从假性紫罗兰酮合成β-紫罗兰酮中主要副产物(I)的分离鉴定

假性紫罗兰酮在浓硫酸及 - 2 0°C低温条件下反应 ,主要生成 β-紫罗兰酮 ,少量的 α-及 γ-紫罗兰酮 ,同时生成副产物 ( I)及 ( II)。用 IR、1H NMR及 MS光谱分析方法 ,对副产物 ( I)进行了结构鉴定 ,结构为 3,4,4a,5 ,8,8a-六氢 - 2 ,5 ,5 ,8a-四甲基 - 2 H - 1 -苯并吡喃     

浅述毒死蜱的合成

介绍了毒死蜱及其中间体三氯吡啶酚合成路线及方法,并对其合成路线进行简单述评。     

Investigation of bio-ethanol steam reforming over cobalt-based catalysts

The catalytic performance of cobalt catalysts supported on γ-Al₂O₃, TiO₂, ZrO₂ were studied for bio-ethanol steam reforming (BESR) reaction. The supported catalysts (10 wt%Co) were prepared by impregnation and characterized through Thermogravimetric analysis (TGA), H₂ chemisorption, laser Raman Spectroscopy, Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS), and temperature-programmed reaction (TPRxn). The metallic cobalt sites were found to correlate with the BESR reaction activity. The reaction and H₂ chemisorption showed that ZrO₂ supported catalyst showed the best dispersion and best catalytic activity. Over the 10% Co/ZrO₂ catalyst, using a H₂O:EtOH:inert molar ratio of 10:1:75 and a GHSV = 5000 h⁻¹, 100% ethanol conversion and a yield of 5.5 mol H₂/mol EtOH were obtained at 550 °C and atmospheric pressure.     

低(等)压合成氨的最佳H2/N2与催化活性的关系

采用高压催化剂性能评价实验装置，在压力分别为7.0,10.0和15.0MPa，温度分别为350,400和450℃条件下，在H2／N2为1.6-3.0范围内研究了H2／N2对A301，ZA－5和A110－2型催化剂的活性和合成塔出口氨浓度的影响。在压力和空速一定的条件下，最佳H2／N2随反应温度而异。在350，400和450℃下，最佳H2／N2分别为1.8-2.2,2.2-2.5和2.5-3.0。由此可见，合成氨反应的速率达到最大值时的最佳H2／N2值与反应的进程有关。为此提出了催化剂效率K（Catalysis efficiency)的概念来表征在催化剂作用下反应器出口氨浓度趋近平衡的程度，即K＝CNH3／C^*NH3。根据实验结果，得到了最佳H2／N2与催化剂效率的定量关系：（H2／N2）m=1.5(1 CNH3/C^*NH3)=1.5(1 K)。由此可以根据催化剂在不同反应条件下的催化剂效率来确定最佳H2／N2。凡是会降低催化剂效率的因素，都会使最佳H2／N2降低。各种影响因素对最佳H2／N2的影响中，反应温度的影响最大，其次是空速和催化剂的活性，而压力和惰性气体含量的影响相对较小。在低温（低压）下合成氨，宜采用较低的H2／N2。     

<Superscript>1</Superscript>H NMR characterization of milk lipids: A comparison between cow and buffalo milk

Characterization of the lipid fraction of raw cow and buffalo milk samples, collected in different breeding areas in Apulia, a region of southern Italy, were performed by means of ¹H NMR. The aim of this work was to establish whether FA composition data obtained by ¹H NMR can be used in the differentiation of buffalo and cow milk samples according to species. A complete assignment of the signals present in the spectrum was attempted by COSY, heteronuclear coherence spectra. Quantification of FA was carried out by inserting the integrals of particular peaks in suitable calculations. Multivariate statistical analysis, conducted on the results of the quantification, permitted buffalo and cow milks to be distinguished.     

超磁致伸缩作动器的率相关Hammerstein模型与H∞鲁棒跟踪控制

利用Hammerstein模型对超磁致伸缩作动器（Giant magnetostrictive actuators,GMA）的率相关迟滞非线性进行建模,分别以改进的 Prandtl-Ishlinskii（Modified Prandtl-Ishlinskii）模型和外因输入自回归模型（Autoregressive model with exogenous input,ARX）代表Hammerstein模型中的静态非线性部分和线性动态部分,并给出了模型的辨识方法. 此模型能在1～100Hz频率范围内较好地描述GMA的率相关迟滞非线性. 提出了带有逆补偿器和H∞鲁棒控制器的二自由度跟踪控制策略,实时跟踪控制实验结果证明了所提策略的有效性.     

微波辐射下一步合成2-甲氧基-3-氰基-4-芳基吡啶和2-氨基-3-氰基-4-芳基吡喃衍生物

2，5－双亚苄基环戊酮与丙二腈在氢氧化钠－甲醇或哌啶－乙醇中，经微波辐射一步合成了2－甲氧基－3－氰基－4－芳基吡啶和2－氨基－3－氰基－4－芳基吡喃衍生物，反应在3－9mi内完成，产率56％－78％。     

2,2′-oxo-1,1′-azobenzene: microbial transformation of rye (Secale cereale L.) allelochemical in field soils byAcinetobacter calcoaceticus: III

Acinetobacter calcoaceticus, a gram-negative bacterium isolated from field soil, was found to be responsible for the biotransformation of 2(3H)-benzoxazolinone (BOA) to 2,2-oxo-1,1-azobenzene (AZOB). Experiments were conducted to evaluate the transformation of BOA to AZOB by this microbe in sterile and nonsterile soil. Transformation studies with soils inoculated withA. calcoaceticus indicated that the production of AZOB increased linearly with the concentration of BOA in sterile soil and showed a quadratic trend in nonsterile soils. This also indicated that all soil types studied for the transformation experiments might containA. calcoaceticus capable of the conversion of benzoxazolinones.     

碱金属盐对低氢酯比下苯甲酸甲酯加氢催化剂的修饰

为了考察了Mn与Zn摩尔配比以及不同碱金属盐修饰制得的锰锌复合氧化物催化剂对苯甲酸甲酯气固催化加氢合成苯甲醛反应活性和选择性的影响,在氢酯比为1.5的条件下,进行苯甲酸甲酯催化加氢反应,发现以5%LiCl修饰的活性组分负载量为25%、n(Mn)/n(Zn)为1.14的MnO-ZnO/γ-Al2O3催化剂,在常压、430℃、空时为1.84 h时,苯甲酸甲酯的转化率为97.71%,苯甲醛的选择性为84.80%.     

H4SiW12O40-PAn催化剂催化合成苯甲醛乙二醇缩醛

报道了以自制的H4SiW12 O40 (硅钨酸 ) -PAn (聚苯胺 )为催化剂 ,通过苯甲醛和乙二醇为原料合成了苯甲醛乙二醇缩醛。实验表明 :合成苯甲醛乙二醇缩醛适宜反应条件为 :n(苯甲醛 ) /n(乙二醇 ) =1 /2 .0 ,催化剂用量为反应物料总质量的 1 .0 % ,环己烷为带水剂 ,反应时间 1 .0h。上述条件下 ,苯甲醛乙二醇缩醛的收率可达 86.7% .