铁-钼/活性炭催化剂的费-托合成反应性能

用微型固定床反应器和原位穆斯堡尔谱考察了在活性炭担载的铁-钼双金属催化剂上的费-托合成反应和在反应条件下的物相。已知在费-托合成中铁有利于生成长链烃,钼有利于生成低碳烃。铁-钼/活性炭催化剂则综合了铁和钼的性质,其中铁-钼/油棕炭催化剂具有很好的活性和液化石油气选择性。在反应中,富钼催化剂的主要物相为铁-钼碳化物,而富铁催化剂的物相则为铁-钼碳化物和e’-Fe_2·2C碳化铁。     

Synthesis and herbicidal activities of methyl-1-(2,4-dichlorophenoxyacetoxy)alkylphosphonate monosalts

A series of 1-(2,4-dichlorophenoxyacetoxy)alkylphosphonic acid dimethyl esters 5 and its corresponding phosphonate monosalts 6 were synthesized as potential herbicide. The phosphonate monosalts can be prepared from 1-(2,4-dichlorophenoxyacetoxy)alkylphosphonic acid dimethyl esters 5, which were synthesized by the condensation of O,O-dimethyl-1-hydroxyalkylphosphonates with dichlorophenoxyacetic chloride. This method provides a simple and efficient procedure for the synthesis of phosphonate derivatives containing sensitive groups to acid, base or water such as carboxylate ester bond; and the herbicidal activity of title compounds was evaluated in a set of experiments in greenhouse. Most of the compounds exhibited notable herbicidal activity.     

Synthesis, Crystal Structure and Inhibition of the K562 Cell Proliferation of N＇-Tertbutylaminocarbonyl-N-2-chlorophenoxyacetylthiourea

The title compound N'-tert-butylaminocarbonyl-N-2-chlorophenoxyacetylthiou- rea has been synthesized for the first time. Complete assignments were achieved by IR, 1H NHR and single-crystal X-ray diffraction analyses. The inhibitory rate of the cellular growth of K562 cells (chronic myeloid 1eukemic cells) was measured using MTT [3-(4,5-dimethylthiazo-2-y1)-2,5-di- phenyltetra-zolium bromide] assay. The cell apoptosis was assessed by agarose gel electrophoresis to find that the title compound has antiproliferation and apoptosis inducing effects on K562 cells. In order to investigate the relationship between structure and activity of the target compound, we report its crystal structure and biological behavior in the present paper. Crystallographic data: C14H18- ClN3O3S, Mr = 343.82, orthorhombic, space group Pnma, a = 19.786(6), b = 6.789(2), c = 12.938(4) , V = 1738.0(9) 3, Z = 4, Dc = 1.314 g/cm3, F(000) = 720, μ(MoKα) = 0.354 mm-1, R = 0.0378 and wR = 0.0941. The molecule is a planar structure.     

Mixed Cationic‐nonionic Surfactants and pH Adjustment Route to Synthesize High‐quality MCM‐48

Using the mixture of cetyltrimethylammonium bromide (CTAB) and p‐Octyl polyethylene glycol phenyl ether (OP‐10) as templates, siliceous MCM‐48 materials can be synthesized with low molar ratio of CTAB to silica (0.139:1) and low concentration of mixed surfactants (ca.5%) and within a wide range of OP‐10/CTAB ratio (0.08?0.25). The materials were characterized by X‐ray powder diffraction, N₂ adsorption/desorption isotherm, TEM, TG‐DSC and ²⁹Si MAS NMR. Measurements indicated that the use of mixed surfactants allowed better condensation and higher ordering of the cubic mesostructure; at the same time, some properties of these materials were sensitive to the OP‐10/CTAB ratio. It was also found that the reduced pH of the gel which had been crystallized for a certain time gave a highly reproducible synthesis with a high silica yield (about 95%). Furthermore, the reaction mechanism of the synthesis is discussed in detail.     

Synthesis of New Chiral C2-Symmetrical Bis(oxazoline )Compounds

New chiral C2-symmetrical bis(oxazoline)compounds bearing one isobutyl-,secbutyl-benzyl- or isopropyl-substituent at the 4-position have been prepared and characterized.     

Synthesis and Characterization of a [Mn12O12(O2CR)16(H2O)4] Complex Bearing Paramagnetic Carboxylate Ligands. Use of a Modified Acid Replacement Synthetic Approach

Summary.  A new modified approach for the synthesis of Mn₁₂ clusters, based on the use of complex [Mn₁₂O₁₂(O₂C ^t Bu)₁₆(H₂O)₄] (2) as starting material to promote the acidic ligand replacement, is presented here. This new synthetic approach allowed us to obtain complex [Mn₁₂O₁₂(O₂CC₆H₄N(O^•) ^t Bu)₁₆(H₂O)₄] (3), whose preparation remained elusive by direct replacement of the acetate groups of Mn₁₂Ac (1). Complex 3 bearing open-shell radical units, was prepared to increase the total spin number of its ground state, and consequently, to increase T _B , with the expectation that the radical ligands may couple ferromagnetically with the Mn₁₂ core. Unfortunately, magnetic measurements of complex 3 revealed that the sixteen radical carboxylate ligands interact antiferromagnetically with the Mn₁₂ core to yield a S = 2 magnetic ground state. Corresponding author. E-mail: vecianaj@icmab.es Received March 27, 2002; accepted May 2, 2002     

几种杂多阴离子柱撑水滑石的合成与吸附行为

柱撑水滑石类层柱状阴离子粘土是一类新型层柱材料，由于其二维孔道结构的可调变性及潜在的择形催化性能，已引起人们的重视[1-3]．迄今，人们已合成了包括无机和有机阴离子，同多和杂多阴离子（Polyoxometalates，简称POMs）以及配合物阴离子在内的多种柱撑水滑石，其中同多和     

A new anode material LiMoS2 for use in rechargeable Lithium Ion Batteries

The novel applications of molybdenum disulfide in recent research were reviewed, such as in lubricant, catalyst and photoelectrochemical solar cells. Recently, we found that LiMoS2 is a good candidate for new anode materials for lithium ion batteries with high lithium storage capacity.Here, the anode material LiMoS2 was synthesized by a hydrothermal method at 150℃ and the electrochemical characterization as an anode material for lithium ion batteries was examined.put in Teflon-lined stainless steel autoclaves of capacity 40 mL. Distilled water was used to fill the autoclaves to 70 % of the total volume. The autoclaves were maintained at 150℃ for 24 h and then cooled naturally. The resulting dark-gray powders were filled and washed with distilled water,diluted hydrochloric acid and ethanol, successively. The final products were dried at 80℃ for 24 h.The powder X-ray diffraction pattern showed the prepared LiMoS2 was amorphous structure. A test cell using LiMoS2 as the active material was discharged and charged between 3 and 0.01 V with respect to Li metal at a constant current density of C/5 (that is, one lithium per formula unit in 5 hours). During the first discharge, the potential rapidly drops to reach a large plateau at 2.2 V, then slowly drops to the other plateau at 0.8 V, and then continuously decreases down to 0.01V. There is only a plateau at 1.35 V in the subsequent discharge curves. The plateaus of charge potential appear at about 1.9 V.The irreversible loss was 41% in the first cycle. The ratio of discharge and charge is more than 99%in the subsequent cycles. Moreover, the ratio of discharge and charge almost reaches 100% after thedemonstrated that LiMoS2 has a very high capacity and a good cycle-ability as an anode material forlithium ion batteries.     

含硅二硫代磷酸酯的合成及生物活性

硅基甲硫醇Ｒ＾１Ｒ＾２ＣＨ３ＳｉＣＨ２ＳＨ与Ｏ，Ｏ－二烷基二硫代磷酸酯（ＲＯ）２Ｐ（Ｓ）ＳＨ及甲醛可顺利地发生类Ｍａｎｎｉｃｈ缩合反应，利用此反应和硅基甲硫醇与Ｏ，Ｏ－二乙基－Ｓ（２－溴乙基）二硫代磷酸酯的取代反应合成了３７种新的含硅二硫代到酯化合物（ＲＯ）２Ｐ（Ｓ）Ｓ（ＣＨ２）ｎＳＣＨ２ＳｉＣＨ３Ｒ＾１Ｒ＾２（ｎ＝１，２），在初筛浓度下，该类化合物具有一定的杀虫，杀螨活性。     

Molten salt synthesis (MSS) of Cu2Mo6S8—New way for large-scale production of Chevrel phases

The Chevrel phase (CP), Mo₆S₈, was found to be an excellent cathode material for rechargeable magnesium batteries. Mo₆S₈ is obtained by a leaching process of Cu₂Mo₆S₈, which removes the copper. A new method of Cu₂Mo₆S₈ production was developed. In contrast to the well-known solid-state synthesis of CP, the method is based on the reaction in a molten salt media (KCl). A fast kinetics of this reaction allows using less active, but more convenient precursors (sulfides instead of sulfur), decreasing temperature and synthesis duration, as well as operation in the inert atmosphere instead of dynamic evacuated systems. It was shown that the composition and the electrochemical behavior of the products obtained by MSS and by the solid-state synthesis are identical. Thus, the molten salt method is extremely attractive for the large-scale production of the active materials for Mg batteries.