竹叶提取物对铝在HCl溶液中的缓蚀作用

用不同浓度的C₂H₅OH（体积分数：20%-80%）从金竹竹叶中提取制备出竹叶缓蚀剂（简称为PSLE）,用紫外-可见（UV-Vis）光谱和傅里叶变换红外（FTIR）光谱对其进行了表征,并对总黄酮含量进行了测定. 采用失重法、动电位极化曲线、电化学阻抗谱（EIS）和扫描电子显微镜（SEM）研究PSLE在HCl 介质中对铝的缓蚀作用.采用量子化学密度泛函理论（DFT）研究了两个主要竹叶黄酮成分牡荆苷和异牡荆苷的吸附方式. 结果表明：PSLE对铝具有良好的缓蚀作用,且在铝表面的吸附符合Langmuir 吸附等温式. 缓蚀率随其浓度的增加而增大,但随温度的升高和盐酸浓度的增加而降低. 竹叶总黄酮含量和竹叶缓蚀剂的缓蚀性能有良好的相关性,初步推测竹叶缓蚀剂的有效成分主要为竹叶黄酮类化合物. PSLE为阴极抑制型缓蚀剂;EIS 在高频区呈容抗弧,在低频区呈感抗弧,添加PSLE后,阻抗值显著增大. SEM表明添加PSLE对铝的腐蚀产生了明显的抑制作用.量子化学计算结果表明,牡荆苷和异牡荆苷的吸附中心主要集中在竹叶黄酮骨架（FBS）.     

Synthesis of 1‐Methyl‐3‐aryl‐substituted Titanocene and Zirconocene Dichlorides and Crystal Structure of Bis[η5‐1‐methyl‐3‐(α, α‐dimethylbenzyl) cyclopentadienyl] titanium Dichloride

The syntheses of a series of l‐methyl‐3‐aryl‐substituted titanocene and zirconocene dichlorides are reported. These complexes are synthesized by the reaction of 2‐ and 3‐methyl‐6, 6‐dimethylfulvenes (1:4) with aryllithium, followed by the reaction with TiCl₄·2THF, ZrCl₄ and (CpTiCl₂)₂O respectively, to give complexes 1–5. The complex [η⁵‐1‐methyl‐3‐(α, α‐dimethylbenzyl) cyclopentadienyl] titanium dichloride has been studied by X‐ray diffraction. The red crystal of this complex is monoclinic, space group P2_t/C with unit cell parameters: a =6.973(6) × 10^?1 nm, b =36.91(2) × 10^?1 nm, c = 10.063(4) × 10^?1 nm, α=β= γ = 93.35(5)°, V = 2584(5) × 10^?3 nm³ and Z = 4. Refinement for 1004 observed reflections gives the final R of 0.088. There are four independent molecules per unit cell.     

3,9‐Bis(dicyanomethylene)‐2,4,8,10‐tetrathiaspiro[5.5]undecane

The title compound, 2,2′‐(2,4,8,10‐tetra­thia­spiro­[5.5]­undec­ane‐3,9‐diyl­idene)­bis­(propane­di­nitrile), C₁₃H₈N₄S₄, has been designed and synthesized for use as a potential new organic molecular electronic material. The spiro‐annulated structure has twofold symmetry and is formed by two equal push–pull ethyl­ene units, with the cyclo­alkyl­thio groups as electron donors and the cyano groups as electron acceptors. The intermolecular S?N non‐bonded separation within a layer in the lattice is 3.296 (6) Å, indicating a strong intermolecular interaction between the cyano groups and the S atoms, while the S atoms in two neighbouring mol­ecules have a shortest S?S contact of 3.449 (3) Å. In addition, attractive C—H?N and C—H?S interactions bridge adjacent mol­ecules either within a layer or between layers. In short, these four types of intermolecular interactions combine to form an extended three‐dimensional network in the lattice, resulting in a highly ordered array of molecular packing.     

固相氯化法合成氯化聚乙烯的红外光谱研究

本文研究在不同条件固相氯化聚乙烯(CPE)的红外光谱,探讨了一步和两步氯化合成的CPE的结构差别,着重讨论了两步氯化的CPE结构特点。从观察表征结晶结构和—(CH_2)_n—链段氯分布的特征频率变化表明,低温固相氯化主要发生在无定形区,并且在CPE中形成高氯化和低氯化链段(或未氯化)的嵌段结构。在两步固相氯化时,晶区受到较大程度的破坏,氯化作用已不局限在无定形区,其结晶结构的破坏主要同第二步氯化程度有关,即使CPE氯含量相同,若前后两步氯化程度不同,结构有很大差异。     

~(13)C-NMR STUDY ON THE CHAIN TERMINAL STRUCTURE OF POLY-1,3-PENTADIENE POLYMERIZED WITH RARE EARTH CATALYST

The sequence distribution and the terminal structures of poly-1,3-pentadiene chains obtained by rare earth catalyst and effect of polymerization temperature on microstructure of the polymer have been investigated by ~(13)C-NMR method. According to experimental results it was supposed that terminal active growing chain of the polymer would be four types of anti- and syn-η~3-allyl structures. When polymerization temperature was reduced, the content of cis-1,4-poly-1,3-pcntadiene increases. It can be explained by isomerization between anti- and syn-η~3-allyl. The process forming trans-1,2 unit instead of 3,4-unit were also described.     

圆二色谱中的激子手性法在有机化学中的应用

激子手性法是圆二色谱领域内,近一、二十年内发展的一种测定有机化合物绝对构型的可靠方法。本文对其基本原理及规律作一简要介绍。并以邻二醇、共轭烯酮,共轭二烯及丙烯醇为例,介绍本法在测定绝对构型中的应用。此外,本法也可用于糖类的结构研究。     

热脱附-气相色谱质谱分析热环境下汽车沙发释放的挥发性有机物

汽车沙发部件在热环境中,会释放出许多挥发性有机物(VOC),污染环境,危害人体健康.本研究将汽车沙发放置在2 m3特制塑料采样袋中,在热环境下释放挥发性有机物,然后以Tenax管富集有机物,用热脱附-气相色谱质谱进行分析.结果表明:汽车沙发在热环境状态下,挥发出大量有机物,共定性检测出49种挥发性有机物(VOC),包括...     

Polyfluorenes containing pyrazine units:Synthesis,photophysics and electroluminescence

A series of conjugated copolymers of 9,9-dioctylfluorene and symmetrical pyrazine unit (BY) were synthesized by Suzuki copolymerization and were used as novel light-emitting materials in PLEDs.Efficient energy transfer was observed in both thin film and solution.Compared with the lowest occupied molecular orbital (LUMO) energy level of the polyfluorenes homopolymer (PFO),the lower LUMO energy levels of copolymers indicated that the introduction of the BY unit would be benefit to electron injection.The turn-...     

食品中铝检测方法研究进展

介绍了食品中铝的来源,并综述了近十年中食品中铝测定方法的研究进展,包括电感耦合等离子体原子发射光谱法、电感耦合等离子体质谱法、石墨炉原子吸收光谱法、电化学分析法以及分光光度法等方法(引用文献75篇)。     

疏水/亲水大孔聚二乙烯基苯/聚(N-2-氨基乙基丙烯酰胺)IPN树脂的合成及对水杨酸吸附性能研究

采用分步悬浮聚合法制备了聚二乙烯基苯/聚丙烯酸甲酯(PDVB/PMA)大孔互穿聚合物网络,将其中的聚丙烯酸甲酯用乙二胺氨解,合成了具有疏水/亲水性能的聚二乙烯基苯/聚(N-2-氨基乙基丙烯酰胺)(PDVB/PNAEAM)大孔互穿聚合物网络(IPN);测定了该树脂的孔结构、含水量、弱碱交换量和溶胀性能;测定了该树脂对水杨酸在不同温度下的吸附等温线,利用热力学函数关系计算出了吸附焓、自由能和熵.推测PDVB/PNAEAM IPN树脂中疏水性的PDVB一网具有疏水作用吸附能力、亲水性的PNAEAM一网具有氢键作用吸附能力.动态吸附及脱附实验表明湿态PDVB/PNAEAM IPN树脂对水溶液中水杨酸的饱和吸附量达到46.1mg/mL.树脂可以通过4%NaOH溶液再生.PDVB/PNAEAM IPN树脂在分离工业废水中水杨酸等芳香有机酸有良好的应用前景.