Optimization of an Alkaline Hydrolysis Preparation of Capilliposide-A from Lysimachia capillipes Hemsl. Using Response Surface Methodology Coupled with HPLC-ELSD Analysis

Capilliposide-A, a rare secondary saponin found in Lysimachia capillipes, has been reported to exhibit good biological activities. However, it is difficult to obtain a sufficient of capilliposide-A for further research through column chromatography and chemical synthesis. The aim of this work was to establish an efficient approach for the convenient preparation of this steroid saponin based on alkaline hydrolysis. The hydrolysis conditions were optimized by response surface methodology after a preliminary investigation of the affecting factors by single-factor experiments. Under the optimal conditions, the macroporous resin that adsorbed capilliposide-B and capilliposide-C was hydrolyzed in an 8% (w/v) NaOH solution at 35 °C for 65 h, and the yield of capilliposide-A was 68.90%. The results demonstrated that this newly developed approach is efficient for the preparation of capilliposide-A, and this approach is also crucial for further development and clinical applications.

     

Heterobimetallic Cluster-Based Coordination Polymers: Assembly,Structures and Third-Order Nonlinear Optical Properties

Reactions of (NH₄)₂WS₄ with CuCN, CuCN/1,2-bis(4-pyridyl)propane (bppa) or [Cu(MeCN)₄]PF₆/bppa under different reaction conditions afforded a set of two- or three-dimensional W/Cu/S cluster-based coordination polymers including {[Et₄N]₂[WS₄Cu₄(μ-CN)₂(μ-I)₂]}_n ( 1 ), [WS₄Cu₄(μ-CN)₂(bppa)₂]_n ( 2 ) and {[WS₄Cu₄(bppa)₄](PF₆)₂}_n ( 3 ), respectively. Compound 2 can be readily formed from reaction of 1 with bppa under solvothermal conditions. Compounds 1 and 2 feature two-dimensional networks with a “sql” topology, while 3 possesses a two-fold interpenetrated three-dimensional net with a rare “reo” topology. Compounds 1 – 3 in DMF exhibited different third-order nonlinear optical responses, and they all showed a reverse saturable absorption while 2 held a strong self-focusing effect.     

NiS助催化剂的硫调控光沉积合成及其增强g-C3N4的光催化产氢性能

作为一种非金属聚合半导体,石墨相氮化碳(g-C3N4)具有特殊的能带结构、可见光响应能力以及优良的物理化学性质以及生产成本低等特点,因而已成为目前光催化领域的研究热点.然而,由于g-C3N4被光激发的电子与空穴极易复合,导致g-C3N4材料的光催化性能并不理想.而助剂修饰是实现光生载流子有效分离以提高光催化活性的有效途径.众所周知,贵金属Pt可以作为光催化产氢的反应位点,但高昂的成本限制了它的实际应用.所以,开发高效的非贵金属助剂很有必要.近年来,NiS作为优良的电子助剂在光催化领域受到广泛关注.大量研究表明,NiS可以作为g-C3N4的产氢活性位点用于提高其光催化产氢性能.NiS助剂主要是通过水热、煅烧和液相沉淀的方法修饰在g-C3N4的表面上.相较而言,助剂的光沉积方法具有一些独特的优势,例如节能、环保、简易并且能够实现其原位牢固地沉积在光催化剂的表面.然而g-C3N4光生电子和空穴强还原和氧化能力容易导致像Ni^2+的还原和S^2-的氧化等副反应发生,因此NiS助剂很难光沉积在g-C3N4材料表面.本文采用硫调控的光沉积法成功合成了NiS/g-C3N4光催化材料,该法利用g-C3N4在光照条件下产生的光生电子结合S以及Ni^2+生成NiS,然后原位沉积在g-C3N4表面.由于E0(S/NiS)(0.096 V)比E0(Ni^2+/Ni)(-0.23 V)更正,所以NiS优先原位沉积在g-C3N4表面.因此,硫调控的光沉积法促进了NiS的生成,并抑制了金属Ni等副反应的形成.通过X射线光电子能谱分析NiS/g-C3N4的表面化学态,表明该方法能成功地将NiS修饰在g-C3N4的表面,这也得到透射电镜和高分辨透射电镜结果的证实.光催化产氢的结果表明,NiS/g-C3N4光催化剂实现了良好的光催化性能,其最优产氢速率(244μmol h^?1 g^?1)接近于1 wt%Pt/g-C3N4(316μmol h^?1 g^?1).这是因为硫调控的光沉积法实现NiS助剂在g-C3N4表面的修饰,从而促进光生电子与空穴的有效分离,进而提高光催化制氢效率.此外,在该方法中,NiS的形成通常在g-C3N4光生电子的表面传输位点上,因此也能够使NiS提供更多的活性位点以提高界面产氢催化反应速率.电化学表征结果也进一步证明NiS/g-C3N4光催化剂加快了电子与空穴的分离和转移.更重要的是,这种简易且通用的方法还可以实现CoSx,CuSx,AgSx对g-C3N4的助剂修饰,并且都提高了g-C3N4的光催化产氢性能,表明该方法具有一定的普适性,为高效光催化材料的合成提供了新的思路.     

Accelerated FeIII/FeII redox cycle of Fenton reaction system using Pd/NH2-MIL-101(Cr) and hydrogen

In this paper, a novel improvement in the catalytic Fenton reaction system named MHACF-NH₂-MIL-101(Cr) was constructed based on H₂ and Pd/NH₂-MIL-101(Cr). The improved system would result in an accelerated reduction in Fe^III, and provide a continuous and fast degradation efficiency of the 10 mg L^-1 4-chlorophenol which was the model contaminant by using only trace level Fe^II. The activity of Pd/NH₂-MIL-101(Cr) decreased from 100% to about 35% gradually during the six consecutive reaction cycles of 18 h. That could be attributed to the irreversible structural damage of NH₂-MIL-101(Cr).     

粉喷桩单桩承载力确定方法的比较

粉喷桩在高速公路软土地基处理中得到了广泛的应用,但其承载力的合理确定是工程实际中关心的一个重要问题。通过对工程中常用的几种粉喷桩单桩承载力确定方法的比较,分析了各自存在的问题和适用条件,提出了在实际工程应用中确定水泥搅拌桩单桩承载力的选用建议。     

MWCNTs复合物纳米流体的摩擦学性能

将油性剂油酸(OA)填充进多壁碳纳米管(MWCNTs)的空腔内制备复合物，再以复合物为添加剂制备一种纳米流体，考察了复合物的质量分数、MWCNTs的酸处理时间以及摩擦测试条件等对纳米流体摩擦学性能的影响，并分析了复合物的润滑机理. 结果表明:油酸被成功填充到经酸处理的MWCNTs管内，填充率约20%；摩擦过程中，复合物制备的纳米流体的摩擦系数有不断减小趋势，其减摩效果甚至优于同等含量的油酸乳化液；当复合物的质量分数为0.1%左右时，纳米流体可获得最佳的减摩、抗磨效果；随着酸化处理时间的增加，复合物制备的纳米流体的减摩、抗磨性能会有所提高. 摩擦过程中，复合物可释放出油酸并形成润滑膜，MWCNTs则能够在油酸形成的润滑膜上发挥“微轴承”的作用，从而使复合物获得更加优良的减摩、抗磨效果.      

Multi-multifractality,dynamic scaling and neighbourhood statistics in weighted planar stochastic lattice

The dynamics of random sequential partitioning of a square into ever smaller mutually exclusive rectangular blocks, which we call weighted planar stochastic lattice (WPSL), is governed by infinitely many conservation laws. Recently, we have shown one of the infinitely many conservation laws can be used as multifractal measure. In this article, we show that except the conservation of total area, each of the infinitely many non-trivial conservation laws is actually a multifractal measure and hence WPSL is a multi-multifractal. We then look at the block size distribution function and find that it exhibits dynamic scaling revealing that the spatial patterns of WPSL of different sizes are statistically self-similar. Besides, we investigate how the mean area ⟨A⟩_k of blocks with k neighbours and the average number of neighbours m_k of a typical cell that neighbours a k-sided block behaves with k. These results suggest that the Lewis law, ⟨A⟩_k∝k, is obeyed for up to k ≈ 8 and the Aboav–Weaire law, km_k∝k, is violated for the entire range of k.     

Amine Salt–Catalyzed Synthesis of 5-Substituted 1H-Tetrazoles from Nitriles

The [3 + 2] cycloaddition reaction between sodium azide and various organic nitriles proceeds smoothly in the presence of amine salts as catalyst in dimethylformamide. The corresponding 5-substituted 1-H tetrazoles were obtained under mild condition in good to excellent yields. Supplemental materials are available for this article. Go to the publisher's online edition of Synthetic Communications® to view the free supplemental file.     

基于二氧化硅球腔微电极阵列的过氧化氢生物传感器制备

以聚苯乙烯(PS)微球阵列为模板,采用溶胶-凝胶法在氧化铟锡( ITO)电极上制备了二氧化硅(SiO2)球腔阵列,扫描电镜显示此方法制备的SiO2球腔阵列高度有序.电化学研究结果表明,该球腔阵列的循环伏安曲线符合微电极阵列的电化学特点.将血红蛋白(Hb)作为氧化还原模型蛋白直接吸附于球腔内,制得电流型过氧化氢(H2O2...     

Fourier transforms on Cantor sets: A study in non-Diophantine arithmetic and calculus

Fractals equipped with intrinsic arithmetic lead to a natural definition of differentiation, integration, and complex structure. Applying the formalism to the problem of a Fourier transform on fractals we show that the resulting transform has all the required basic properties. As an example we discuss a sawtooth signal on the ternary middle-third Cantor set. The formalism works also for fractals that are not self-similar.