煤直接液化油中混合酚的分离研究

利用分子筛择形特点，对煤直接液化油中的混合酚实施高效分离。本研究选取间甲酚和对甲酚作为分离煤直接液化油馏分段混合酚的模型化合物，采用化学液相沉积法对HZSM-5吸附剂的孔口结构进行改变，分析分子筛硅铝比及颗粒粒径对模型化合物间甲酚和对甲酚吸附分离性能的影响，以获得高性能固相吸附剂，并将其应用于180-190℃馏分段混合酚分离。结果表明，当分子筛硅铝比为25、粒径为3-5 μm时，分子筛的孔口结构调节效果最优；当正硅酸乙酯的最小用量为0.2 mL/g时，固相吸附剂的吸附量为0.03 g/g，对甲酚选择性高于95%。由于外表面沉积物对吸附剂的孔口结构变化，导致对甲酚选择性的提高。进一步采用HZSM-5（1）吸附剂对真实煤直接液化油混合酚的分离中发现，苯酚和对甲酚的选择性均达到100%。     

Polyvinylpyrrolidone and graphene-modified hematite nanoparticles for efficient electrocatalytic oxidation of p-nitrophenol

Journal of Solid State Electrochemistry - Polyvinylpyrrolidone (PVP) and graphene (G)-modified iron oxides (Fe2O3-PVP-G) are prepared by a simple hydrothermal reaction. Their morphology and...     

12β-Acetyloxyperforatin,a New Limonoid from Harrisonia Perforata

A new A, D-seco limonoid, named 12-acetyloxyperforatin (1), along with three known ones, were isolated from the leaves of Harrisonia perforata. Their structures were elucidated on the basis of spectroscopic analysis, including extensive NMR techniques and computational modelling. These compounds showed no inhibitory activity against the 11β-HSD1 enzyme.     

Finding any given 2‐factor in sparse pseudorandom graphs efficiently

Given an $n$‐vertex pseudorandom graph $G$ and an $n$‐vertex graph $H$ with maximum degree at most two, we wish to find a copy of $H$ in $G$, that is, an embedding $\phi :V\left(H\right)\to V\left(G\right)$ so that $\phi \left(u\right)\phi \left(v\right)\in E\left(G\right)$ for all $uv\in E\left(H\right)$. Particular instances of this problem include finding a triangle‐factor and finding a Hamilton cycle in $G$. Here, we provide a deterministic polynomial time algorithm that finds a given $H$ in any suitably pseudorandom graph $G$. The pseudorandom graphs we consider are $\left(p,\lambda \right)$‐bijumbled graphs of minimum degree which is a constant proportion of the average degree, that is, $\mathrm{\Omega }\left(pn\right)$. A $\left(p,\lambda \right)$‐bijumbled graph is characterised through the discrepancy property: $|e\left(A,B\right)?p|A||B||<\lambda \sqrt{|A||B|}$ for any two sets of vertices $A$ and $B$. Our condition $\lambda =O(p^{2}n/\log n)$ on bijumbledness is within a log factor from being tight and provides a positive answer to a recent question of Nenadov. We combine novel variants of the absorption‐reservoir method, a powerful tool from extremal graph theory and random graphs. Our approach builds on our previous work, incorporating the work of Nenadov, together with additional ideas and simplifications.     

Convergence of the viscosity solution of non-autonomous Hamilton-Jacobi equations

In this paper,we investigate the non-autonomous Hamilton-Jacobi equation ■ where H is 1-periodic with respect to t and M is a compact Riemannian manifold without boundary.We obtain the viscosity solution denoted by T_(t_0)~tφ(x) and show T_(t_0)~tφ(x) converges uniformly to a time-periodic viscosity solution u~*(x,t) of ?_tu+H(t,x,?_xu,u)=0.     

A Photoactivated Cu–CeO2 Catalyst with Cu-[O]-Ce Active Species Designed through MOF Crystal Engineering

Fully utilizing solar energy for catalysis requires the integration of conversion mechanisms and therefore delicate design of catalyst structures and active species. Herein, a MOF crystal engineering method was developed to controllably synthesize a copper–ceria catalyst with well-dispersed photoactive Cu-[O]-Ce species. Using the preferential oxidation of CO as a model reaction, the catalyst showed remarkably efficient and stable photoactivated catalysis, which found practical application in feed gas treatment for fuel cell gas supply. The coexistence of photochemistry and thermochemistry effects contributes to the high efficiency. Our results demonstrate a catalyst design approach with atomic or molecular precision and a combinatorial photoactivation strategy for solar energy conversion.     

Investigation of mononuclear,dinuclear, and trinuclear transition metal (II) complexes derived from an asymmetric Salamo‐based ligand possessing three different coordination modes

A new asymmetric Salamo‐based ligand H₂L was synthesized using 3‐tert‐butyl‐salicylaldehyde and 6‐methoxy‐2‐[O‐(1‐ethyloxyamide)]‐oxime‐1‐phenol. By adjusting the ratio of the ligand H₂L and Cu (II), Co (II), and Ni (II) ions, mononuclear, dinuclear, and trinuclear transition metal (II) complexes, [Cu(L)], [{Co(L)}₂], and [{Ni(L)(CH₃COO)(CH₃CH₂OH)}₂Ni] with the ligand H₂L possessing completely different coordination modes were obtained, respectively. The optical spectra of ligand H₂L and its Cu (II), Co (II) and Ni (II) complexes were investigated. The Cu (II) complex is a mononuclear structure, and the Cu (II) atom is tetracoordinated to form a planar quadrilateral structure. The Co (II) complex is dinuclear, and the two Co (II) atoms are pentacoordinated and have coordination geometries of distorted triangular bipyramid. The Ni (II) complex is a trinuclear structure, and the terminal and central Ni (II) atoms are all hexacoordinated, forming distorted octahedral geometries. Furthermore, optical properties including UV–Vis, IR, and fluorescence of the Cu (II), Co (II), and Ni (II) complexes were investigated. Finally, the antibacterial activities of the Cu (II), Co (II), and Ni (II) complexes were explored. According to the experimental results, the inhibitory effect was found to be enhanced with increasing concentrations of the Cu (II), Co (II), and Ni (II) complexes.     

Dimeric Manganese-Catalyzed Hydroarylation and Hydroalkenylation of Unsaturated Amides

An unprecedented Mn(I)-catalyzed selective hydroarylation and hydroalkenylation of unsaturated amides with commercially available organic boronic acids is reported. Alkenyl boronic acids have been successfully employed for the first time in Mn(I)-catalyzed carbon–carbon bond formation. A wide array of β-alkenylated amide products can be obtained in moderate to good yields, which offers practical access to five- and six-membered lactams. This protocol has predictable regio- and chemoselectivity, excellent functional group compatibility and ease of operation in air, representing a significant step-forward towards manganese-catalyzed C−C coupling.     

基于吸收系数的生脉注射液中聚山梨酯80含量测定新方法

聚山梨酯80又名吐温80，为一种亲水型非离子表面活性剂，是食品、保健品和药品中常用的辅料，作为增溶剂和澄清剂广泛用于中药注射剂。近年来，不良反应的发生使得聚山梨酯80的质量和应用愈加受到重视，有研究认为其加入可能引起注射剂不良反应增加。为避免超量使用，有必要对该辅料的投料加以严格控制。中药注射剂中聚山梨酯80的含量测定是当下研究的热点和难点，可以通过分光光度法、分子排阻-蒸发光散射检测法(SEC-ELSD)、液质联用法(LC-MS)直接测定，也可以水解后法经液相色谱-紫外检测法(HPLC-UV)或气相色谱法(GC)间接测定。但由于聚山梨酯80为聚氧乙烯聚合数目不同的混合物、不同厂家生产的聚山梨酯80化学组分及比例存在较大差异，难以采用统一的转换公式或对照品准确定量。此外，中药注射剂的复杂基质造成的假阳性干扰也对定量提出了挑战。为解决以上问题，以生脉注射液为例，提出基于吸收系数的中药注射剂中聚山梨酯80含量测定新方法。优化检测波长、显色剂种类、液液萃取过程振荡和静置时间，在6个不同品牌仪器上测得聚山梨酯80-硫氰酸钴配合物的吸收系数(E1%_{1 cm})为104.23，相对标准偏差(RSD)为2.08%。生脉注射液稀释10倍后，精密量取供试品溶液1.0 mL，精密加入硫氰酸钴溶液10 mL，二氯甲烷20 mL，涡旋振荡3 min。将混合液移至分液漏斗中，静置30 min，取下层二氯甲烷液，将前1 mL弃去，接收约15 mL，在320 nm处测定吸光度，再根据Lambert-Beer定律，利用获得的吸收系数计算得到聚山梨酯80的含量。方法阴性无干扰，精密度和重复性相对标准偏差均低于3%，平均回收率为98.42%。为进一步验证方法的准确性，分别采用吸收系数法和标准曲线法测定了2个厂家的10批生脉注射液，并与实际投料量比较。配对t检验结果表明，当置信度为95%时，两种方法无显著性差异，吸收系数法测得结果与企业生产中聚山梨酯的实际投料量也无显著性差异。研究采用前人未采用的、灵敏度更高的320 nm为检测波长，显著降低了基质干扰，克服了中药注射剂中聚山梨酯80测定结果与实际投料量难以吻合的问题。吸收系数法无需使用对照品，亦不用制备标准曲线，可为中药注射剂中聚山梨酯80的检查标准提供切实可行的解决方案。所建方法灵敏、准确、快速、简便，为含聚山梨酯80制剂的质量控制提供了关键常数及新的思路。