微波辐射法合成α-萘甲醚的研究

用微波辐射法合成α－萘甲醚，考察了不同条件对产率的影响，此法反应时间短，产率可达75％。     

Efficient combination of task-specific ionic liquid and microwave dielectric heating applied to one-pot three component synthesis of a small library of 4-thiazolidinones

The first report of the use of task-specific ionic liquid as synthetic equivalent of ionic liquid-phase matrice for the preparation of a small library of 4-thiazolidinones is reported in this paper. The starting (ethyleneglycol)ionic liquid-phase is functionalized in good yields with 4-(formylphenoxy)butyric acid by using usual esterification reaction conditions (DCC/DMAP as catalyst). The synthesis of the ionic liquid-phase bound 4-thiazolidinones was performed by a one-pot three-component condensation under microwave dielectric heating. The final cleavage under microwave/catalysis strategy provides the expected 4-thiazolidinones in high purity after flash-chromatography purification. According to the ionic liquid-phase organic synthesis (IoLiPOS) methodology, it was found that optimized reaction conditions were performed by standard analytical methods (NMR, TLC). The ¹H, ¹³C NMR spectrum of some representative 4-thiazolidinones and ionic liquid-phase bound benzaldehyde are also reported.     

微波辐照增强原煤磁分离脱硫机理探讨

采用~(57)Fe穆斯堡尔谱学方法,研究微波-磁分离法脱硫机理及微波辐照深度对脱硫率的影响。结果表明,微波选择性介质加热,可以激励煤中顺磁性黄铁矿FeS_2热解,使其转化为非化学计量的磁黄铁矿Fe_(1-x)S(0相似文献   

A kinetic study of methane conversion by a dinitrogen microwave plasma

Conversion of CH₄ with a N₂ microwave plasma (2.45 GHz) is studied. The experiments cover the absorbed microwave power range 300–700 W with 17–62% of methane in the gas mixture, with pressures of 10–40 mbar and flow rates of 140–650 ml· min^–1. The yields of C₂ hydrocarbons and dihydrogen are analyzed by gas chromatography. The distance of methane addition downstream of the plasma plays an important role on the composition and the concentration of the products obtained. This distance mainly determines the energy concentrated in the active species of the plasma when they react with methane. Different behaviors for acetylene formation, on the one hand, and for ethane and ethene formation, on the other hand, have been observed, and this finding allows us to propose a kinetic mechanism for the decay of methane and for the formation of C₂ hydrocarbons.     

制备纳米氧化锌的新方法

以草酸和醋酸锌为原料，用室温固相化学反应首先制备前驱物二水合草酸锌，后者在微波场辐射分解得到产物纳米氧化锌。用XRD，TEM和IR等技术对产物的组成，大小及形貌进行了表征。结果表明：产物纳米氧化锌为粒度分布均匀的球形六角晶系结构，平均粒径约为8nm。     

噻吩及衍生物的微波反应机理研究

应用量子化学理论，初步探讨了苯－噻吩协同分离的可能性，利用微波诱导反应提高了选择性，介绍了在复合催化作用下，对Ｄｉｅｌｓ－Ａｌｄｅｒ，ａｃｙｌａｃｙｌａｔｉｏｎ，ＨｙｄｒｏｇｅｎＥｘｃｈａｎｇｅ几个基元反应的机理。     

Hydrophilic Treatment of the Dyed Nylon-6 Fabric using High-density and Extensible Antenna-coupling Microwave Plasma System

High density and well surface-distributed oxygen microwave plasma with an extensible antenna-coupling design was utilized to modify a densely weaved and large-surface-area Nylon-6 fabric within a short treatment time. Plasma pretreatment and subsequent acrylic acid (AAc) or 2-hydroxyethyl methacrylate (HEMA) grafting process were studied and optimized at the stage after dyed and finished procedure. The monomer-grafted dyed Nylon-6 fabrics evolved lasting hydrophilic properties and thereafter created or improved surface properties such as water diffusion, drainage, moisture regain and water absorbency, in different degrees. The pHEMA-grafted sample exhibited minor effect in color perception, which was also much hydrophilic than the pAAc-grafted one. Based upon surface analyses and wetting assessment, the penetration of HEMA monomer into the plasma-treated fabric matrix contributed to the facilitation of wetting properties. This work accordingly ensures such plasma-induced system to incorporate with the pattern of hydrophilic properties on the analogous textiles without interrupting their finishing process.     

Simple Method for Simultaneous Determination of Selenium and Arsenic in Human Hair by Means of Atomic Fluorescence Spectrometry with Hydride Generation Technique

This study describes a simple, rapid and reliable method for simultaneous determination of selenium and arsenic in human hair by means of atomic fluorescence spectrometry combined with a hydride generation technique (HG-AFS). The procedure developed encompasses microwave digestion of a sample in the nitric acid environment only. The interferences caused by nitrous oxides are eliminated by removing a gas from above the digested solution with a stream of argon. The sample is then chemically treated in a flow-through hydride generation system and exposed to measurements in a double-channel atomic fluorescence spectrometer. The method permits determining both analytes in the linear range of 0.5–100µgL^–1 with a detection limit equal to 0.2µgL^–1, as well as with very good repeatability not exceeding 1% for Se and 2% for As. No mutual interferences from either of the analytes in the concentrations ranges matching the hair composition were found. The method was verified in terms of accuracy with the use of a reference material and then applied to the analysis of the natural samples of human hair.     

Comparison of Pyrolysis and Microwave Acid Digestion Techniques for the Determination of Mercury in Biological and Environmental Materials

 Microwave digestion reduction-aeration and pyrolysis combined with cold vapour atomic absorption and cold vapour atomic fluorescence are compared for the determination of total mercury in several biological and environmental matrices. The biological samples were digested in a mixture of HNO₃/H₂O₂, the environmental samples in a mixture of HNO₃/HClO₄. After reduction with SnCl₂, the mercury was collected by two-stage gold amalgamation. After microwave digestion reduction-aeration, detection limits of 1.4 ng g⁻¹ and 0.6 ng g⁻¹ were obtained for cold vapour atomic absorption spectrometry (CVAAS) and cold vapour atomic fluorescence spectrometry (CVAFS), respectively, for 250 mg of environmental samples. For biological samples (500 mg) the detection limits were 0.7 ng g⁻¹ (CVAAS) and 0.4 ng g⁻¹ (CVAFS). After pyrolysis, detection limits of 3.5 ng g⁻¹ and 1.6 ng g⁻¹ for CVAAS and CVAFS, respectively, were obtained for a 10 mg sample. Pyrolysis can only be applied when the organic content of the sample is not too high. Accurate results were obtained for 8 certified reference materials of both environmental and biological origin. In addition, a real sludge sample was analysed. Author for correspondence. E-mail: richard.dams@rug.ac.be Received September 18, 2002; accepted December 3, 2002 Published online May 5, 2003