Gold(I)-catalyzed synthesis of 1,5-benzodiazepines directly from o-phenylenediamines and alkynes

A unique gold(I)-catalyzed highly atom-economic synthesis of 1,5-benzodiazepines directly from o-phenylenediamines and alkynes has been achieved for the first time.     

芳香硝基化合物原位液相加氢一锅法合成喹啉类化合物

以芳香硝基化合物为起始原料,以2%Pt-Sn/γ-Al2O3为催化剂,采用原位液相加氢法可以一锅法合成喹啉类化合物,考察了Pt/Sn摩尔比、反应温度、原料浓度和水含量等对反应性能的影响.结果表明,在Pt/Sn摩尔比0.5,220oC,5.0MPa,原料浓度6%,水含量30%及反应物停留时间为72s的条件下,生成产物6-甲氧基-2-甲基喹啉的收率可达72%.     

不锈钢丝网上Cu基催化剂的制备及反应性能

采用阳极氧化技术在不锈钢丝网上成功地自生长了结构致密的氧化物膜,并以此为载体,通过电化学沉积工艺制备了Cu/不锈钢丝网催化剂。以甲苯、丙酮、乙酸乙酯及二氯甲烷为模型反应,考察了4种不同种类挥发性有机化合物(VOCs)在该催化剂上的完全氧化活性。结果表明电化学沉积时间为15 min制备得到的催化剂上完全氧化丙酮、甲苯、乙酸乙酯及二氯甲烷的温度分别为240、220、260和440℃。在220℃反应条件下进行60 h的甲苯氧化稳定性试验结果显示该催化剂催化氧化甲苯的转化率一直保持98%以上,表现出较好的稳定性。扫描电镜,X射线衍射及X射线光电子能谱等表征结果表明,不锈钢丝网载体表面的阳极氧化物膜有利于提高活性组分的分散度。设计采用电沉积工艺大大提高了催化剂表面活性物种与载体的结合牢固度。     

Noncrystalline blue-emitting 9,10-diphenylanthracene end-capped with triphenylamine-substituted fluorene

Two blue-emitting oligomers, namely FDPA1 and FDPA2 containing 9,10-diphenylanthracene core end-capped with triphenylamine-substituted fluorene has been synthesized and characterized. The spiro-configuration end-capping groups imparts two compounds with pronounced morphological stability (T_g > 185 °C, T_d > 420 °C) and excellent hole injection ability (E_HOMO > −5.27 eV) with the advantageous optical characteristics of corresponding core. Scanning electron microscope (SEM) and X-ray diffraction (XRD) reveal that the two oligomers form excellent amorphous films and possess good morphological stability after annealing.     

Effects of Li2CO3 as a secondary lithium source on the LiFePO4/C composites prepared via solid-state method

Li₂CO₃ was used as the secondary lithium source for the synthesis of LiFePO₄/C composites via a solid-state reaction method by adopting Li₃PO₄ as the main lithium source. The main purpose of using Li₂CO₃ is to compensate for the partial lithium loss during the sintering while reducing the usage of excess Li₃PO₄. In this study, the effects of Li₂CO₃ amount on the phase, structural and electrochemical properties of LiFePO₄/C material were systematically investigated. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), constant-current charge–discharge test and cyclic voltammetry (CV). The results showed that by adding an appropriate amount of Li₂CO₃, the impurities, e.g. Li₃PO₄, normally appearing in the final product, could be excluded. It was found that LiFePO₄/C with Li₂CO₃ in 6% excess (vs. stoichiometric LiFePO₄) exhibited the best electrochemical performance, which delivered initial discharge capacities of 141.7, 125.2, 119.9 and 108.9 mAh g^?1, respectively, at 0.5, 1, 2 and 5C rates. The capacity was reduced to 113.4 mAh g^?1 after 50 cycles at 2C rate, with capacity retention rate of 94.6%.     

New ternary molten salt electrolyte based on alkali metal triflates

A novel molten salt electrolyte composed of lithium triflate (CF₃SO₃Li, LiTf), sodium triflate (CF₃SO₃Na, NaTf), and potassium triflate (CF₃SO₃K, KTf) has been prepared and characterized by thermogravimetry/differential thermal analysis (TG/DTA), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry. TG/DTA shows that the electrolyte was thermally stable when the temperature was under 400 °C. Its thermal stability gradually decreased with increase of LiTf concentration. The ionic conductivity of molten salt electrolyte has been evaluated by EIS and its value exceeds 10⁻² Scm⁻¹ in the temperature range from 230 to 270 °C. The electrochemical window of the electrolyte at the molar ratio of 0.5/1/1 is about 4.7 V at 250 °C. This electrolyte with low melting point exhibits promising characteristics for high-temperature lithium batteries.     

Efficient synthesis of β-enaminoesters via highly stereoselective Reformatsky reaction with disubstituted formamides as novel electrophiles

An efficient synthesis of various β-enaminoesters has been achieved via Reformatsky reaction with disubstituted formamides as novel electrophiles. The exclusive β-enaminoester E-isomers were obtained in 60-72% yield.     

C-LiFePO4/聚三苯胺复合锂离子电池正极材料的制备与性能

通过低温溶剂热法和高温热处理技术合成了橄榄石结构的LiFePO₄/carbon (C-LiFePO₄)纳米材料. 在此基础上,通过溶液共混法制备了一种新型的聚三苯胺(PTPAn)修饰包覆的C-LiFePO₄复合锂离子电池正极材料(C-LiFePO₄/PTPAn). 利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、电化学阻抗谱(EIS)以及恒电流充放电等测试方法,考察PTPAn 包覆量对C-LiFePO₄/PTPAn 复合正极材料性能的影响. 结果表明：通过溶液共混法PTPAn能够致密地包覆在C-LiFePO₄表面,形成一个有效的电子/离子传输通道从而有效提高CLiFePO₄基复合材料的电化学活性. 所有样品中C-LiFePO₄/10% (w) PTPAn作为正极材料呈现出最佳的电化学性能,在0.1C倍率恒流充放电下材料首次放电比容量为154.5 mAh·g^-1,在10C高倍率恒流充放电下材料的放电比容量达到114.2 mAh·g^-1. 当C-LiFePO₄/PTPAn 复合材料表面包覆的PTPAn 含量进一步增加,复合材料的电化学性能出现下降的趋势. 电化学阻抗测试表明PTPAn包覆层明显减小了C-LiFePO₄电极的电荷转移电阻.     

组合型Pt/TiO_2催化剂用于低温催化甲苯完全氧化

将均匀分布的纳米Pt粒子直接吸附到TiO2载体上,即制得了组合型Pt/TiO2催化剂(Pt/TiO2-AS).与浸渍法制备的Pt/TiO2催化剂(Pt/TiO2-WI)比较,Pt/TiO2-AS催化剂在催化甲苯完全氧化反应中表现出了很好的催化性能,甲苯转化率为100%时的反应温度低至150°C,而且即使在较高甲苯浓度和较高气体空速下,该催化剂也能保持较好的催化性能.通过X射线衍射(XRD)、N2吸附-脱附(BET)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、氢气程序升温还原(H2-TPR)及傅里叶变换红外(FTIR)光谱等对两种Pt/TiO2催化剂的结构和表面性能进行了表征.结果表明组合型Pt/TiO2-AS催化剂粒径小(2.5 nm),活性组分主要以Pt0形式存在且分布在载体表面,而且载体表面Ti―O键活化使催化剂具有较强的催化氧化能力.另外,活性中心的价态变化(Pt0→Ptδ+)是导致Pt/TiO2-AS催化剂失活的主要原因.     

HPLC间接测定电氧化合成中的茴香醛二甲基缩醛

在无水KF-CH3OH体系中直接电氧化合成的茴香醛二甲基缩醛(p-MBDMA)遇水易发生水解。研究表明在甲醇、乙腈和水的酸性混合溶液中,p-MBDMA在色谱柱中能迅速彻底地水解为茴香醛,故利用其水解反应建立了一种间接测定p-MBDMA的高效液相色谱(HPLC)方法。选择最佳流动相为水-甲醇-乙腈(50:30:20),用磷酸调节pH值至3.0,并探讨了测定机理。建立的HPLC测定方法准确、可靠,已应用于电化学合成p-MBDMA的分析,并可满足工业化生产的分析要求。