A simple, rapid, and efficient oxidation of oximes to ketones and aldehydes with manganese dioxide catalyzed by kieselguhr under solvent-free conditions

A simple, rapid, and efficient oxidation of oximes to the corresponding ketones and aldehydes with manganese dioxide catalyzed by kieselguhr under solvent-free conditions at room temperature in the yields between 82 and 98 is described. It seems that kieselguhr in the present procedure can highly expedite the reaction rate. By comparing to other methods described previously, the main advantages of this oxidation are that the oxidations are more efficient, the reaction conditions are milder, the reaction times are shorter, and the work-up is easier. Furthermore, the amount of manganese dioxide used in this oxidation is largely decreased.     

A type of spectrophotometer with both SCI and SCE measurement structures

In order to measure the color of different samples with different surface texture, multiple measurement and observation conditions are needed from the instrument. Thus, both SCI (specular component included) and SCE (specular component excluded) measurement conditions are included in most color measuring instruments today. In current design, a light trap is established in the integrating sphere, and the instrument uses mechanical control to switch between SCI and SCE measurement modes. However, establishing a light trap inside the integrating sphere will affect the SCI and SCE measurement results. This article discusses the problems in current design, proposes a dual light source structure that includes both SCI and SCE measurement conditions, and then evaluates the structure with experiments. The experiment results show that the improved structure is more suitable for color measuring instruments with both SCI and SCE modes, and it has high practical value.     

表面增强拉曼光谱研究自组装单分子层在化学接触和纳米隔绝下的分子振动活性变化(英文)

为确定表面增强拉曼光谱中某些有争议的弱振动模式是来自高阶的影响还是分子基团对称性变化的影响,本文以1,4-苯二硫醇作为探针分子提供了一种实验验证的框架方法.光谱实验显示,观测到的有争议的弱振动模式并不是来自高阶的影响,而是分子基团对称性变化所致.我们的实验框架方法很容易拓展开来,如用于研究其它波长激光激发的类似体系或有机分子搭接的分子结.     

液相色谱-电雾式检测器同时测定生物缓冲溶液中盐酸胍与氯离子含量

提出了液相色谱法测定生物缓冲溶液中盐酸胍与氯离子含量。以Acclaim Trinity P1色谱柱(3.0mm×100mm,3μm)为分离柱,乙腈和0.020mol.L-1乙酸铵溶液按30比70混合(用乙酸调节pH至5.0)为流动相进行淋洗,用电雾式检测器检测,雾化器温度25℃,采样频率5Hz。盐酸胍和氯离子的峰面积与质量浓度均在0.20～5.00g.L-1范围内呈线性关系,方法检出限(3S/N)分别为0.005,0.001g.L-1。采用标准加入法做回收试验,盐酸胍和氯离子的平均回收率分别为96.0%和92.5%,相对标准偏差(n=7)均小于1.0%。     

MoO2@氮掺杂碳复合物的制备及其降解有机污染物

以多巴胺、钼酸铵、碳酸氢铵为原料，通过一步煅烧法合成一种 MoO₂@氮掺杂碳复合物(MoO₂@CN)，并利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、拉曼光谱(Raman)等对其进行表征。以卡马西平(CBZ)为目标污染物，以过一硫酸氢钾(PMS)为氧化剂，在温度为25 ℃、pH为6.5的条件下，MoO₂@CN/PMS在12 min内对CBZ的去除率达99.2%，与商用MoO₂相比，其表观速率常数k_obs(0.393 min^-1)是商用MoO₂(0.016 4 min^-1)的24.0倍，这主要是由于制备的MoO₂@CN比商用MoO₂具有更好的电子传输能力以及更大的比表面积。MoO₂@CN在 pH为 2.5~10.5时均能有效降解 CBZ，而且对大多数染料、酚类化合物、抗生素等多种污染物均具有良好的降解性能。此外，MoO₂@CN/PMS在60 min内对CBZ的总有机碳(TOC)去除率高达74.0%。电子顺磁共振波谱(EPR)和自由基猝灭实验显示MoO₂@CN/PMS体系中主要起作用是硫酸根自由基(SO₄^·-)和羟基自由基(·OH)。更有意思的是，在Fe²⁺/PMS体系加入MoO₂@CN后，其催化降解CBZ的性能显著增强，k_obs(1.25 min^-1)是单独Fe²⁺/PMS体系(0.079 7 min^-1)的15.7倍，这主要归因于MoO₂@CN的引入加快了Fe³⁺到Fe²⁺的转变，导致更多·OH的生成。     

New simple exact penalty function for constrained minimization

By adding one variable to the equality-or inequality-constrained minimization problems, a new simple penalty function is proposed. It is proved to be exact in the sense that under mild assumptions, the local minimizers of this penalty function are precisely the local minimizers of the original problem, when the penalty parameter is sufficiently large.     

Synthesis of aromatic diamine-based benzoxazines and effect of their backbone structure on thermal and flammability properties of polymers

Three kinds of novel aromatic diamine-based benzoxazines containing naphthalene, propane-2,2-diyldibenzene and neopentyl groups in the backbone, respectively (designated as BAPNCP, BAPBACP and BAPNPGCP, respectively), were synthesized and characterized. In addition, the effects of backbone structures on curing behaviors of the monomers and thermal and flammability properties of the resulting polymers were systematically studied. The results indicated that BAPNPGCP displayed the highest enthalpy of the curing reaction associated with the ring-opening of benzoxazine, which was due to the effect of benzoxazine ring content per unit mass. Interestingly, the 5 wt% weight loss temperature and char residue after thermogravimetric test for poly(BAPNPGCP) were 8 °C and 7% higher than those of poly(BAPBACP). Meanwhile, the total heat release of poly(BAPNPGCP) was less than half of that for poly(BAPBACP), indicating the substantial effect of benzoxazine ring content on flammability and char formation. Furthermore, it was found that poly(BAPNCP) gave the best thermal stability and flame retardancy, which was due to the synergistic effect between naphthalene group and benzoxazine ring content. This study provides new insight into the curing behavior of benzoxazine and further understanding on the high performance of polybenzoxazine.