5-羟基色满的合成

以2',6'-二羟基苯乙酮为起始原料,在钠催化下和甲酸乙酯缩合制得5-羟基-4-色酮,然后催化氢化还原得到5-羟基-4-色满酮,最后用锌汞齐还原制得5-羟基色满。所设计的5-羟基色满合成路线总收率能达到37%,是合成5-羟基色满的新路线。     

6-羟基色满的合成

以2′,5′-二羟基苯乙酮和原甲酸三乙酯缩合得到6-羟基-4-色酮,再经催化氢化得到标题化合物。这是合成6-羟基色满的新路线,收率能达到47%。     

3,4-二羟基苯腈的合成

以3-甲氧基-4-羟基苯甲醛（香兰素）为原料,经与盐酸羟胺反应得到3甲氧基-4-羟基苯腈,再与碱金属卤化物经脱甲基化反应合成3,4-二羟基苯腈,产品含量99.8%,以香兰素计总收率75.2%。与其他合成方法比较,这条合成路线更适合于工业化。     

4-羟基吡啶的合成工艺进展

分别介绍了以草酸二乙酯、丙酮、氨气为原料经缩合、水解、氨化和热解反应合成4-羟基吡啶;以吡啶、氯化亚砜为起始原料经氯化和水解反应合成4-羟基吡啶;以4-氨基吡啶为起始原料经重氮和水解反应合成4-羟基吡啶;并对这些合成路线进行了探讨.     

C.I.颜料橙65的合成研究

本文简述了由2-羟基-1-萘醛和邻苯二胺及镍盐来合成C.I.颜料橙65。着重介绍了以β-萘酚为起始原料来合成中间体2-羟基-1-萘酚的工艺路线选择,及温度、时间、pH值对2-羟基-1-萘醛产率的影响;以邻硝基苯胺为起始原料来合成中间体邻苯二胺的工艺路线的选择,及温度、pH值、Ni催化剂对邻苯二胺合成的影响。     

硫酸催化合成α-溴-4-羟基苯乙酮

介绍已有的合成路线,经过评价提出新的合成方法,即在硫酸催化下用对羟基苯乙酮α-溴化合成了α-溴-4-羟基苯乙酮。反应条件:反应物摩尔比为1·01·0,反应温度80~90℃;催化剂用量为反应物酮的70%(质量比),反应时间4h。收率为83·5%。     

2-溴甲基-3-羟基吡啶合成工艺的改进

2-溴甲基-3-羟基吡啶是合成常山酮的中间体,以3-羟基吡啶为起始原料,经胺甲基化、醋酐乙酰化、浓氢溴酸水解3步反应,合成2-溴甲基-3-羟基吡啶,总收率达56.79%。通过MS和1 H NMR对化合物结构进行表征。该方法原料是工业级,反应条件平和,对设备的要求不高,可以满足工业化路线的要求。     

中间体2,4-二羟基苯乙酮合成工艺研究

介绍了合成2,4-二羟基苯乙酮的工艺路线：在催化剂的作用下,由原料间苯二酚和冰醋酸经付-克反应合成2,4-二羟基苯乙酮。最佳反应条件为：冰醋酸用量12 g、催化剂用量16 g、反应时间1.5 h、反应温度135℃。产品经紫外、红外、熔点和Rf值鉴定为2,4-二羟基苯乙酮。     

1,3-二羟基萘的合成与应用

综述了1,3-二羟基萘的合成与应用。合成路线包括以3-羟基-1-萘磺酸钠,4-羟基-2-磺酸钠,1,3-茶二磺酸为原料的碱熔法;纳米二氧化钛水性悬浮液中萘的光催化直接氧化二羟基化制备法;由γ苯基乙酰乙酸乙酯或苯基乙酰氯在硫酸中环合制备三种合成方法。从工艺简便性和环保角度出发,应着重研究和开发光催化羟基化法。有26篇参考文献。     

1-[2-(2-羟基乙氧基)乙基]哌嗪的合成研究进展

简述了6种常见的1-[2-(2-羟基乙氧基)乙基]哌嗪的合成路线,并对其优缺点进行了比较。     

The promotion of CO electro-oxidation on platinum-bismuth as a model for surface mediated oxygen transfer

The results of electrochemical studies of CO oxidation on clean and bismuth modified Pt(1 1 0)-(1×2) and Pt(1 1 1) surfaces and a supported platinum catalyst are compared. The effect of sub-monolayers of bismuth is to increase the CO oxidation potential on Pt(1 1 0)-(1×2), and decrease it on Pt(1 1 1). This primarily reflects the rather low potential for CO oxidation characteristic of the more open packed Pt(1 1 0)-(1×2) surface, and the higher potential characteristic of the close packed Pt(1 1 1) face. The oxidation potential of CO in the intermixed CO/Bi phases on the single crystals is very similar. The effect of bismuth on the supported platinum catalyst is to increase the CO oxidation potential by a similar amount to that found for Pt(1 1 0)-(1×2). In addition, modification by bismuth results in a concomitant reduction in the CO tolerance of the commercial catalyst. CO oxidation on the catalyst exhibits poisoning by bismuth in a similar fashion to Pt(1 1 0)-(1×2), and the bismuth redox couple on the catalyst is the same as that found on Pt(1 1 0)-(1×2). High coverages of bismuth on the catalyst do not appear to reduce its activity for hydrogen oxidation. These results are discussed in the context of the requirement for surface mediated oxygen transfer during CO electro-oxidation.     

利用酒精废液浓缩液生产有机-无机复混肥技术

介绍利用酒精废液生产有机-无机复混肥的工艺流程、原料配比及关键设备的操作控制。酒精废液利用列管式蒸发器浓缩至w(H2O)约40%,再与尿素、磷酸一铵、氯化钾等通过转鼓造粒机生产的11-7-7-20(有机质)有机-无机复混肥符合国家标准。     

La2/3Sr1/3MnO3(La1.4Sr1.6Mn2O7)/Ce0.8Gd0.2O2-δ复合阴极的微观结构及热膨胀性能

采用固相反应法制备La2/3Sr1/3MnO3(LSMO3)粉体,用溶胶-凝胶法分别制备La1 4Sr1 6Mn2O7(LSMO7)和Ce0.8Gd0.2O2-δ(CGO)粉体.分别将LSMO3和LSMO7粉体与CGO粉体以1∶1的质量比均匀混合,在300MPa下冷等静压成型,并在1 500℃烧结2 h,制备了LSMO3/CGO和LSMO7/CGO复合阴极材料.研究了2种复合阴极材料的微观结构和热膨胀性能.结果表明:LSMO3/CGO与LSMO7/CGO烧结体在150～1 000℃温度范围内的平均线性热膨胀系数分别为1.52×10-5/K和1.53×10-5/K,与CGO固体电解质具有相近的热膨胀性能.烧结体断面形貌分析表明:LSMO3/CGO复合阴极具有与CGO相似的断面显微结构.     

甲氧头孢菌素中间体7-AMCA的合成工艺优化

7β-氨基-3-（1-甲基-1H-四唑-5-硫甲基）-3-头孢烯-4-羧酸（7-AMCA）是合成甲氧头孢菌素关键中间体7β-氨基-7α-甲氧基-3-（1-甲基-1H-四唑-5-硫甲基）-3-头孢烯-4-羧酸二苯甲酯（7-MAC）的重要中间体。采用7-氨基头孢霉烷酸（7-ACA）和1-甲基-1H-1,2,3,4-四唑-5-硫醇（5-MMT）为原料,以乙酸为溶剂,甲磺酸为催化剂,经亲核取代制备得到7-AMCA。本文主要探讨了物料配比、催化剂用量、反应时间和温度等因素对反应的影响,并通过二次回归建立了数学模型,确定了合成7-AMCA的最佳工艺条件。在此基础上合成的产品收率高达93．24％,HPLC纯度98．76％。产品结构经^1H NMR和IR表征确认。     

Theoretical study of benzene,toluene, and dibromobenzene at a Si(111)7×7 surface

Theoretical Austin model 1 (AM1) calculations on the adsorption of benzene and toluene on Si(111)7×7 are presented. Both physisorbed and chemi-sorbed states have been calculated for up to three adsorbed molecules per half unit cell of the Si(111)7×7 surface. Secondly, theoretical calculations on the induced attachment of benzene as well as rationalization of the dynamics of the halogenation reaction of 1,2- and 1,4-dibromobenzene on Si(111)7×7 are reviewed. The main incentive for this study was the interpretation of recent experimental scanning tunneling microscopy (STM) results from the Toronto laboratory on a new electron-induced or photo-induced attachment process for benzene on Si(111), and, particularly, experimental results related to the thermal dissociative reactions of 1,2- and 1,4-dibromobenzene on a Si(111)7×7 surface. The central objective is to relate the reagent geometry in 1,2-dibromobenzene and 1,4-dibromobenzene to the Br-Br pair distance of dibrominated Si(111)7×7. For benzene, we propose a possible path for the conversion from the normal strained di-sigma-bound state (S) at Si(111) to a more strongly bound state (B) consisting of a phenyl plus an H-atom adsorbed species. For 1,2- and 1,4-dibromobenzene dibromination of silicon, evidence has been found for two mechanisms of reaction. One reaction pathway involves intermediate binding of the organic molecule on the Si surface through C-Si bonds, analogous to the benzene S structure. The second dynamical pathway involves intermediate binding through weak Br. Si attachment followed by formation of pairs of covalently-bound Br-Si. The outcomes from the two dynamical pathways are consistent with the observed STM patterns for pairs of Br-Si at Si(111) 7×7 due to the reaction of 1,2- and 1,4-dibromobenzene.     

摩擦材料中纤维品种的选择及性能研究

采用干法工艺热压成型,制备混杂纤维增强无石棉摩擦材料,热压温度为165℃,压力为25 MPa,热压时间为500 s,在180℃下热处理120 min。测定材料的摩擦磨损性能、物理性能。结果表明,玻璃纤维混杂增强摩擦材料的摩擦因数在0.33⁰.41之间变化,磨损率为0.28×10-70.41之间变化,磨损率为0.28×10-7⁰.54×10-7cm3/(N·m),洛氏硬度为HRM 76.0,密度为2.18 g/cm3。     

钛白粉——硫酸用量增长

介绍了硫酸法和氯化法钛白粉生产工艺.钛白粉生产是硫酸主要非化肥用户,硫酸消费量7 000～7 500 kt/a.过去10年亚洲钛白粉需求量每年以5％ ～ 6％的速率递增,其中中国则以6.5％的速率增长.预计到2020年全球钛白粉总需求为7 600 kt,其中中国需求达到2 800 kt;届时钛白粉行业耗酸量会达到8 000 ～9 000 kt.未来硫酸法钛白粉产能将继续扩张,尤其是在中国、印度、巴西和越南等国家.     

Large‐Scale X‐Ray Microtomography Analysis of Fiber Orientation in Weld Line of Short Glass Fiber Reinforced Thermoplastic and Related Elasticity Behavior

Large‐scale X‐ray microcomputed tomography (μ‐CT) is used to investigate microstructural features of weld lines in a short glass fiber reinforced polymer. The main originality of this work is related to the evaluation of local structural and mechanical characteristics in zones of unmastered heterogeneities. Complete and incomplete injection molded plates are considered to investigate weld lines with and without process‐induced porosity. Using a helical scanning trajectory, the full 3D microstructure is obtained at centimetric scale to cover a large zone including first contact between colliding fronts at a voxel size of 3 μm. Microstructure analyses show that weld line area is ill‐ordered at the fiber and structure length scales. Near the first contact point, fiber orientations show the signature of vortexes, which mark the presence of repulsive forces. The presence of micrometric porosity is only confirmed in incomplete plates. μ‐CT images are used as inputs to create a full‐scale finite element model for assessing strain localization. Predicted principal strains are compared to digital image correlation measurements performed during uniaxial tensile tests. Full‐scale modeling combined to 3D high‐resolution imaging proves high potential to correlate local fiber heterogeneities with strain localization effects.

     

LIQUID-LIQUID EXTRACTION OF 2,3-BUTANEDIOL FROM DILUTE AQUEOUS SOLUTIONS WITH MIXED SOLVENTS

Distribution coefficients for the liquid-liquid extraction of 2,3-butanediol (5wt%) in aqueous solutions with binary mixtures of 4-nonylphenol (0-67 vol%), toluene and several alcohols, (2-ethyl-l-hexanol, 1-oclanol and 1-decanol) at 25°C are reported. The distribution coefficients were in the following ranges: 4-nonylphenol + toluene (0-0·23), 4-nonylphenol + 2-ethyl-l-hexanol (0·23 - 0·27), 4-nonylphenol + 1-octanol (0.21-0·33) and 4-nonylphenol + 1-decanol (0·22-0·37). The largest distribution coefficient was found to be 0·37 for the mixed solvent 4-nonylphenol+1-decanol (50vol%), which shows a slight decrease in the separation factor. Activity coefficients at infinite dilution were determined using the MOSCED model and a similar trend for all the solvent mixtures of 4-nonylphenol and alcohols was found.