Optimization of biodiesel production via transesterification of soybean oil using α-MoO3 catalyst obtained by the combustion method

A catalyst based on MoO₃ was synthesized by a simple and fast pilot-scale combustion reaction method and applied to the conversion of soybean oil to biodiesel via transesterification. For that, the statistical analysis of the catalyst amount and temperature, factors that influence the process, was evaluated by means of central composite design 2². MoO₃ was characterized in terms of structure by X-ray diffraction (XRD), textural characterization Brunauer-Emmett-Teller (BET), density by helium pycnometry (DE), particle size analysis (DG) and acidity tests by temperature-programmed desorption of ammonia (NH₃-TPD), chemical analysis by X-ray fluorescence (EDX), morphology by scanning electron microscopy (SEM) and catalytic properties. The transesterification products were characterized by gas chromatography (GC), acidity index (AI) and kinematic viscosity (KV). The results indicate the catalyst formation with a surface area of 1.36 m²g^?1, and density of 4.5 g/cm³ which consists of a single crystalline phase of orthorhombic configuration, with total NH₃ acidity of 33.61 μ.mol/g. Morphological characterization revealed that the catalyst is formed by irregular plates of various sizes and shapes, with a wide sizes range of agglomerated particles. In the soybean oil transesterification reactions, the catalyst was active showing 96.9% conversion to ethyl esters. The experimental design was meaningful and predictive, with a reliability level of 95%. The statistical analysis identified temperature as a significant variable for the adopted planning. To conclude, a new single-phase catalyst (α-MoO₃) has been developed and successfully applied to the biodiesel Synthesis from soybean oil. These results have a positive and promising impact for biodiesel production by transesterification of soybean oil against ethanol.     

一种通过梯形PPMgLN波导倍频实现带宽可调谐光源的理论研究

本文设计了一种梯形的周期极化掺镁铌酸锂(PPMgLN)波导,并通过在传播方向上引入温度梯度来拓宽其倍频(SHG)过程的泵浦光源可接收带宽。通过有限差分的光束传输法,计算波导的有效折射率,并进行波导尺寸的设计。结果表明,通过改变梯形波导不同位置的温度,使其形成一个温度梯度,可拓宽泵浦光源的波长可接收带宽。本文所设计的PPMgLN波导最大泵浦光源可接收带宽为C波段,即1 530~1 565 nm,该波导可倍频C波段,得到输出波段带宽为765~782.5 nm,温度调谐范围为30~150 ℃。     

Improved Method for the Total Synthesis of Azaperone and Investigation of Its Electrochemical Behavior in Aqueous Solution

Azaperone, with anti-anxiety and anti-aggressive activities used in veterinary medicine, is a member of the butyrophenone class. It is ordinarily utilized for a wide range of indications, such as sedation, obstetrics, and anesthesia. In this research, an improved synthetic route is presented for azaperone using a phase-transfer catalyst(PTC). In general, it was synthesized as a dopamine antagonist in four steps. The bis(2-chloroethyl) amine intermediate is easily obtained after the conversion of the alcohol groups into the chloride leaving group using thionyl chloride(95% yields). The alkylation of commercially available 2-amino pyridine in the presence of PTC was then carried out, giving 1-(pyridin-2-yl) piperazine with 75% yield. 1-(Pyridin-2-yl) piperazine was finally alkylated using 4-chloro-1-(4-fluorophenyl) butan-1-one to achieve azaperone with 60% yield. The butyrophenone intermediate was obtained via the Friedel-Crafts reaction of fluorobenzene with 4-chlorobutyryl chloride in the presence of AlCl₃. High efficiency, gentle reaction conditions, and fast and simple procedure are the advantages of this method. Also, the electrochemical oxidation behaviour of azaperone was investigated using cyclic and differential pulse voltammetry techniques. Cyclic voltammetric studies indicated an irreversible process for azaperone electro-oxidation with a peak potential of 0.78 V in a phosphate buffer solution(pH=7.0) vs. Ag/AgCl(saturated KCl) electrode. The value of the peak current vs. the azaperone concentration was enhanced linearly in the range of 10―70 μmol/L, and the detection limit was found to be 3.33 μmol/L.     

白云石制备似立方体状方解石型碳酸钙晶体及其机理研究

以轻烧白云石粉、氯化铵和二氧化碳为原料,在未使用晶型控制剂的情况下,通过蒸氨-沉钙过程制备出了似立方体状碳酸钙。研究了反应温度、溶液中钙离子浓度、通气速率、搅拌速度以及陈化时间对碳酸钙中方解石相含量以及晶体形貌的影响,并探索了沉钙反应的晶型控制机理。结果表明,在反应温度40 ℃、钙离子浓度0.05 mol/L、通碳速率100 mL/min、搅拌速度400 r/min和陈化时间2 h的条件下,制备出形貌规整、粒径分布均匀的似立方体状碳酸钙,平均粒径为5~10 μm。该研究为提升白云石的使用价值、生产高附加价值的碳酸钙产品,以及提高白云石资源的利用率提供理论基础。     

Interface‐fitted moving mesh method for axisymmetric two‐phase flow in microchannels

A boundary‐fitted moving mesh scheme is presented for the simulation of two‐phase flow in two‐dimensional and axisymmetric geometries. The incompressible Navier‐Stokes equations are solved using the finite element method, and the mini element is used to satisfy the inf‐sup condition. The interface between the phases is represented explicitly by an interface adapted mesh, thus allowing a sharp transition of the fluid properties. Surface tension is modelled as a volume force and is discretized in a consistent manner, thus allowing to obtain exact equilibrium (up to rounding errors) with the pressure gradient. This is demonstrated for a spherical droplet moving in a constant flow field. The curvature of the interface, required for the surface tension term, is efficiently computed with simple but very accurate geometric formulas. An adaptive moving mesh technique, where smoothing mesh velocities and remeshing are used to preserve the mesh quality, is developed and presented. Mesh refinement strategies, allowing tailoring of the refinement of the computational mesh, are also discussed. Accuracy and robustness of the present method are demonstrated on several validation test cases. The method is developed with the prospect of being applied to microfluidic flows and the simulation of microchannel evaporators used for electronics cooling. Therefore, the simulation results for the flow of a bubble in a microchannel are presented and compared to experimental data.     

Tb3Pd2, Er3Pd2 and Er6Co5–x: structural variations and bonding in rare‐earth‐richer binary intermetallics

The three binary Tb/Er‐rich transition metal compounds Tb₃Pd₂ (triterbium dipalladium), Er₃Pd₂ (trierbium dipalladium) and Er₆Co_5–x (hexaerbium pentacobalt) crystallize in the space groups Pbam (Pearson symbol oP20), P4/mbm (tP10) and P6₃/m (hP22), respectively. Single crystals of Tb₃Pd₂ and Er₆Co_5–x suitable for X‐ray structure analysis were obtained using rare‐earth halides as a flux. Tb₃Pd₂ adopts its own structure type, which can be described as a superstructural derivative of the U₃Si₂ type, which is the type adopted by Er₃Pd₂. Compound Er₆Co_5–x belongs to the Ce₆Co_2–xSi₃ family. All three compounds feature fused tricapped {TR₆} (R = rare‐earth metal and T = transition metal) trigonal prismatic heterometallic clusters. R₃Pd₂ is reported to crystallize in the U₃Si₂ type; however, our more detailed structure analysis reveals that deviations occur with heavier R elements. Similarly, Er₆Co_5–x was assumed to be stoichiometric Er₄Co₃ = Er₆Co_4.5. Our studies reveal that it has a single defective transition‐metal site leading to the composition Er₆Co_4.72(2). LMTO (linear muffin‐tin orbital)‐based electronic structure calculations suggest the strong domination of heteroatomic bonding in all three structures.     

One‐pot synthesis of a multi‐template molecularly imprinted polymer for the extraction of six sulfonamide residues from milk before high‐performance liquid chromatography with diode array detection

A highly selective molecularly imprinted polymer sorbent was synthesized and employed for the simultaneous determination of six sulfonamide antibiotic residues (sulfanilamide, sulfacetamide, sulfadiazine, sulfathiazole, sulfamerazine, and sulfamethizole) in milk samples. Multi‐analyte imprinted particles were used as a sorbent in solid‐phase extraction. Sulfonamides were separated on a high‐performance liquid chromatography column (Merck–Lichrospher RP18e, 5 μm 250 × 4 mm) and further identified and quantified by diode array detection. Several parameters including required loading of the molecularly imprinted polymer sorbent, mass of milk, volume, and type of elution solvent, as well as time for absorption and elution were investigated to obtain optimal experimental conditions. For comparison purpose, a non‐imprinted polymer was applied under the optimum conditions. The validation study according to the European Union Decision 2002/657/EC was based on the investigation of linearity, selectivity, stability, limits of detection and quantitation, decision limit, detection capability, trueness, precision, and ruggedness according to Youden's approach. The decision limit and detection capability values in the milk were achieved from 101.9 to 113.5 μg/kg and from 114.4 to 135.4 μg/kg, respectively, depending on the target sulfonamide drug. Finally, the optimized protocol was successfully applied to commercial milk samples and human breast milk.     

Separation and purification of scandium: From industry to medicine

Scandium and its compounds are used in many modern industrial fields due to its unique chemical and physical properties. It is mainly recovered from residues and wastes in the production of other metals. The exploitation of the ores and wastes could contaminate water and soil creating environmental problems. This paper discusses recent developments and tendencies in scandium separation, purification and preconcentration from different wastes, residues, environmental samples as well as in the production of radiopharmaceuticals for nuclear medicine, both in the laboratory and on the industrial scale. The period reviewed here mainly includes publications that have appeared, since 2010.     

Condensed Mode Cooling of Ethylene Polymerization in Fluidized Bed Reactors

This review gives an overview of the evolution of the technology of condensed mode cooling, primarily for the case of ethylene polymerization on supported catalysts in fluidized bed reactors. It is well known that this mode of heat removal is quite effective in allowing polyolefin manufacturers to increase significantly production rates. What is perhaps less well understood are all of the issues that, in addition to the effect of the latent heat of vaporization of injected liquid components, also have an impact on the rate of production and behavior of the reactor. However, the liquid components injected into the reactor can vaporize rapidly under full‐scale conditions, leaving behind several heavy components (with respect to ethylene) that have numerous effects on how the particles behave, on the reaction rate, and on fluidization, fouling, and other parameters related to reactor and process performance.