缓慢炭化部分氧化对制备煤质活性炭的影响

研究了炭化升温速度、炭化低温区引入空气部分氧化对活性炭制备过程中炭化阶段、炭化物结构、活性炭性能等的影响。结果表明，炭化时低温部分氧化可提高炭化物得率，使炭化物微晶的ｄ００２值升高和Ｌｃ值减小；而较慢的炭化升温速度有利于制备优质活性炭。缓慢炭化、部分氧化可以在一定程度上控制炭化路径，使炭化向生成取向性差、难石墨化、各向同性、呒定形炭多的炭化物的方向进行；并讨论了它们控制炭化的作用机理。以此为指导，     

新型2-氧代-1,2,4-三唑并[3,2-d][1,5]苯并氧氮杂类稠杂环的合成

将取代色满酮(1)与芳肼反应生成的腙与HNCO发生[3+2]环加成反应,加成产物(2)经氧化得到偕偶氮异氰酸酯(3).化合物3在HBF4的催化下发生环化-重排反应,得到新颖的三环系2-氧代-1,2,4-三唑并[3,2-d][1,5]苯并氧氮杂化合物5a～5g.     

Effect of ionic additives on the elution of sodium aryl sulfonates in supercritical fluid chromatography

Addition of a small amount of polar solvent (i.e., modifier) to CO2 in packed column supercritical fluid chromatography (SFC) has shown major improvements in both polar analyte solubility and interaction of the polar analyte with the stationary phase. Recently, the addition of an ionic component (i.e., additive) to the primary modifier by one of us has been shown to extend even further the application of SFC to polar analytes. In this work, the effect of various ionic additives on the elution of ionic compounds, such as sodium 4-dodecylbenzene sulfonate and sodium 4-octylbenene sulfonate, has been studied. The additives were lithium acetate, ammonium acetate, tetramethylammonium acetate, tetrabutylammonium acetate, and ammonium chloride dissolved in methanol. Three stationary phases with different degrees of deactivation were considered: conventional cyanopropyl, deltabond cyanopropyl, and bare silica. The effect of additive concentration and additive functionality on analyte retention was investigated. Sodium 4-dodecylbenzene sulfonate was successfully eluted using all the additives with good peak shape under isocratic/isobaric/isothermal conditions. Different additives, however, yielded different retention times and in some cases different peak shapes.     

烯烃的有机催化不对称环氧化反应

介绍了用手性酮，手性亚胺盐为催化剂以及手性胺为催化剂前体的新型有机催化不对称环氧化反应。     

通过密度函数理论表征炭质吸附剂的孔径分布

通过密度函数理论（DFT-DensityFunctionalTheory）对炭质吸附剂的孔径分布进行了表征。该法以多孔固体上N2吸附分子模型为依据，用一种方法对多孔固体的孔径分布从微孔到大孔范围进行确定。本文用该法对自制的聚丙烯腈活性炭纤维、国产煤质活性炭及日本产活性炭微球等六种炭质吸附剂的孔径分布进行了表征。     

Sm2O3对CuO-γ-Al2O3催化剂性能的影响

在色谱微反流动法实验装置上考察了负载Ｓｍ２Ｏ３对ＣｕＯγＡｌ２Ｏ３催化剂ＣＯ氧化活性的影响，并运用Ｘ射线衍射（ＸＲＤ）、程序升温还原（ＴＰＲ）及程序升温脱附（ＴＰＤＭＳ）技术研究了Ｓｍ２Ｏ３对ＣｕＯγＡｌ２Ｏ３催化剂的物相结构、氧化还原特性及表面氧的脱附与恢复行为的影响。结果表明，负载适量的Ｓｍ２Ｏ３对ＣｕＯγＡｌ２Ｏ３催化剂表面氧的脱出与恢复有促进作用，可使部分γＡｌ２Ｏ３相变成γＡｌ２Ｏ３和θＡｌ２Ｏ３的混合型。负载适量的Ｓｍ２Ｏ３能改善催化活性，而负载过量的Ｓｍ２Ｏ３则使ＣｕＯ催化剂上ＣｕＯ的晶粒增大，从而对催化活性起了抑制作用。     

Synthesis and biological activity of novel epothilone aziridines

[reaction: see text]. A series of 12alpha,13alpha-aziridinyl epothilone derivatives were synthesized in an efficient manner from epothilone A. The final semisynthetic route involves a formal double-inversion of stereochemistry at both the C12 and C13 positions. All aziridine analogues were tested for effects on tubulin binding polymerization and cytotoxicity. The results indicate that the aziridine moiety is a viable isosteric replacement for the epoxide in the case of epothilones.     

PREPARATION AND CHARACTERIZATION OF SHISH-KEBAB TYPE LIQUID CRYSTALLINE POLY（p-PHENYLENEVINYLENE）

Novel shish-kebab type liquid crystalline poly（p-phenylenevinylene） derivatives were synthesized by Stille coupling reaction from 2,5-bis[（4-n-alkoxyl）benzoyloxy]1,4-dibromobenzene （monomer l） and 1,2-bis（tributylstannyl） ethylene （monomer 2）. The polymers with alkoxy groups are soluble in common organic solvents and exhibit blue fluorescence. Both the cast film and the annealed film have large red-shifts in fluorescence spectra and show yellow fluorescence. The polymers with CN and NO2 groups show poor solubility and green fluorescence. All the polymers possess liquid crystalline smectic phases. The melting point （Tm） of the polymers decreases when the length of the alkoxy tails of the mesogenic units increases. The polymers are easily aligned under a magnetic field of 10 Tesla. It is found that the conjugated backbone and LC side chain are aligned perpendicular and parallel to the magnetic field, respectively. The polymers show optical dichroism in fluorescence spectra, suggesting that they are available for advance materials with linear optical polarization.     

库仑滴定法测定有机硅样品中的氮含量

本文利用库仑滴定法研究了高分子和低分子硅氮化合物及含氮有机硅样品中氮含量的测定,并研究和讨论了影响测定结果准确性的因素。     

High-yield solvothermal formation of magnetic CoPt alloy nanowires

One-dimensional (1D) magnetic nanomaterials have attracted much attention recently because of their applications in magnetic recording and spintronics. Nevertheless, it remains a challenge to prepare free-standing magnetic nanowires in high yield. This Communication reports the successful high-yield synthesis of an interesting 1D ferromagnetic CoPt alloy by direct decomposition of platinum acetylacetonate and cobalt carbonyl compound in ethylenediamine solvent through a solvothermal reaction. The CoPt alloy nanowires obtained have a tunable diameter of 10-50 nm and a length along the longitudinal axis of up to several microns, depending on crystallization temperature and reaction time. A unique formation mechanism involving coarsening and ripening under solvothermal conditions was discovered. This research opens new opportunities in synthesizing nanomaterials through low-temperature solvothermal processes.