Storage Stability of LiFePO4/C in Humid‐hot Air

Storage stabilities of LiFePO₄/C composite at different conditions are investigated in terms of structural and electrochemical evolutions. The results from different aging tests indicate that moisture and temperature are the key factors that have the most profound effects on the structure homogeneity which in turn influences the electrochemical performance of LiFePO₄/C. Although the storage in a humid‐hot environment, such as saturated humidity air at 50°C, does not greatly influence the discharging capacity of LiFePO₄/C, it does reduce the initial charging capacity, thus the amount of reversible Li⁺ ions in a practical LiFePO₄/graphite cell decreases. This impact is explained by the lithium extraction during the storage, forming olivine FePO₄ and associated Li₃PO₄. Elevated storage temperature also favors the delithiation process. The degree of delithiation increases from about 6% at 50°C to 18% at 80°C. It is also found that re‐calcination at 650°C effectively resolves the problem of the structural heterogeneity of the stored LiFePO₄/C. Therefore both the initial charging capacity and coulombic efficiency of the stored sample in the first cycle revert to the original value of the fresh one.     

锂离子电池负极材料ZnMn2O4微米空心球的制备和电化学性能

通过溶剂热方法合成了ZnMn2O4微米空心球,并探讨了其形成机理。采用XRD,SEM,TEM等测试手段对产物的结构、形貌和组成进行了表征。实验结果表明,溶剂热反应条件如反应温度、反应介质对于产物的结构和形貌起着关键作用。在140℃,采用乙醇和水作为反应介质,反应6 h可以制备出直径约3μm的ZnMn2O4微米空心球;当以乙醇为溶剂,反应6 h可以得到团聚的尺寸约250 nm的ZnMn2O4纳米颗粒。将所制备的ZnMn2O4微米空心球/纳米颗粒组装成锂扣式模拟电池,考察其电化学脱嵌锂性能。电化学测试结果显示,与ZnMn2O4纳米颗粒相比,空心结构的ZnMn2O4微米球具有较高的初始放电容量(1335 mAh·g-1)和较好的倍率性能,有望作为锂离子电池的新型负极材料。     

磁性可见光催化剂BiVO4/Fe3O4的制备及催化活性

采用超声法将磁基体Fe3O4和BiVO4复合,制备了易于固液分离的磁性可见光催化剂BiVO4/Fe3O4。采用X射线衍射(XRD)、傅立叶转换红外光谱(FTIR)、紫外-可见漫反射光谱(DRS)、透射电子显微镜(TEM)和磁学性质测量系统(MPMS)对产物进行了表征,并以亚甲基蓝为目标降解物,考察了BiVO4/Fe3O4的可见光催化活性。当BiVO4与Fe3O4质量比为5:1时,BiVO4/Fe3O4的催化活性最高,反应经过5 h,对亚甲基蓝的降解率达到92.0%,而单独使用BiVO4为催化剂,降解率仅为72.5%。这表明Fe3O4不仅起到磁基体的作用,还起到助催化剂的作用。BiVO4/Fe3O4在外加磁场的作用下很容易被分离,撤消外加磁场后,通过搅拌又可重新分散。BiVO4/Fe3O4 3次回收后的降解率仍高于80%。     

Convenient Synthesis of Terminal Alkynes from anti‐3‐Aryl‐2,3‐dibromopropanoic Acids Using a K2CO3/DMSO System

A convenient, efficient, and generally applicable method was developed for the synthesis of terminal alkynes from anti‐3‐aryl‐2,3‐dibromopropanoic acids in the presence of DMSO and K₂CO₃.     

Determination of metoprolol in rabbit blood using capillary electrophoresis with laser-induced fluorescence detection

This work described a sensitive method for determination of metoprolol in rabbit plasma.The method involved purification by ultrafiltration,derivatization with fluorescein isothiocyanate,determination by capillary electrophoresis(CE) coupled with laser-induced fluorescence(LIF) detector.Other components in plasma including a variety of amino acids and proteins did not interfere with the determination of metoprolol in experimental condition.The assay had a wide range(2.0-500 ng/mL) of linearity and a detection limit of 0.8 ng/mL.The intra- and inter-day precisions were satisfactory with relative standard deviation(RSD) less than 10.0%and accuracy within 10.0%.This method was successfully applied to pharmacokinetic study of metoprolol in rabbit blood.     

Dielectric analysis on phase transition and micelle shape of polyoxyethylene trisiloxane surfactant in dilute aqueous solution

The cloudy Silwet L-77 aqueous solution on the concentration range from 0.5%to 50%was investigated by dielectric relaxation spectroscopy.The concentration dependence of phase microstructure was confirmed by means of analyzing the dielectric parameters of bulk solution.The relaxation behavior was assigned to the interfacial polarization between the micelle and the medium,and the relaxation distribution parameter was used to figure the shape transition from sphere to ellipsoid with the concentration increasing.The synchronous reduction of permittivity and conductivity indicated the formation of the lamellar phase. As compensation,the quantity of the surfactant liquid phase gradually decreased,whose shape constantly kept ellipsoidal.     

High performance liquid chromatography with immobilized Ru(bpy)_3~(2+)-KMnO_4 chemiluminescence detection and its application in metabolism of repaglinide in pig liver microsomes

A novel high performance liquid chromatography-chemiluminescence（HPLC-CL） method for investigation of in vitro metabolism of repaglinide in pig liver microsomes with microdialysis sampling technique was developed.The chromatographic separation was performed on a Hypersil BDS-C18 column with an isocratic mobile phase consisting of methanol and 0.01 mol/L KH₂PO₄（pH 3.0）（volume ratio 75:25） at a flow rate of 1.0 mL/min.The detection was based on the chemiluminescence reaction of repaglinide with acidic potassium permanganate（KMnO₄） and tris（2,2’-bipyridyl）ruthenium（Ⅲ）(Ru（bpy）₃³⁺),which was immobilized on the cationic ion-exchange resin for obtaining high sensitivity and reducing consumption of expensive reagent.     

The first catalytic asymmetric addition of diethylzinc to aldehyde promoted by chiral thiourea

A series of C₂-symmetric and asymmetric chiral thiourea derivatives were synthesized from commercial L-phenylalanine.All of the new compounds have been fully characterized by IR,¹H NMR,¹³C NMR,MS spectra and elemental analyses.The chiral thioureas were used as chiral ligands in the catalytic enantioselective ethylation of aldehydes with diethylzinc,the corresponding sec-alcohols were gained with excellent enantioselectivities（up to 87.1%ee） and high yields（up to 76.7%） after the conditions were optimized.     

Synthesis and characterization of novel conjugated polymers based on 3-cyclobutene-1,2-dione moiety

Three novel conjugated polymers bearing 3,4-bis（4-hexylthiophen-2-yl）-3-cyclobutene-1,2-dione unit in their main chain have been synthesized successfully in good yields through Suzuki or Stille coupling reaction.Their molecular structures have been confirmed by FT-IR,¹H NMR and ¹³C NMR.All these copolymers exhibit broad and strong absorption bands in UV-vis region,and their optical band gaps are calculated to be 1.6-2.0 eV.suggesting that they have good coverage with the solar spectrum.These polymers have good thermostability and solubility in common organic solvents.Moreover,all these objective macromolecules possess high electron affinity of～3.8 eV determined from cyclic voltammetry measurement,implying that they are potential n-type polymeric photovoltaic materials.     

Synthesis and characterization of novel conjugated polymers based on 3-cyclobutene-l,2-dione moiety

Three novel conjugated polymers bearing 3,4-bis(4-hexylthiophen-2-yl)-3-cyclobutene-1,2-dione unit in their main chain have been synthesized successfully in good yields through Suzuki or Stille coupling reaction.Their molecular structures have been confirmed by FT-IR,~1H NMR and ~(13)C NMR.All these copolymers exhibit broad and strong absorption bands in UV-vis region,and their optical band gaps are calculated to be 1.6-2.0 eV.suggesting that they have good coverage with the solar spectrum.These polymers...