氯化铁催化合成富马酸二甲酯

氯化铁可代替硫酸催化酯化反应，探讨了氯化铁催化合成富马酸二甲酯的条件，操作简便，反应温和，无腐蚀，减少了污染与产品纯化。     

2,6-萘二甲酸二甲酯与一些二甲基萘所形成的激基复合物

2,6-萘二甲酸二甲酯与一些二甲基萘可以形成激基复合物。本文通过稳态和动态荧光光谱研究了这类激基复合物的形成与分子结构的关系。结果表明,尽管这些二甲基萘的电离能基本相同,但因取代基位置不同使分子中电荷分布不同,从而影响了激基复合物的形成能力。     

Preparation,characterization, and adsorption properties for metal ions of a novel chelating resin containing sulfoxide and diethylene glycol

A novel chelating resin containing sulfoxide and diethylene glycol, poly{4‐vinylbenzyl‐[2‐2‐(hydroxyethyl)ethoxyl]sulfoxide} (PVESO) was synthesized using chloromethylated polystyrene (PS‐Cl) as material. Its structure was characterized by elemental analysis, infrared spectra, and scanning electron microscopy (SEM). The adsorption capacities of the resin for Hg²⁺, Ag⁺, Cu²⁺, Zn²⁺, and Pb²⁺ at various pH values were determined. The maximum adsorption capacities for Hg²⁺ and Ag⁺ were 1.56 and 0.75 mmol g^?1 respectively. The resin had high selectivity for Hg²⁺ and Ag⁺ over the pH range 1.0–7.0. The adsorption capacities for Hg²⁺ and Ag⁺ under competitive condition were also determined by batch experiment method. In addition, the adsorption kinetics of the resin towards Hg²⁺ at different temperatures was also investigated. The results showed that the adsorption rate was governed by film diffusion at 20°C and 25°C, by particle diffusion at 30°C and 35°C. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 6054–6059, 2006     

Crystalline complex between poly(γ-methyl l-glutamate) and dimethyl phthalate

The crystalline complex between poly(γ-methyl l-glutamate) (PMLG) and dimethyl phthalate (DMP) has been formed in films cast from a solution in dichloroethane. It has the stoichiometry of 1 mol of DMP to three or four residues of PMLG and shows two definite characteristics in X-ray diffraction patterns; one is the large hexagonal unit cell with the edge of around 28 Å and another the ‘extra’ 5.07 Å meridional reflection which can not be interpreted by a PMLG α-helical conformation. The structural examination for the films with various DMP contents is carried out by X-ray, viscoelastic, and d.s.c. measurements and the following structure is proposed for the crystalline complex. Four PMLG are associated to form a group which is hexagonally packed and DMP molecules, located in the gaps between groups, form a specific favourable helical structure along PMLG chains in which the van der Waals stacking of benzene rings of DMP is significant.     

Selective O-methylation of phenol with dimethyl carbonate over X-zeolites

The O-methylation of phenol with dimethyl carbonate proceeds selectively in the vapor phase over alkali ion exchanged X-zeolites. Thus, a 76% yield of anisole was obtained with a 93% selectivity over NaX at 553 K. The participation of basic sites in the O-methylation is suggested.     

Influences of zinc oxide and an organic additive on the electrochemical behavior of pure aluminum in an alkaline solution

The corrosion behavior of pure aluminum in inhibited and uninhibited 4 MKOH was investigated by means of hydrogen collection, polarization curve measurement and electrochemical impedance spectroscopy (EIS). The results showed that the corrosion of pure aluminum was greatly inhibited by the addition of ZnO and dimethyl amine epoxy propane (designated as DE). EIS and EDAX analyses revealed that ZnO produces its effect by depositing on the aluminum surface, which increases the overpotential of hydrogen evolution. It was also found that the addition of DE could greatly improve the deposition of zinc layers.     

对叔丁基苄胺的合成研究

摘要选择Delepine反应法的路线合成对叔丁基苄胺，并对反应投料比、反应温度及酸化后的反应时间进行了优化试验，得到了较好的反应条件：反应温度为40℃，对叔丁基苄氯与乌洛托品投料比为1：1；加入酸和醇后的保温时间为2h，从而使反应收率稳定在90％以上，含量达到95％。     

Thermodynamic studies on the complete phase diagram of aqueous two phase system containing polyethylene glycol dimethyl ether 2000 and di-potassium hydrogen phosphate at different temperatures

The liquid-liquid equilibrium of polyethylene glycol dimethyl ether 2000 (PEGDME₂₀₀₀)+K₂HPO₄+H₂O system has been determined experimentally at T=(298.15,303.15,308.15 and 318.15) K. The liquid-solid and complete phase diagram of this system was also obtained at T=(298.15 and 308.15) K. A nonlinear temperature dependent equation was successfully used for the correlation of the experimental binodal data. Furthermore, a temperature dependent Setschenow-type equation was successfully used for the correlation of the tie-lines of the studied system. Moreover, the effect of temperature on the binodal curves and the tie-lines for the investigated aqueous two-phase system have been studied. Also, the free energies of cloud points for this system and some previously studied systems containing PEGDME₂₀₀₀ were calculated from which it was concluded that the increase of the entropy is the driving force for formation of aqueous two-phase systems. Additionally, the calculated free energies for phase separation of the studied systems were used to investigate the salting-out ability of the salts having different anions. Furthermore, the complete phase diagram of the investigated system was compared with the corresponding phase diagrams of previously studied systems, in which the PEGDME₂₀₀₀ has been used, in order to obtain some information regarding the phase behavior of these PEGDME₂₀₀₀+salt+water systems.     

Ti(OC4H9)4-PbO均相催化反应蒸馏合成碳酸二苯酯

通过对碳酸二甲酯与苯酚酯交换法反应蒸馏合成碳酸二苯酯的研究,筛选合适的催化剂和寻找最佳的工艺条件,为将来碳酸二苯酯的工业化打下基础.实验结果表明在常压下,温度132℃,原料中苯酚与碳酸二甲酯的摩尔配比为21,苯酚与催化剂的摩尔配比为10.012,钛酸四丁酯与氧化铅的摩尔配比为11,反应时间12 h,碳酸二甲酯总转化率为45.43%,碳酸二苯酯产率为26.33%,碳酸苯甲酯产率为19.10%,碳酸二苯酯的选择性为57.96%,且无苯甲醚和CO2生成.所选催化剂Ti(OC4H2)4-PbO的催化性能明显优于二丁基二月桂酸锡和PbO.     

A preparation method for observing intracellular structures by scanning electron microscopy

In order to observe intracellular structures by scanning electron microscopy, excess cytoplasmic matrix must be removed from the fractured surface of cells. Previously we reported an Osmium-DMSO-Osmium method devised for this purpose. This method is very effective in revealing intracellular structures, but requires osmium tetroxide for initial fixation with some consequent disadvantages. In the present study, a revised Osmium-DMSO-Osmium method is reported, in which an aldehyde mixture is used as the initial fixative instead of osmium tetroxide. As fixation is carried out by perfusion in this revised method, better preservation of fine structures is achieved than by the original method, especially in the central nervous tissue which tends to suffer from post-mortem degeneration. Moreover this method can be applied to cytochemical studies of intracellular structures with a scanning electron microscope (SEM). In this study, acid phosphatase of lysosomes is demonstrated in a coloured SEM micrograph.