化学键合吸附剂的合成及吸附行为

在无定型硅胶上化学键合十八烷基三氯硅烷，键合率17%-20％，粒度5μm-10μm，以此键合的吸附剂可有效地吸附香烟烟气中的焦油、亚硝胺，吸附率分别为15%-18％和37%-43％，研究了化学键合吸附剂的粒度和加入量对吸附性能的影响。     

Determination of panaxadiol and panaxatriol in ginseng and its preparations by capillary supercritical fluid chromatography (SFC).

Capillary supercritical fluid chromatographic (SFC) method has been developed for the determination of panaxadiol and panaxatriol in ginseng and its preparations. 0.1 g ginseng or an appropriate amount of its preparations was hydrolysed by 15% H2SO4 in an ethanol:water (1:1 v/v) solution for 4 h followed by 15% NaOH for 0.5 h. The mixture was extracted by cyclohexane. The cyclohexane extracts were purified by a partition column and concentrated by an adsorption column and then analysed by SFC. Methyltestosterone was used as the internal standard.     

超高交联吸附树脂吸附对硝基苯乙酮的热力学研究

比较两种超高交联聚苯乙烯吸附树脂NJ-8、AM-1与Amberlite XAD-4(以下简称XAD-4)对对硝基苯乙酮的静态吸附行为，根据吸附等温线研究了吸附热力学性质．在298～318K和研究的浓度范围内，NJ-8，AM-1、XAD-4对对硝基苯乙酮的吸附平衡数据符合Freundlich吸附等温方程．结果表明：吸附为放热过程，适当降低温度有利于吸附．计算了对硝基苯乙酮在NJ-8，AM-1、XAD-4树脂上的吸附焓变、自由能变，吸附熵变．对吸附行为作了合理的解释。     

双核银络合物[Ag_2(dppm)_2(Py)_2(μ-Cl)]ClO_4的合成与结构

二-(二苯基膦)甲烷(dppm)是一种易与金属形成多核络合物的有机膦配体。我们用dppm作为配体合成了一系列银的多核络合物,并对其结构进行了研究。本文报导了其中一个双核化合物[Ag_2(dppm)_2(Py)_2(μ-Cl)]ClO_4的合成及晶体结构、分子结构的测定。     

Hydrothermal synthesis and crystal structure of a layered vanadium oxide with an interlayer metal coordination complex: [Co(phen)3][V10O26]·H2O

A novel compound, [Co(phen)₃][V₁₀O₂₆]·H₂O, was hydrothermally synthesized and characterized by single-crystal X-ray diffraction. This compound crystallizes in the orthorhombic space group Ccca with a=13.447(3), b=29.936(6), c=23.252(5) Å, V=9360(3) Å³, Z=8 and R=0.0285. Data were collected on a Rigaku R-AXIS RAPID IP diffractometer at 293 K in the range of 1.36<θ<24.99°. The structure of the compound consists of vanadium oxide layers, which are built up from the infinite VO₄ chains by corners and edges sharing. The [Co(phen)₃]²⁺ complexes occupy the interlayer space and contact each other via π−π stacking interactions of the phen groups to form infinite one-dimensional chains.     

富烯碳原子簇的石墨层间闭合形成机理

本文提出了富烯碳原子簇的石墨层间闭合形成机理，由该机理推出的许多结果与实验事实符合很好。我们认为碳原子簇自由基的快速淬灭及其淬灭速度是富烯碳原子簇形成及其丰度的决定因素。由此得出富烯碳原子簇在给定实验条件下产生的必然性，并预言不同大小的富烯碳原子簇可以通过优化实验条件选择性地合成。     

Syntheses of seven-membered rings: ruthenium-catalyzed intramolecular [5+2] cycloadditions

The Ru-catalyzed intramolecular [5+2] cycloaddition of cyclopropylenynes is investigated with respect to the regio- and diastereoselectivity as well as the functional group compatibility of the reaction. Evidence for the mechanism as occurring through a ruthenacyclopentene intermediate is elucidated from 1) the study of the diastereoselectivity of the cycloaddition; 2) the effect of variation of substituents on the regioselectivity of cyclopropyl bond cleavage in 1,2-trans- and 1,2-cis-disubstituted cyclopropanes and 3) examples that clearly do not involve ruthenacyclohexene as intermediates as products still incorporate the cyclopropyl moiety. The scope and limitations of the Ru-catalyzed cycloaddition are discussed and compared with the Rh-catalyzed reaction. The potential power of this methodology towards natural product total synthesis is demonstrated by the formation of several polycyclic systems with the chosen reaction conditions and readily available cyclopropylenyne substrates.     

后交联型St-DVB大孔吸附树脂对低级醇类的吸附性能研究

分别在静态和动态条件下研究了Friedel—Crafs后交联型聚苯乙烯-二乙烯基苯(St-DVB)大孔吸附树脂对水溶液中多种低级一元醇的吸附性能，测定静态吸附等温线和动态吸附曲线，并分别按照Langmuir和Freundlich模型进行拟合．结果显示，树脂对水中低浓度低级一元醇的吸附过程属于放热的物理吸附过程，树脂吸附能力随着一元醇碳原子数的增加，即分子内疏水基团质量的增加而增加；树脂对直链醇的吸附能力稍强于同分异构的支链醇．     

Oxorhenium(V) dithiolates catalyze the oxidation by tert-butyl hydroperoxide of sulfoxides and sulfides, including 4,6-dimethyldibenzothiophene

tert-Butyl hydroperoxide (TBHP) efficiently converts a wide variety of sulfides to sulfoxides and sulfones. The method offers the advantage that one product or the other can be obtained in high purity by a modest variation of conditions. The reactions occur smoothly at 25minus sign50 C in chloroform and, to the extent studied, in toluene and methylene chloride. A catalyst is required; the most extensively studied was MeReO(mtp)PPh(3), 1, where mtpH(2) is 2-(mercaptomethyl)thiophenol. Other chelating dithiolate ligands can be used with comparable results. These oxidations were tested for dialkyl, alkylminus signaryl, and diaryl sulfides; thiophenes; and thianthrene. Even the "hard" sulfide, 4,6-dimethyldibenzothiophene (DMDBT) was quantitatively oxidized to the dioxide with TBHP:DMDBT 3.0-3.5 and 0.05-3.8 mol % 1. The mechanism was explored in kinetics studies carried out only for methyl tolyl sulfide. The product buildup curve was complex, with an induction period followed by a rapid growth phase. The kinetic data could be modeled adequately but not perfectly by allowing five rate constants to refine. Their values are consistent with the chemical sense of the mechanism.