Preparation of 1,1,1,3,3-pentafluoropropane (HFC-245fa) by using a SbF5-attached catalyst

In this report, a simple process for preparing HFC-245fa through the reaction of 1,1,1,3,3-pentachloropropane (PCP) and anhydrous HF via two-step vapor-phase catalytic fluorination is described. The antimony pentafluoride catalyst was supported on inert porous materials to improve the catalytic activity. The resulting process catalyst not only exhibited high catalytic activity and excellent thermo-stability, but also improved the performance of SbF₅, in terms of hygroscopicity and corrosion.     

AN INVESTIGATION ON THE ab initio CALCULATION OF INTERMOLECULAR INTERACTION——NON-BONDED INTERACTION IN THE HYDROGEN BOND COMPLEX (HF)_2

An ab initio calculation of the hydrogen bond complex (HF)_2 is given with the 6-311 G~(**) basis set, according to which the potential surface around the balance point of the distancès and the orientations between two HF molecules is obtained. The atomic charges in the system are calculated with the PD/LSF method (potential-derived/least-square-fitting method) and then an analysis of the hydrogen bond interaction between two HF molecules is given with the (exp-6-1) potential function, by means of which it is shown that the main interaction between them is not an electro-static but a charge transfer one. The potential curve between two HF molecules is like a Morse function.     

丝网印刷普鲁士蓝修饰电极催化还原测定过氧化氢

制备了普鲁士蓝修饰的丝网印刷过氧化氢传感器,研究了过氧化氢在该修饰电极上的电催化还原特性,考察了有关修饰膜制备和试验条件对传感器性能的影响。结果表明,pH4.0的0.2mol·L-1KH2PO4 K2HPO4缓冲溶液(PBS)中,修饰电极对过氧化氢显示出快速的电化学响应,较高的稳定性、重现性和催化活性,测定的线性范围为1.0×10-5～1.0×10-3mol·L-1,相关系数为0.999,检出限为6.0×10-6mol·L-1(3σ)。电极制作方法简便,可用于实际样品的测定。     

The initial oxidation of magnesium: an in situ study with XPS,HERDA and ellipsometry

The initial oxidation of magnesium at oxygen partial pressures between 1.3 × 10^?8 and 1.3 × 10^?5 Pa and at temperatures ranging from 273 to 550 K has been investigated in situ with X‐ray photoelectron spectroscopy (XPS), ellipsometry and high resolution elastic recoil detection analysis (HERDA). Quantitative analysis of the XPS spectra showed a clear oxygen deficiency with respect to MgO for the initial oxide. HERDA measurements confirmed this relatively low oxygen content in the thin oxide layers formed. Ellipsometry measurements showed that the electronic structure of the initially formed oxide differs significantly from that of bulk MgO. The band gap values at room temperature for the oxide layers investigated are clearly smaller than the value for bulk MgO. Copyright © 2006 John Wiley & Sons, Ltd.     

Effects of <Emphasis Type="Italic">L</Emphasis>-Carnitine on Sucrose-Induced Hyperlipidaemia

Summary. L-Carnitine, L-(−)-β-hydroxy-γ-trimethylaminobutyrate, plays an important role as a factor necessary for the transport of long-chain fatty acids into the mitochondria. In order to investigate the influence of L-carnitine on hyperlipidaemias, the experimental model of the sucrose-induced hypertriglyceridaemia of the rat was used. In these experiments L-carnitine in the dose of 11 mg per day and 100 g body weight (over the period of 1 week) was able to antagonize the sucrose-induced hypertriglyceridaemia and the increase of serum free fatty acid level in female rats of the Wistar strain. Carnitine administration did not change the activities of lipogenic enzymes and fatty acid synthesis in the liver. However, L-carnitine increases the rate of hepatic fatty acid oxidation. Our results indicate a hypotriglyceridemic and free fatty acid lowering effect of L-carnitine, and suggest the use of this compound in the therapy of hyperlipidaemias.     

N,N-二甲基甲酰胺中电沉积制备镁镍储氢合金

采用恒电位沉积法, 选用适宜的添加剂和络合剂, 成功地从N,N-二甲基甲酰胺(DMF)中沉积出致密的黑色Mg-Ni储氢合金膜. 并初步探讨了其共沉积机理. XRD显示沉积层中含有非晶态Mg-Ni相和微晶态Mg相. SEM图及相应能谱图分析表明合金颗粒以团聚状态存在, 合金成分不是很均匀. AAS分析表明沉积合金中Mg的原子摩尔分数达27.3%. LAND电池测试系统测得所镀合金膜的放电比容量最高为172.4 mAh/g.     

K对Mn—Co—O的结构及氧化活性的影响

利用XRD,TPD,TFD-MS及催化氧化反应等实验技术,研究了K对Mn-Co-O的结构及氧化活性的影响。XRD结果表明,Mn-Co-O系已形成反尖晶石型的MnCo_2O_4结构;K-Mn-Co-O系中除MnCo_2O_4型结构外,还有新相KMnO_2存在。根据O_2的TPD-MS及吡啶的TPD结果,Mn-Co-O中添加适量的K能提高供氧活性和增加供氧数目,但酸中心数目减少,强度降低。K对Mn-Co—O催化剂氧化活性的影响随反应物分子结构的不同而异,对乙酸乙脂、苯甲酰氯等极性有机物的完全氧化反应,K能提高氧化活性,但对苯、正己烷等非极性有机物的完全氧化反应,K使其活性降低。     

Voltammetry in Undiluted Acetic Acid. In Situ Determination of Water

Water present in undiluted acetic acid can be monitored in situ with Pt and Au microelectrodes using differential pulse and square‐wave voltammetries. Both reduction and oxidation peaks can be obtained. The best quantitative analytical results were obtained for the anodic peak, the Pt microelectrode, and differential pulse voltammetry. The anodic water peak is located at +1.55 V vs. the quasi reference Pt electrode. The voltammetric peak obtained at Pt electrode is apparently not a diffusional one, however, the calibration plot obtained by employing this peak is linear over a wide concentration range, up to 4 mol dm^?3. The detection limit has been estimated as 2.3 mM or 0.0043 v/v%. The developed method may be particularly useful, since the Karl Fischer method can not be used to determine water in glacial acetic acid due to the estrification reaction of acetic acid with methanol. A voltammetric wave of undiluted acetic acid could not be obtained in the positive and negative ranges of potential.     

Electroless preparation and electrochemical behavior of a platinum-doped nickel hexacyanoferrate film–zinc modified electrode: catalytic ability of the electrode for electrooxidation of methanol

The use of a zinc substrate as an electrode and the modification of its surface by means of a thin film of platinum-doped nickel hexacyanoferrate (Pt-NiHCF) were developed. The modification conditions of the zinc surface including the electroless deposition of metallic nickel on the electrode surface from NiCl₂ solution, chemical derivatization of the deposited nickel to the NiHCF film in 0.5 M K₃[Fe(CN)₆] solution, and electrochemical penetration of metallic platinum into the modified film are described. The modified zinc electrodes prepared under optimum conditions show a well-defined redox couple due to the [Ni^IIFe^III/II(CN)₆]^1–/2– system. The effects of pH, the alkali metal cation, and the anion of the supporting electrolyte on the electrochemical characteristics of the modified electrode were studied in detail. The diffusion coefficients of hydrated alkali metal cations in the film (D), the transfer coefficient (), and the transfer rate constant for the electron (k_s) were calculated in the presence of some alkali metal cations. The electrocatalytic activity of the modified electrode for methanol oxidation was demonstrated. The stability of the modified electrode under various experimental conditions was investigated.     

Reactions of 1,2,4-Triazines with Nucleophiles. 6. Use of SNH Methodology for the Direct Introduction of Cyclic Diketone Residue into the 1,2,4-Triazine Ring FORENAME = D. N.

3-R-6-Phenyl-1,2,4-triazine 4-oxides react with cyclic -diketones (dimethylbarbituric acid, dimedone, and indan) in both acidic (substrate activation) and basic conditions (nucleophile activation) with formation of ^H-adducts, intermediates in the nucleophilic substitution of hydrogen (S_N ^H) in 3-R-5-Nu-4-hydroxy-6-phenyl-4,5-dihydro-1,2,4-triazines. Oxidative aromatisation of these intermediates or auto-aromatisation of acylated (benzoyl chloride) at the NOH -adducts with elimination of benzoic acid gave the corresponding substituted 1,2,4-triazine 4-oxides or 1,2,4-triazines.