Preparation of a novel molecularly imprinted polymer for the highly selective extraction of baicalin

The selective extraction of baicalin is important to its quality control especially when the matrices are complicated. In this work, a novel molecularly imprinted polymer was prepared for the selective extraction of baicalin in herbs. The molecularly imprinted polymer was synthesized by the copolymerization of 4‐vinyl pyridine and ethylene glycol dimethacrylate in the presence of baicalin by a precipitation polymerization method. After the optimization of parameters for molecularly imprinted polymer preparation, including the functional monomer, porogen, sampling solvent, and washing solvent, good selectivity was obtained, with an imprinting factor of about 4, which is much better than that achieved by the bulk‐polymerization method. The performances of the prepared molecularly imprinted polymers were systematically investigated, including adsorption kinetics, isotherm experiment, and Scatchard analysis. On the basis of the good adsorptive capability of the prepared molecularly imprinted polymer, it was also applied for the pretreatment of baicalin in Scutellaria baicalensis Georgi. The result showed that most of the matrices were removed and baicalin was selectively enriched.     

Dopant-free NiOx Nanocrystals: A Low-cost and Stable Hole Transport Material for Commercializing Perovskite Optoelectronics

Advancing inverted (p-i-n) perovskite solar cells (PSCs) is critical for commercial applications given their compatibility with different bottom cells for tandem photovoltaics, low-temperature processability (≤100 °C), and promising operational stability. Although inverted PSCs have achieved an efficiency of over 25 % using doped or expensive organic hole transport materials (HTMs), their synthesis cost and stability still cannot meet the requirements for their commercialization. Recently, dopant-free and low-cost non-stoichiometric nickel oxide nanocrystals (NiO_x NCs) have been extensively studied as a low-cost and effective HTM in perovskite optoelectronics. In this minireview, we summarize the synthesis and surface-functionalization methods of NiO_x NCs. Then, the applications of NiO_x NCs in other perovskite optoelectronics beyond photovoltaics are discussed. Finally, we provide a perspective for the future development of NiO_x NCs for the commercialization of perovskite optoelectronics.     

Extraction and characterization of highly pure alumina (α, γ, and θ) polymorphs from waste beverage cans: A viable waste management approach

The recycling and recovery of important materials from inexpensive feedstock has now become an intriguing area and vital from commercial and environmental viewpoints. In the present work, extraction of different single phases of alumina (α, γ, θ-Al₂O₃) having high purity (>99.5 %) from locally available waste beverage cans (～95 % Al) through facile precipitation route calcined at distinct temperatures has been reported. The optimization of process technology was done by a variety of different synthesis parameters, and the production cost was estimated between 84.47-87.45 USD per kg of alumina powder. The as prepared alumina fine particles have been characterized using different sophisticated techniques viz. TG-DTA, WD-XRF, XRD, FT-IR, SEM, DLS-based particle size analysis (PSA) with zeta (ζ) potential measurement and UV–Visible Spectroscopy. X-ray diffractogram confirms the formation of γ-, θ-, and α-alumina at 500–700 °C, 900–1000 °C, and 1200 °C respectively and crystallite size, crystallinity, strain, dislocation density, and specific surface area were measured using major X-ray diffraction peaks which varies with temperature. The SEM studies showed that the as prepared alumina particles were agglomerated, irregular-shaped with particle size (0.23–0.38 µm), pore size, and porosity were calculated from SEM image. ζ-potentials at different pH values as well as isoelectric point (IEP) of α, γ, and θ alumina were calculated in an aqueous medium which changes with temperature. The direct band gap (E_g) energies were found between 4.09 and 5.19 eV of alumina obtained from different calcination temperatures. The synthesized materials can be used in sensors, ceramics, catalysis, and insulation applications.     

Copolymeric nano/microgels of N-isopropylacrylamide and carboxyalkyl methacrylamides: Effect of methylene chains and the ionization state of the weak acids on size and sensitivity to pH and temperature

ABSTRACT

We prepared nano/microgels by precipitation copolymerization of N-isopropylacrylamide (NIPAAm), and one of three different carboxyalkyl methacrylamides [methacryloylamido hexanoic acid (M₅), 8-methacryloylamido octanoic acid (M₇), and 11-methacryloylamido undecanoic acid (M₁₀)], either in the acid forms or as carboxylates (potassium salts). The hydrodynamic diameter (Dh) of the nano/microgels prepared with the carboxylates was smaller (≈100 nm for M₁₀ copolymers), compared to the size of homopolymeric NIPAAm microgels prepared by dispersion polymerization (around 600 nm), indicating that the carboxylates act as surfactants reducing the size of the seeds during the polymerization process. These materials presented a swollen-shrunken transition temperature (T _tr) similar to the T _tr of the homopolymeric NIPAAm microgels, without pH sensitivity. On the other hand, the copolymeric microgels prepared from the acid form of the comonomers have a similar or bigger size than NIPAAm microgels. For these copolymers, the T _tr can be tuned by the type and proportion of acid comonomer used and present pH sensitivity. This is important for biomedical applications such as positive temperature control release. Polyelectrolyte titration demonstrates that the nano/microgels prepared with the carboxylates behave as hard spheres, while the microgels prepared with the weak acid behave as porous materials.     

Improved performance of porous LiFePO4/C as lithium battery cathode processed by high energy milling comparison with conventional ball milling

Porous LiFePO₄ is synthesized and coated with amorphous carbon by using high energy nano-mill (HENM) processed solid-state reaction method. FeCl₃ (38%) containing water solution which is originated from pickling of steel scrap (waste liquid) is used as a source material in this study. The result indicates that LiFePO₄ powders are well coated with the amorphous carbon. HENM process successfully produces the porous LiFePO₄ with homogeneously distributed pores and a well networked carbon web, which delivers an enhanced electrochemical rate capability. HENM process is incorporated as an effective route for reducing particle size, distributing particle homogeneously and averting agglomeration of particles of precursor in this study. X-ray diffraction, scanning electron microscopy with elemental mapping, transmission electron microscopy with selected area (electron) diffraction, Raman spectroscopy, cyclic voltammetry, and galvanostatic charge/discharge are employed to characterize the final product. Electrochemical measurement shows that the synthesized LiFePO₄/C composite cathode delivers an initial discharge capacity of 161 mAhg⁻¹ at 0.1C-rate between 4.2 and 2.5 V. Remarkably, the cathode delivers 101.9 mAhg⁻¹ at high charge/discharge rate (10 C).     

Study on the Agglomeration Kinetics of Uranium Peroxide

Considering the previous study dealing with thermodynamic and kinetic phenomena (nucleation and crystal growth) during the uranium peroxide precipitation, this work focuses on the agglomeration mechanism. It provides the results obtained from the experiments carried out in a MSMPR reactor operating at steady state. The influence of the operating parameters on the uranium peroxide agglomerates was studied in order to identify the agglomeration kernel. The method is based on the resolution of the population balance equation using the method of moments and the experimental particle size distributions. The results lead to a size-independent kernel directly proportional to the crystal growth rate. Under the stirring conditions studied, the agglomeration appears to be significantly reduced by mixing which results in a kernel inversely proportional to the average shear rate. The agglomeration kinetic law obtained in this study will be used for the process modelling in a further study.     

A novel and simple pathway to synthesis of porous polyurea absorbent and its tests on dye adsorption and desorption

A novel one-step protocol for the preparation of porous polyurea material (PPU) through precipitation polymerization of toluene diisocynate (TDI) is presented. The process is based on step polymerization of one singlemonomer, TDI, with water in water-acetonemixed solvent. PPU is obtained without need for any porogen or additives, and no any chemical modification on the outcome polymer is necessary. The morphology, pore size and size distribution of PPU are characterized by scanning electron microscope and BET nitrogen adsorption. Taking acid fuchsine (AF) and Congo Red as dye examples in wastewaters, their adsorption on, desorption from PPU and the reusability of PPU were tested. Experimental conditions for AF adsorption were optimized with regard to pH, adsorption time, AF concentration and amount of PPU. Results demonstrate that the as-prepared PPU is of high performance in dyes adsorption and recycled use. This work presents therefore a novel and attractive candidate for removal of anionic dyes from wastewaters.     

Selective solvation effects in phase separation in aqueous mixtures

Selective solvation can be crucial in phase separation in polar binary mixtures (water–oil) with a small amount of hydrophilic ions or hydrophobic particles. They are preferentially attracted to one of the solvent components, leading to a number of intriguing effects coupled to phase separation. For example, if cations and anions interact differently with the two components, an electric double layer emerges at a liquid–liquid interface. The main aim of this paper is to show that a strongly hydrophilic (hydrophobic) solute induces precipitation of water-rich (oil-rich) domains above a critical solute density n_p outside the solvent coexistence curve.     

Effects of cosolvent on formation and morphology of microspheres in precipitation polymerization of divinylbenzene in supercritical carbon dioxide

Precipitation polymerizations of divinylbenzene(DVB) in pure supercritical carbon dioxide,and parallel runs with presence of a cosolvent were carried out.The results showed that use of acetone as the cosolvent contributed greatly to the formation of the monodisperse microspheres.PDVB microspheres,with obviously higher uniformity than reported up to date,were achieved using 6-7 mL of acetone in a reactor of 50 mL with DVB concentration of 0.4 mol/L under 16 MPa,a much lower pressure than previously reported without use of cosolvent.