide Nb production reached 78 000 t in 2020. The reduced ore offer justifies the recycling of these metals from tin slag, contributing to the circular economy. Nb₂O₅ and Ta₂O₅ extraction either from the primary source or the tin slag is an industrial challenge. Nb and Ta dissolution processes already implemented are fluoride leaching, sulphuric leaching, alkaline leaching, and alkaline roasting. The fluoride process raises environmental concerns about waste control. The sulphuric method can be managed to have higher Nb and Ta extraction in a less aggressive process, if some changes are implemented, such as increasing the number of extraction steps, decreasing the pulp density, or increasing the temperature; however, the efficiency of this methodology must be tested for tin slag. The alkaline method seems to be more selective to Nb and Ta by reactants and temperature control. Despite those well-established Nb and Ta treatments, they must be adapted to recover Nb and Ta from slag. The slag has low Nb and Ta content, while high Si and Ca concentrations exist in the matrix. This paper brings the main methods used to extract the Nb and Ta from the primary resources and an overview of Nb and Ta recovery from the slag. This investigation comes as a tool to guide the development of new methods to recover Nb and Ta from low-grade sources such as tin slag.     

HDPE/LLDPE reactor blends with bimodal microstructures—part I: mechanical properties

Reactor blends of polyethylene/poly(ethylene-co-1-octene) resins with bimodal molecular weight and bimodal short chain branching distributions were synthesized in a two-step polymerization process. The compositions of these blends range from low molecular weight (LMW) homopolymer to high molecular weight (HMW) copolymer and, vice versa, HMW homopolymer to LMW copolymer. The physical properties of the blends were found to be consistent with the nature of the individual components. For the tensile properties, the stiffness decreases with increasing the fraction of the copolymer, regardless of the molecular weight of the homopolymer fraction. For these blends with bimodal microstructures, it was confirmed that the degree of crystallinity governs the stiffness of the polymer. However, the energy dampening properties of the polymers benefit from the presence of the copolymer. A balance of stiffness and toughness can be obtained by altering the composition of the blends. For some blends, the presence of HMW homopolymer can dominate the tensile properties, showing little variation in the stiffness with increased addition of copolymer. It was also demonstrated that the testing conditions and thermal treatment of the polymer greatly influence the resulting elastic and energy dampening properties. Depending on the desired application, annealing these polymers (especially very low density copolymers) not only increases the crystallinity and stiffness, but also changes the frequency response of the dynamic mechanical properties.     

Ammonium complex of niobium as a precursor for the preparation of Nb2O5/Al2O3 catalysts

Ammonium oxalate complex of niobium was investigated as an aqueous precursor for the preparation of x% Nb₂O₅/Al₂O₃ (x=5, 10, 20 and 30 wt.%) samples. Catalysts with the same Nb₂O₅ contents were also prepared from the traditional niobium oxalate/oxalic acid aqueous solution. The catalysts were characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), temperature-programmed reduction (TPR), infrared spectroscopy of chemisorbed pyridine and X-ray photoelectron spectroscopy (XPS). A comparison with the preparation method using the niobium oxalate salt was performed. The results showed that the niobium precursor influence the species growing leading to phases with different reducibility. The XPS revealed the presence of multilayers of niobium oxide on the Nb₂O₅/Al₂O₃ samples prepared by using niobium ammonium oxalate complex, while the ones obtained from niobium oxalate led to Nb₂O₅ particles islands. The addition of niobium oxide decreased the fraction of Lewis acid sites and increased the fraction of Brønsted acid sites, independent of the precursor salt. However, the creation of BAS was more pronounced on the Nb₂O₅/Al₂O₃ samples prepared from niobium oxalate.     

Periplasmic expression of human growth hormone via plasmid vectors containing the {lambda}PL promoter: use of HPLC for product quantification

The influence of different factors acting on Escherichia coliperiplasmic expression of recombinant human growth hormone (hGH)in shake flask cultures has been investigated. Bacterial vectorscontaining the phage