以粉煤灰为原料制备ZSM-5沸石分子筛及其储氢性能

近年来,随着国内燃煤发电量的持续增长,作为燃煤电厂最主要的固体废弃物,粉煤灰的排放量也随着燃煤消耗的增长而急剧增加,引发了严峻的社会和环境问题。粉煤灰中的铝和硅元素含量很高,具有极高的提取价值。本文先对粉煤灰进行酸处理,除去粉煤灰中碱金属元素,提高硅铝比,之后采用水热合成法直接合成了高结晶度的ZSM-5沸石分子筛,此外还在水热合成时加入一定比例正硅酸乙酯(TEOS)后制备高硅铝比ZSM-5沸石分子筛,对二者在结构、结晶度和储氢性能方面进行了研究。结果表明,加TEOS后的ZSM-5的储氢性能比没有加TEOS的储氢量高,储氢量从0.584%增加到0.846%。     

脱氢枞酸酯键合硅胶色谱固定相的制备及应用

A dehydroabietic acid glycidyl methacrylate ester (DAGME)-bonded silica stationary phase (Sil-DAGME) was fabricated in this paper. The DAGME was firstly prepared using dehydroabietic acid and glycidyl methacrylate via a ring-opening addition reaction, and then grafted onto the surface of a thiol-functionalized spherical silica by click reaction to obtain the Sil-DAGME. The successful immobilization of DAGME on the silica was confirmed through series of characterizations including Fourier-transform infrared spectroscopy (FT-IR), thermal gravimetric analysis (TGA)and elemental analysis (EA). The chromatographic performance and retention mechanisms of Sil-DAGME were validated using a variety of compounds including alkylbenzenes, Tanaka standard test mixtures, polycyclic aromatic hydrocarbons, phenols and flavonoids. Meanwhile, the Sil-DAG⁃ME exhibits multiple interactions, including hydrophobic, π-π and hydrogen bonding interaction between the stationary phase and the analytes during the separation process due to the co-existing of benzene ring, carbonyl group, hydroxyl group and hydrophobic rigid tricyclic hydrophenanthrene skeleton in the DAGME on the silica surface. Based on synergistic action of multiple retention mechanisms, the probe molecules metioned above achieved ideal resolution and flexible selectivity in separation. In addition, the Sil-DAGME not only exhibited good stability, repeatability and reproducibility with the run-to-run relative standard deviations (RSDs) of 0. 050%-0. 19% (n = 10), the daytoday RSDs of 0. 25%-1. 0% (n = 7), and the column-to-column RSDs of 0. 78%-2. 1% (n = 3) for the retention time, but also showed an excellent separation ability for Yew tree bark extract. In short, the application of dehydroabietic acid in chromatographic separation materials not only provided a new approach for the separation and detection of paclitaxel, but also presented a reference for the design stationary phase using natural product rosin as functional ligand. © 2023, China Association for Instrumental Analysis. All rights reserved.     

Self-assembly behaviour of amphiphilic diblock copolymer in selective solvents studied by synchrotron small-angle x-ray scattering

The aggregation behaviour of styrene-vinyl benzoic acid (PSm-b-PVBAn) amphiphilic diblock copolymers in selective solvents with different m and n was investigated by synchrotron small-angle x-ray scattering (SAXS). We have carried out a detailed analysis of scattering intensity, dimension, shape and microstructure of the diblock copolymers of narrow distribution in water, methanol, ethanol and isopropanol selective solvents, respectively. We have found that the aggregation behaviour of the copolymer depends on the nature of the solvent and the micelle forms fiat disc objects with the ratio of radius ω=0.4. The average radius gyration Rg of the copolymer decreases as solvents change from isopropanol to ethanol and to methanol, and increases with increasing pH in aqueous solution, but decreases with the addition of COCl2 in ethanol solvent. The scattering intensity of diblock copolymer micelle follows I(h) ∝ h^-α in different selective solutions, suggesting that the PSm-b-PVBAn coils have self-similar structure behaviour or a fractal structure in the selective solvents. All of these revealed that the aggregation behaviour of the diblock copolymer changes dramatically with experimental condition in the selective solvent. The increase of mass fractal dimension (Dm) from 2.12 to 2.47 indicates that the copolymer chain changes from a swollen coil to a rather compact disc in the course of changing solvents, decreasing surface fractal dimension (Ds) from 2.98 to 2.58 indicates that the copolymer micelle change from a rather rough surface to a smooth form in the course of increasing pH in aqueous solutions, and increasing Dm and Ds from 2.29 to 2.35 and 2.70 to 2.90, respectively, indicates the shrinkage of copolymer micelle to a rather compact and rough disc form by adding COCl2 in ethanol solvents.     

富硒灵芝中一种新含硒蛋白的纯化、性质及其自由基清除活性研究

通过硫酸铵沉淀、离子交换层析和分子排阻层析等方法, 从富硒灵芝中获得了一种新的含硒蛋白, 命名为Se-GL-P, 并研究了此蛋白的性质、抗氧化活性与其硒含量间的关系. 结果表明, 此蛋白的分子量为36600, 分子中约含有19.8%的糖链, N端的氨基酸残基序列为DINGGGATLPQKLYLTPDVL, 属于DING蛋白家族. 硒含量为4.87 mg/g, 具有较高的羟自由基和超氧自由基清除活性. 研究发现, Se-GL-P的抗氧化活性的提高与其中硒含量的提高相关.     

生物样品中微量硒测定方法的进展

概述了近年来硒含量测定方法如荧光法、原子吸收光谱法、原子荧光法、等离子体发射光谱法、分光光度法、气相色谱法、高效液相色谱法等的研究进展,阐述了各种方法在实际研究中的优势与不足,引用文献63篇。     

Burgers-BBM方程新的精确解

借助两个推广形式的Riccati方程组和Mathematica软件，求出了Burgers-BBM方程，BBM方程，KDV—Burgers方程的大量新的精确解，包括各种形式的孤立波解和三角函数周期解．     

WEIGHTED COMPOSITION OPERATORS ON WEIGHTED DIRICHLET SPACES

We characterize the boundedness and compactness of weighted composition operators on weighted Dirichlet spaces in terms of Nevanlinna counting functions and Caxleson measure.     

邻苯二酚与乙醇单醚化反应用固体酸催化剂表面上的积炭行为

 研究了邻苯二酚与乙醇气固相单醚化反应用固体酸催化剂表面上的积炭行为，并用TG－DTA，BET，GC－MS，FT－IR和元素分析等手段对积炭物种进行了表征．结果表明，催化剂上有两种类型的积炭，一类属可溶性积炭，主要由二苯醚及其衍生物组成，可在低温燃烧除去；另一类属不可溶性积炭，主要为缺氢的芳烃类聚合物或类石墨碳，需在高温下才能烧除．积炭主要发生在4～8nm范围的中孔内，导致反应后的催化剂大孔范围的孔分布所占的分数增大．随着反应的进行，总积炭量逐渐增多．     

制备方法对CuO—Ce0．7Zr0．3O2催化剂的氧缺位和CO氧化活性的影响

采用溶胶-凝胶法和溶胶-凝胶 浸渍法两种方法制备了CuO-Ce0.7Zr0.3O2催化剂,并对催化剂进行了XRD、Raman等表征,考察了催化剂的CO氧化性能.研究结果表明,溶胶-凝胶法制备的CuO-Ce0.7Zr0.3O2催化剂的CO氧化活性明显高于溶胶-凝胶 浸渍法制备的CuO/Ce0.7Zr0.3O2催化剂,CuO-Ce0.7Zr0.3O2催化剂容易形成氧缺位和表面高分散CuO的颗粒较大,从而提高催化活性.