含二氧杂环异黄酮的合成

本文报道含有3', 4'-亚甲二氧基, 3', 4'-亚乙二氧基, 3, 4'-三亚甲二氧基的异黄酮类化合物的合成, 所得25个新化合物的结构经元素分析、^1H NMR谱确证; 紫外光谱表明有异黄酮特征吸收。文中并对反应机理进行了探讨。     

碱性介质中高择优取向（220）镍电极上丙醇的电氧化

对１．０ｍｏｌ／ＬＮｉＳＯ４和０．５ｍｏｌ／Ｌ Ｈ３ＢＯ３体系，控制电位为一１．２５Ｖ，沉积６０ｍｉｎ，制得高择优取向镍电极。该镍电极经Ｘ射线衍射测定其织构度ＴＣ２２０为９２％。采用循环伏安法研究了１ｍｏｌ／Ｌ ＮａＯＨ溶液中高择翁取向镍电极上丙醇的电催化氧化机理有活性，结果表明：高择优取向镍电极对正丙醇的电催化活性高，对异丙醇的电催化活性小；推导出正丙醇的电氧化动力学方程，运用稳态极经曲线测定了     

高效毛细管电泳法手性分离伪麻黄碱

以三甲基-β-环糊精(TM-β-CD)为手性选择剂,用毛细管区带电泳法对手性药物伪麻黄碱进行了分离.系统地考察了不同的手性选择剂及其浓度、缓冲溶液的浓度和pH、分离电压等对分离的影响.结果发现,在Tris-H3PO4(10 mmo1.L-1 Tris,5 mmo1.L-1 H3PO4,PH 2.74)缓冲溶液中,TM-β-CD为15 mmo1.L-1,分离电压18 kV条件下,伪麻黄碱对映体在6 min内获得快速基线分离.由此建立了可靠、快速的分析方法.     

LiCoO_2 electrode/electrolyte interface of Li-ion batteries investigated by electrochemical impedance spectroscopy

The storage behavior and the first delithiation of LiCoO2 electrode in 1 mol/L LiPF6-EC:DMC:DEC elec- trolyte were investigated by electrochemical impedance spectroscopy (EIS). It has found that, along with the increase of storage time, the thickness of SEI film increases, and some organic carbonate lithium compounds are formed due to spontaneous reactions occurring between the LiCoO2 electrode and the electrolyte. When electrode potential is changed from 3.8 to 3.95 V, the reversible breakdown of the resistive SEI film occurs, which is attributed to the reversible dissolution of the SEI film component. With the increase of electrode potential, the thickness of SEI film increases rapidly above 4.2 V, due to overcharge reactions. The inductive loop observed in impedance spectra of the LiCoO2 electrode in Li/LiCoO2 cells is attributed to the formation of a Li1-xCoO2/LiCoO2 concentration cell. Moreover, it has been demonstrated that the lithium-ion insertion-deinsertion in LiCoO2 hosts can be well described by both Langmuir and Frumkin insertion isotherms, and the symmetry factor of charge transfer has been evaluated at 0.5.     

一缩二甘醇酸体系荧光分析法同时测定钆和铽

本文研究了Ｇｄ＾３＾＋，Ｔｂ＾３＾＋与一缩二甘醇酸形成络合物的荧光性能及发光机理，探讨了Ｇｄ＾３＾＋，Ｔｂ＾３＾＋同时测定的最佳条件和共存离子的影响。Ｇｄ＾３＾＋，Ｔｂ＾３＾＋的检测限分别为１６０和３ｎｇ／ｍｌ。并将该法成功地应用于稀土氧化物中Ｇｄ＾３＾＋，Ｔｂ＾３＾＋的测定。     

Characterization of mesoporous nanocrystalline TiO2 photocatalysts synthesized via a sol-solvothermal process at a low temperature

Nanocrystalline TiO₂ samples with mesoporous structure were prepared via a solvothermal treatment of surfactant-stabilized TiO₂ sols. The samples were obtained from media of different acidities including nitric acid, deionized water, and ammonia (denoted as HT-1, HT-2 and HT-3, respectively). These samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), N₂-sorption (BET surface area), micro-Raman spectroscopy, infrared absorption spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). The photocatalytic activities of the samples were tested by the self-photosensitized degradation of an azo dye, Mordant Yellow 10 (MY), in aqueous solution under visible light irradiation. The results reveal that all three samples have high surface area and are pure anatase phase. The sample prepared in nitric acid medium possesses the most ideal mesoporous structure and also exhibits a blue shift in the Raman spectrum. All three samples show much higher photocatalytic activity than the commercial P-25. The activity order of the three samples is HT-1>HT-2>HT-3.     

NITROXIDE-MEDIATED FREE RADICAL SYNTHESIS OF MESOGEN-JACKETED LIQUID CRYSTAL POLYMERS*

The first TEMPO-mediated "living" free radical polymerization of liquid crystallinemonomer, 2, 5-bis[(4-methoxyphenyl)oxycarbonyl]styrene(MPCS), was carried out at 130℃ withBPO as an initiator. The molecular weight of the polymer can be varied from rather low values to highvalues while maintaining narrow polydispersity. It was observed that the polymerization of MPCSproceeded much faster than that of styrene. A tentative explanation for this fast polymerization wassuggested.     

V2O5-MoO3-SiO2表面复合氧化物催化剂的制备与表征

采用表面改性法制备了V2O5-SiO2,MoO3-SiO2,V2O5-MoO3-SiO2复合氧化物催化剂,并用TPR和IR技术研究了催化剂的表面结构及V=O,M0=O的活性,同时用化学吸附IR技术研究了催化剂样品对异丁烷的化学吸附性能.实验结果表明:这些复合氧化物催化剂对异丁烷都有较高的化学吸附能力;SiO2能缓解表面Lewis碱位V=O和Mo=O的氧化能力,有利于选择氧化.     

高富勒烯的提取,分离和分析

采用二硫化碳重结晶富勒烯混合物或二硫化碳二次抽提烟灰以提取高富勒烯（ｈｉｇｈｅｒｆｕｌｅｒｅｎｅｓ，Ｃｎ，ｎ＞７０）。产物经高效液相色谱分析，高富勒烯的含量从１％分别提高到４％和６％；经激光飞行时间质谱证明，产物中除含主要成分Ｃ６０和Ｃ７０以外，还含有Ｃ７６、Ｃ７８、Ｃ８２、Ｃ８４以及更高碳原子的富勒烯。