Separation of ephedrine stereoisomers by molecularly imprinted polymers--influence of synthetic conditions and mobile phase compositions on the chromatographic performance

Separation of ephedrine stereoisomers by molecularly imprinted polymers was performed to study the factors that affect the selectivity and column efficiency. The polymer synthesized with pentaerythritol triacrylate as the cross-linker and chloroform as the porogen was found to have the best overall separation performance. Investigation of the recognition mechanism by NMR and chromatographic analysis revealed that the major binding forces between the polymer stationary phase and ephedrine are the ionic and hydrogen bonding interactions. Studies of the influence of mobile phase compositions on the HPLC analysis have shown that a methanol-aqueous buffer was the suitable mobile phase for the separation in which pH, ionic strength and water content can be adjusted to optimize the chromatographic analysis.     

基于富勒烯和噻吩聚合物的本体异质结太阳电池

随着全球能源需求量的逐年增加,对可再生能源的有效利用成为亟待解决的问题。现在使用的能源多来自矿物燃料的开采,其中包括石油、天然气和煤等,而这些资源是非常有限的。因此,发展新能源和新能源材料是我国进入21世纪必须解决的重大课题,其中太阳能被认为是清洁可再生新能源的代表之一。基于噻吩跟富勒烯的异质结太阳能电池是目前太阳能电池的重要发展方向之一。该种太阳能电池因其制备简单、成本低廉、重量轻和可制成柔性器件等优点近年来受到多方的广泛重视。经过努力,该种太阳能电池的光电转化性能已经得到了一定提高,最高光电转化效率已达到7%左右,但是跟无机半导体硅和染料敏化太阳能电池相比还有一定差距。因此,这方面的研究任重而道远,研究空间也非常大。本文从材料合成的角度,简要综述了近年来国内外在基于富勒烯和噻吩的异质结太阳能电池方面所取得的最新研究进展,并对下一步需要研究的热点问题作了展望。     

Synergistic effects between silicon-containing flame retardant and potassium-4-(phenylsulfonyl)benzenesulfonate (KSS) on flame retardancy and thermal degradation of PC

A novel flame retardant (PSiN), containing silicon and nitrogen, was synthesized using N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane (KH-602) and diphenylsilanediol through solution polycondesation and it was used together with potassium-4-(phenylsulfonyl)benzenesulfonate (KSS) to prepare a flame-retardant system for polycarbonate (PC). The structure and thermal property of PSiN were characterized by Fourier transform infrared spectroscopy (FTIR), ¹HNMR and thermogravimetric analysis (TG) tests. Flammability and thermal behaviors of PC/KSS/PSiN systems were estimated by limited oxygen index (LOI), cone calorimeter, vertical burning test (UL-94), and TG tests. The results showed that the flame retardancy and char residues of PC/KSS system were improved with the addition of PSiN. When 1 mass% PSiN and 0.5 mass% KSS were incorporated, the LOI value of PC was found to be 46, and class V-0 of the UL-94 test. Moreover, both the heat release rate and the total heat release of PC/KSS/1 mass% PSiN decreased compared with those of PC and PC/KSS systems. The microstructures observed by scanning electron microscopy and FTIR indicated that the surface of the char for PC/KSS/PSiN system hold a more cohesive and denser char structure when compared with the pure PC and PC/KSS system.     

Effects of common synergistic agents on intumescent flame retardant polypropylene with a novel charring agent

In this article, the laboratory-made poly (p-ethylene terephthalamide) (PETA) was used as a novel charring agent and it combined with ammonium polyphosphate (APP) to prepare the intumescent flame retardant (IFR). For improving the flame-retardant efficiency of IFRs on polypropylene (PP), several general synergistic agents, such as common zinc oxide (Com-ZnO), nanometer structural zinc oxide (Nano-ZnO), zeolite 4A, and aluminum hypophosphite(Al(H₂PO₂)₃), were added in composites of PP/IFR, and the synergistic effect was investigated by the limited oxygen index (LOI), the UL-94 (vertical flame) test, thermogravimetric analysis (TG), thermogravimetry-fourier transform infraredspectroscopy (TG-IR) test, and scanning electron microscopy (SEM). It indicated that the flame retardancy was significantly enhanced in terms of prompting the char formation of PETA and interaction between APP and synergistic agents. Overall, Al(H₂PO₂)₃ was the most effective synergistic agent among them. TG-IR analysis showed that the addition of Al(H₂PO₂)₃ could delay the release of NH₃, and make the release of NH₃ more smooth, which was useful to form a dense char. SEM presented that compact, continuous and good intumescent charring layers were observed in all PP/IFR systems with synergistic agent.     

Synthesis of Methyl N‐Aryl Oxamate Using Soluble Polymer Support

A variety of methyl N‐aryl oxamates were synthesized using poly(ethylene glycol) (PEG) as a soluble polymer support and a monoproctection group with excellent yields.     

Boc-protected 1-(3-oxocycloalkyl)ureas via a one-step Curtius rearrangement: mechanism and scope

1-(3-Oxocyclobutyl) carboxylic acid (4a) was converted into N-Boc-protected 1-(3-oxocyclobutyl) urea (5a), a key intermediate for the preparation of agonists of metabotropic glutamate receptor 5, in one-step when treated with diphenyl phosphoryl azide and triethylamine in tert-butanol. The mechanism of the reaction involves a nucleophilic addition of the in situ generated tert-butyl carbamate to the isocyanate intermediate. This reaction is applicable to other 1-(3-oxocycloalkyl) carboxylic acids but not to linear γ-keto carboxylic acids.     

Conductive 2D Metal-organic Framework (Co,NiCo, Ni) Nanosheets for Enhanced Non-enzymatic Detection of Urea

2D metal-organic framework (MOF) has potential applications in electrocatalysis owing to fast mass transfer, charge transfer and large specific surface area. Here, we had prepared three conductive 2D MOF based on Ni, NiCo and Co in a simple and rapid way. The 2D nanostructure of MOF was confirmed by SEM and TEM. The chemical composition was studied by XRD, Raman and XPS spectrum. The electrochemical oxidation and detection was investigated through cyclic voltammetry and current-time method. Their sensing performance for urea was determined by varying oxidation potentials and metal sites. The non-enzymatic Ni-, NiCo- and Co-MOF sensors had good catalytic activity for urea. Compared with NiCo- and Co-MOF, Ni-MOF had a wider linear range (0.5–832.5 μM), high sensitivity (1960 μA mM⁻¹ cm⁻²), low detection limit (0.471 μM), and fast response time. The sensors had well repeatability, reproducibility, and selectivity to specific interfering species. Furthermore, Ni- and NiCo-MOF modified electrode was also applied to detection of milk samples. The results showed that the recovery was satisfactory, which further confirmed the effectiveness of non-enzyme sensor. In general, the highly-sensitive 2D Ni- and NiCo-MOF modified electrode has great potential as nonenzymatic urea sensors for real samples detection in hydrogen energy, clinical diagnostics, and environmental protection, et al.