HPLC semi‐preparative separation of diclazuril enantiomers and racemization in solution

Diclazuril has been widely used in poultry feed for prevention and treatment of coccidiosis, and its chiral separation is rarely reported. Herein, semi‐preparative separation method of diclazuril enantiomers has been developed through normal‐phase high‐performance liquid chromatography. Effects of chiral stationary phases, alcoholic modifiers, and column temperature on separation of diclazuril were discussed in detail. Both the single‐urea‐bound 4‐chlorophenylcarbamoylated β‐cyclodextrin and amylose tris(3,5‐dimethylphenylcarbamate)‐coated chiral stationary phases showed strong ability in separation of diclazuril by using n‐hexane–trifluoroacetic acid–ethanol. Then, semi‐preparative separation of diclazuril was carried out through stacked injection, and the "enantiomeric excess" purities of two fractions were over 98%. Next, the electronic circular dichroism profiles of these two fractions in ethanol solution displayed the mirror image of each other in the range 360–200 nm. Moreover, effects of acidic/basic additive, time, and temperature on racemization of diclazuril enantiomers in ethanol solution have been studied in detail through normal‐phase high‐performance liquid chromatography. Racemization of diclazuril enantiomers was remarkably accelerated through adding triethylamine at high temperature. We envision that this systematic investigation of diclazuril at an enantiomeric level would provide valuable information in future studies involving enantioselective bioactive, metabolic, and toxicological activities.     

A facile synthesis of anatase TiO2 nanosheets-based hierarchical spheres with over 90% {001} facets for dye-sensitized solar cells

Anatase TiO(2) nanosheets-based hierarchical spheres with over 90% {001} facets synthesized via a diethylene glycol-solvothermal route were used as photoanodes of dye-sensitized solar cells, which generated an energy conversion efficiency of 7.51%.     

表面炭化磺酸基型阳离子树脂的制备及其对Fe(Ⅲ)吸附性能的研究

将对苯乙烯磺酸钠(SSS)聚合接枝到表面炭化的CD301树脂表面,成功制备出一种新型吸附材料PSSS-g-CD301。研究了影响表面引发接枝聚合的主要因素,并采用静态法考察了PSSS-g-CD301对Fe(III)的吸附行为。结果表明,在接枝过程中,适宜的接枝时间是10h,适宜的引发剂用量为单体质量的1%,适宜的温度为35℃,适宜的单体质量分数为10%。PSSS-g-CD301对Fe(III)的吸附容量可以达到0.28mmol/g(p H=2,温度288K);准二级动力学方程可以更好地描述吸附动力学规律;吸附行为符合Langmuir与Freundlich吸附模型;热力学参数?H、?G、?S的计算结果表明,该吸附过程为自发的放热过程。     

开口圆环类声子晶体传播禁带特性研究

为衰减中低频振动噪声,本文设计了一种非严格对称的开口圆环类声子晶体结构,基于有限元法和弹性波理论分析了其禁带特性和各方向的振动衰减性能;结合系统的振动模态解释了带隙打开和关闭的原因,并分析了几何参数对带隙宽度的影响规律.结果表明:由于晶体的非严格对称,仅 ΓX方向的传输损耗和禁带特性吻合,且衰减性能优于MΓ 方向,禁带...     

The adsorption behaviours of Pt adatom on pristine and defective bilayer graphene

The structural stability and electronic property of metal Pt atom anchors on two typical substrates (including the pristine and defective bilayer graphene, PBG and DBG) are studied using the first-principles calculations. For the PBG sheets, the Pt atom at the bridge site of bottom layer has only one stable adsorption, which is more stable than other sites of the top layer. For the DBG sheets, the doped Pt below defective site has the larger adsorption energy than that of the upper one. Compared to the isolated graphene films, the Pt(111) substrate-supported graphene systems have effect on the adsorption energies of Pt adatom to some extent, but it does not affect the most preferable configurations. Moreover, the diffusion pathways and energy barriers of Pt adatom on PBG and DBG substrates are comparatively investigated. For the DBG sheets, the Pt dopant has smaller diffusion barrier on upper layer than that of the intercalation process through the defective site. Therefore, the Pt dopant prefers to diffuse on the top layer and then forms the metal impurity. This work provides valuable information on understanding the formation process and intercalation mechanism of metal adatom on graphene sheets.     

基于铅铟合金线的SFQ多芯片超导互连方法研究

用基于铅铟合金线的引线键合(WB)工艺对单磁通量子(SFQ)多芯片的超导互连方法进行了研究,将铅含量75%,铟含量25%的铅铟合金线制备成WB线材,用超声楔形焊工艺成功实现SFQ芯片I/O接口焊盘的超导互连.拉力测试表明室温下铅铟合金线键合强度与同线径金线相当,优于同线径铝线;用开尔文四端法测量了铅铟合金线互连的多级超导转变温度以及线材与超导芯片之间的接触电阻,结果表明该铅铟合金线的超导转变温度为6.63 K,当温度降低至6.63 K或更低时,铅铟合金线的线阻以及线材与SFQ芯片I/O接口焊盘的接触电阻为0,实现了超导互连;并通过热冲击实验验证该WB结构具有优异的热稳定性.     

2，2′－二氨基联苄二磷酸盐的气相色谱分析

The gas chromatographic separation and det erinination of 2,2′diaminodibenzyl diphosphate have beeninvestigated in this paper.A method of base treatment of sample is applied.A column with 1%PEG-20M+1%KON on 301 enamel support is selected.1-Methyl-3, 5-diphenyl pyrazole is used as internal standard.Thecoefficient of variation of the method is 0.32%,The average recovery is 98.97%.     

Facile Synthesis of Liquid Crystal Dimers Bridged with a Phosphonic Group

Liquid crystal (LC) dimers with well-defined composition and structure arouse broad attentions for their exhibiting LC properties beyond conventional low molar mass mesogens and serving as fascinating model compounds for LC polymers. Here in this work, a series of LC dimers bridged with a phosphonic group have been synthesized through a facile free radical mediated addition reaction between hypophosphorous acid and vinyl terminated cyanobiphenyl mesogens with variant length alkyl spacers. In addition, two esterified derivatives and a group of mono-addition homologues with a terminal phosphonic acid group have also been prepared for comparison study. All the newly synthesized compounds exhibit monotropic nematic (N) phase with typical schlieren textures except for the LC dimer with the longest eleven-methylene spacer, which surprisingly shows twist-bend nematic (N_TB) phase directly from the isotropic state upon cooling. Moreover, the thermal transition properties such as the nematic-isotropic transition temperatures and associated entropy changes of the series LC dimers display a modest odd-even effect. Furthermore, both the LC dimers and the mono-addition homologues in N phase are quite easy to achieve homeotropic alignment upon annealing thanks to the supramolecular interactions between the introduced phosphonic acid group and the hydroxylated glass surface. This work thus provides a novel synthesis strategy for a class of LC materials bridged with a phosphonic acid group prone to further functionalization, which may serve as promising vertical alignment agents and pave the way for developing a new kind of functionalized LC materials of N_TB phase.     

Structural,electronic and catalytic performance of single-atom Fe anchored 3Si-doped graphene

By density functional theory (DFT) calculations, it is found that the single-atom Fe anchored three Si modified defective graphene (3Si-graphene-Fe) exhibits the high stability, and this system is semiconducting property and has non-magnetic moment. Besides the most stable configurations, electronic structures and magnetic properties of adsorbed species (O₂, CO, 2CO and CO/O₂) on 3Si-graphene-Fe systems are comparably discussed. The adsorption of O₂ is more stable than that of CO molecule and the coadsorption of 2CO and CO/O₂ has the larger adsorption energy than that of the isolated one. The adsorbed O₂, CO and CO/O₂ can induce the change in magnetic properties of 3Si-graphene-Fe system, and the coadsorbed CO/O₂ on system exhibits the metallic property. Among the reaction mechanisms, the CO oxidation reactions through Eley–Rideal (ER) reactions have lower energy barriers (<0.5?eV) than those of the Langmuir–Hinshelwood (LH) and new termolecular Eley–Rideal (TER) mechanisms, indicating that the ER reaction as starting step is an energetically favourable process. These results provide an important guidance on validating the catalytic activity of single atom on graphene-based materials.     

温敏性荧光纳米材料的合成

合成了以荧光材料罗丹明B/SiO2为核,交联聚N-异丙基丙烯酰胺(PNIPAM)为壳的具有核/壳结构的纳米颗粒。用氢氟酸除去二氧化硅模板核后,形成了核壳结构的温敏荧光微球。28～36℃范围内的温敏性实验表明,该粒子的低临界溶解温度(LCST)为33℃,具有温敏性,用SEM、TEM、XRD、FT-IR等手段对温敏荧光微球的组成和结构进行了表征和分析,探讨了磁性温敏纳米颗粒的制备机理。