对叔丁基苯硼酸的合成及表征

以对叔丁基溴苯为原料，在氮气保护下，通过格氏反应合成了对叔丁基苯硼酸，考察了温度、反应时闻和物料配比等因素对收率的影响，优化合成条件为：n（对叔丁基溴苯）：n（硼酸三甲酯）=1：1．5，反应温度为-20-30℃，反应时闻140min，总收率69．5％。质谱和核磁共振光谱分析表明所得产物与目标产物结构一致。     

两种方法提取琉璃苣叶多糖的理化性质 及生理活性

本研究旨在制备两种琉璃苣叶水溶性多糖，进一步探究其结构特征，并评价其降血糖、抗癌和免疫活性。采用纤维素酶辅助提取（BLP-1）和微波辅助提取法（BLP-2）制备琉璃苣叶水溶性多糖，并比较了BLP-1和BLP-2的理化性质，通过分析α-葡萄糖苷酶和α-淀粉酶的抑制效果来评价BLP-1和BLP-2的降血糖活性，通过检测HepG2、MX-1和A549细胞的抑制率来评价抗癌活性，通过检测RAW246.7的免疫因子分泌来评价免疫活性。结果表明，BLP-1和BLP-2具有不同的多糖和蛋白质含量。BLP-1和BLP-2由阿拉伯糖（Ara）、半乳糖（Gal）、葡萄糖（Glc）、木糖（Xyl）组成，但摩尔比组成不同，其分子量分别为20.1和22.6KDa。热重分析（TGA）表明BLP-2比BLP-1具有更稳定的结构。这两种多糖具有抑制α-葡萄糖苷酶和α-淀粉酶活性、抑制HepG-2、A549和MX-1癌细胞增殖以及激活巨噬细胞RAW 264.7细胞分泌免疫细胞因子以介导细胞免疫反应的潜力。两种多糖可作为新功能食品和医药产品中的生物活性成分，为进一步研究两种多糖的构效关系提供了理论依据。     

ALKYD PAINT WASTE CHARACTERIZATION AND DISTILLATION

In the present study the characterization and distillation of alkyd paint waste have been carried out in order to establish the technical viability of organic solvents recovery and to decide upon the best environmental management for the waste stream from a paint spray-booth application in an automotive component factory. The paint is a black primer based on an alkyd resin with toluene and xylene as solvents, black carbon as pigment, fillers, and other minor components.

The paint, paint wastes, and distillation wastes have been characterized by determination of the physicochemical properties of the solid (solvents content and flash point) and determination of ecotoxicity (EC₅₀), total organic carbon (TOC), and metals concentration of the leachates. The highly volatile matter (HVM) content, determined by the weight loss at 200°C, has been used as a parameter to relate with the hazardous wastes regulations based on the characterization parameters EC₅₀, TOC, and flash point.

Distillation experiments have been performed in a simple batch mode with mixtures of paint waste, water, and additives in order to obtain high efficiencies in the recovery of volatile organic compounds and to obtain a final solid with nonhazardous behavior and good manageability qualities. A fractional factorial design (2^3-1) of experiments was carried out in order to study the influence of the distillation variables: water/paint waste ratio (2/1-3/1 (g/g)), temperature (110°-145°C), alkaline additives (Na(OH),CaO, Ca(OH)₂), and amount of other additives (wt.% of bentonite, cement, and Ca(OH)₂) on the solvent recovery, [% VOCs]_Recovery, on the residual volatile organic compounds, [% VOCs]_{Distillation Waste}, and on the total organic content (TOC) of the waste leachates. The present work shows the quantitative results of the alkyd paint waste distillation process under optimum conditions.     

Analysis of the polyethylene glycol glucosides and FA esters thereof by atmospheric-pressure ionization MS

Polyethylene glycol (PEG) glucosides (PEGG) and the PEGG esters of lauric acid were analyzed by atmospheric-pressure ionization MS (API-MS) with electrospray ionization. Straightforward mass characterization of the complex mixtures could be achieved without prior chromatographic separation. The constituents were identified on the basis of quasi-molecular ions. Individual components could be observed as protonated molecular ions [M+H]⁺ and/or as their NH₄ ⁺, Na⁺, or K⁺ adducts in positive ion mode. The mass spectrometric investigation showed that mixtures of PEGG consisted of monoglucoside, diglucoside, polyglucoside, and free PEG. The esterification product is a mixture of two types of nonionic surfactants: PEG-laurates and PEGG-laurates. The reasons for distortion of the quasi-molecular ion intensities and the stabilization of adduct ions were discussed. The rapid and highly sensitive API-MS analysis technique proposed here is well suited for direct characterization of complex mixtures and suitable for development as a routine analytical method.     

改性磁性壳聚糖微球的制备、表征及性能研究

以(NH4)2Fe(SO4)2.6H2O、NH4Fe(SO4)2.12H2O和壳聚糖为原料,经羟丙基化、胺基化,采用一步包埋法制备了一种新型的多胺基化磁性壳聚糖微球。通过正交实验法确定了磁性微球的最佳制备条件,即搅拌速度1200r/min,壳聚糖用量3.0g,环氧氯丙烷用量2.5mL,乙二胺用量2.5mL。并用IR、TG、XRD和SEM对其结构及形貌进行了表征。结果表明,Fe3O4磁性粒子已包埋了一层胺基化壳聚糖。磁性微球胺基含量为2.302mmol/g;呈较规则的球形,平均粒径为209nm,且具有顺磁性和良好的耐酸性。     

Characterizing image quality of autostereoscopic displays by using the maximum luminance at each viewing position

A metric of the 3D image quality of autostereoscopic displays based on optical measurements is proposed. This metric uses each view's luminance contrast, which is defined as the ratio of maximum luminance at each viewing position to total luminance at that position. Conventional metrics of the autostereoscopic display based on crosstalk, which uses “wanted” and “unwanted” lights. However, in case of the multiple‐views‐type autostereoscopic displays, it is difficult to distinguish exactly which lights are wanted lights and which are unwanted lights. This paper assumes that the wanted light has a maximum luminance at the good stereoscopic viewing position, and the unwanted light also has a maximum luminance at the worst pseudo‐stereoscopic viewing position. By using the maximum luminance that is indexed by view number of the autostereoscopic display, the proposed method enables characterizing stereoscopic viewing conditions without using wanted/unwanted light. A 3D image quality metric called “stereo luminance contrast,” the average of both eyes' contrast, is proposed. The effectiveness of the proposed metric is confirmed by the results of optical measurement analyses of different types of autostereoscopic displays, such as the two‐view, scan‐backlight, multi‐view, and integral.     

Variable temperature13C MAS NMR of KFe2Mn(CO)12 in the solid state and as aCatalyst precursor on a carbon support

Variable temperature¹³C MAS NMR spectra are reported for¹³CO-enriched KFe₂Mn(CO)₁₂ as a solid and also as dispersed clusters on a carbon support. The spectrum of KFe₂Mn(CO)₁₂ at 300 K agrees with the proposed structure for this cluster and shows that the cluster is static. Two bridging carbonyl resonances are clearly resolved and, by comparison with¹³C MAS NMR spectra of Mn₂(CO)₁₀ and Fe₂(CO)₉, all terminal resonances for the cluster can be assigned. When the cluster is supported on carbon, two broad resonances are observed at room temperature which are assignable to KFe₂Mn(CO)₁₂ and a decomposition product, Mn₂(CO)₁₀. The carbonyl ligands in both supported clusters are completely averaged, and KFe₂Mn(CO)₁₂ on the carbon surface demonstrates fluxional behavior similar to that observed for the cluster in solution. For this fluxional process, activation energies of 0.6 kcal/mol and 0.5 kcal/mol are estimated for carbon-supported KFe₂Mn(CO)₁₂ and Mn₂(CO)₁₀, respectively.     

双水解法制备SO4^2-/SnO2·SiO2固体超强酸及其结构表征

用双水解法合成了SO24-/SnO2-SiO2固体超强酸催化剂。采用FTIR、TG-DTA和XRD技术研究了SO24-/SnO2-SiO2的结构,其测试结果表明:SO42-/SnO2-SiO2的结构与其催化活性存在很好的一致性。     

5-氰基-4-氨基咪唑的合成与热性能

咪唑基含能化合物是目前高能化合物的重要研究方向，而5-氰基-4-氨基咪唑是设计、合成新型咪唑联四唑类高能高氮化合物的关键中间体。以5-甲酰胺基-4-氨基咪唑（AICON）为原料，经其与三氯氧磷（POCl3）的脱水反应获得了5-氰基-4-氨基咪唑（AICN），通过优化反应体系、反应温度、反应时间以及物料物质的量比，使得AICN的收率>65%，纯度（HPLC）>99.5%。此外，采用NMR、IR和元素分析对其进行了结构确征，利用热重分析法研究其热性能。结果表明：AICN的最佳反应条件为以POCl3为脱水剂，n(AICON)：n(POCl3)为1:10，反应升温模式为先快速升温至80~85 ℃，维持反应30 min，然后降温至70~75 ℃，维持反应1~1.5 h；AICN在40~1000 ℃温度区间存在两个失重过程，对应的热分解温度区间分别为40~400 ℃和400~1000 ℃、热失重分别为19.8%和60.7%、热分解峰温分别为256.5和698.4 ℃，表明其具有良好的热稳定性。     

二苯并噻吩合成方法的改进

对文献报道的由联苯和硫在AlCl3催化下反应合成二苯并噻吩(DBT方法中的提纯过程作了改进，大大简化了提纯步骤，使制备DBT的时间缩短了一半，产率为63．4％，经提纯后的成品含量达99．7％，其纯度、外观、晶相均优于进口试剂，但成本远低于进口试剂。产品用FT-IR、LRS、XRD和^1H NMR表征结果与文献报道完全相符合。