胺催化下的Baylis-Hillman反应

Baylis-Hillman (B-H)反应是在催化剂作用下由活泼烯烃和亲电试剂发生的偶合反应, 其产物是一个具有多官能团的化合物. 胺类催化剂是反应中应用最广泛的一类催化剂. 综述了各种胺催化下的Baylis-Hillman反应的研究进展.     

LBL分子沉积法制备葡萄糖氧化酶电极

采用以静电力为主的逐层分子交替沉积技术制备葡萄糖氧化酶（GOD）电极.通过带有正电荷的聚二甲基二烯丙基铵盐酸盐（PDDA）和带有负电荷的GOD交替沉积在修饰有3-巯基-1-丙基磺酸钠（MPS）的金电极表面.以甲酸二茂铁为电子媒介体,用循环伏安法检测GOD电极对葡萄糖的响应.结果表明,当GOD电极组装层数小于4时,电流响应随着层数的增加而增大,超过4层时电流响应减小.其中4层GOD修饰电极的线性范围为0.55～6.63 mmol•L－1,当pH为7.0时,响应最大.同时电极的检测重现性能良好,相对标准偏差为2.4％.     

室温制备高合金化Pt-Ru/CMK-3催化剂及其对甲醇的电催化氧化

通过低温络合反应制备了高分散高合金化的Pt-Ru固溶体, 并将其均匀地担载在有序介孔碳CMK-3上, 以形成二元复合金属催化剂. XRD谱图表明,fcc结构的Pt原子部分被hcp结构的Ru原子取代形成置换固溶体， 而且几乎没有未形成合金的Ru存在. TEM和XRD研究结果表明， Pt-Ru/CMK-3催化剂中Pt-Ru合金粒子的平均粒径为27 nm, 且具有良好的均一度. 还研究了催化剂对甲醇的电催化氧化性能, 并与E-TEK公司同类催化剂进行了对比, 研究结果表明, Pt-Ru/CMK-3催化剂具有较大的电化学活性面积, 对甲醇的电催化氧化性能和抗CO中毒能力明显优于其它同类催化剂.     

Reduction and reconstruction of Co3O4 nanocubes upon carbon deposition

We describe a synthetic investigation on the formation of carbon nanofibers using a preshaped free-standing metal-oxide catalyst (single-crystal cobalt oxide (Co(3)O(4)) nanocubes). In reacting with acetylene (C(2)H(2)) vapor, Co(3)O(4) nanocubes are reduced and reconstructed into metallic cobalt. The resultant metal catalyst with a 2-fold symmetry leads to a bilateral base growth for carbon nanofibers. Our findings indicate that an understanding of catalyst-assisted chemical vapor deposition (CVD) mechanisms can be acquired, when the shape, size, and crystal orientation of pristine metal catalysts are made known to the CVD process. By tracing their evolutional changes in structure and composition, the shape-designed model catalysts may offer new opportunities for mechanistic investigations on the chemical reactivity of nanoparticles, general catalyst-assisted material synthesis, and metal intercalation chemistry.     

Synthesis and Crystal Structure of a Tetranuclear Silver Complex with Bis（diphenylphosphino） amine-dioxide as a Tridentate Ligand

1 INTRODUCTION The coordination chemistry of the nitrogen-contai- ning diphosphine ligand bis(diphenylphosphino)ami- ne (Ph2PNHPPh2) has recently received much atten- tion because the P atoms can bridge metal centers in μ-bonding mode to form bi- or polynuclear complex- es[1~10]. It has been shown that the acidity of N–H proton would promote functionalization on the ligand backbone[4, 5, 11]. Although a few complexes contain- ing deprotonated tridentate Ph2PNPPh2 have been synthesi…     

高频燃烧红外吸收光谱法测定钨钛合金中碳含量

建立高频燃烧红外吸收光谱法测定钨钛合金中碳含量的分析方法。在1980 W分析功率下,称取0.3 g样品,以2.0 g钨锡及0.5 g纯铁混合助熔,用高频红外分析仪测定碳。碳的含量在0.013%~0.050%范围内与红外吸收峰面积线性相关,相关系数为0.9993。碳的测定下限为3.6μg/g,方法检出限为1.08μg/g。该法测定结果的相对标准偏差为2.97%~4.11%(n=8),碳的加标回收率为96.2%~103.1%。该方法能够满足合金中碳含量的分析要求。     

液晶聚酯与环氧嵌段共聚物的合成及表征

近年来 ,人们利用高分子液晶作为热固性环氧树脂的改性剂 ,不仅可以提高环氧树脂的韧性和强度 ,而且可以改善其热性能 ,为制备高性能的环氧树脂提供了一条新的途径[1,2 ] .目前报道所使用的液晶聚合物大多为液晶聚酯[3 ] 或液晶性聚氨酯[4] ,这些液晶聚合物与环氧树脂由于存在相容性不好的问题 ,给其实际应用带来了困难 .为了改善二者的相容性 ,本文采用溶液法合成了末端带有反应活性基团的聚酯型液晶聚合物 ,将它再与双酚Ａ环氧预聚物反应 ,制得了高分子液晶环氧嵌段共聚物 ,其合成路线如下 :2ＨＯＣＯＯＣＨ3+ ＨＯ(ＣＨ2 ) 6 ＯＨ　　Ｈ…     

Dienone—phenol Rearrangement of C—9 Oxygenated Decalinic Dienone and Analogs through B—Ring Cleavage

Dehydrogenation of 9-hydroxy decalinic enones and analogs with DDQ resulted in a formal dienone-phenol type rearrangement via B-ring cleavage, while the corresponding dienone acetates underwent base-catalyzed formal dienone-phenol type rearrangement analogously.     

Cu2(μ-dppb)2(μ-Cl)2的合成、晶体结构及非线性光学性质

The complex Cu₂(μ-dppb)₂(μ-Cl)₂ has been synthesized from the reaction of CuCl， dppb and (n-Bu)₄NCl. The crystal belongs to the triclinic with space group P1. The unit cell parameters are: a=9.939(4)?， b=10.083(6)?， c=14.104(5)?， α=76.46(3)°， β=71.02(2)°， γ=70.87(5)°. The single crystal X-ray diffraction analysis reveals that it has a bi-ring structure with a symmetry center at the middle of two Copper atoms. The outer ring is a 14-membered ring of Cu-dppb-Cu-dppb， and the inner ring is a 4-membered ring composed of two Cl^- and two Cu(Ⅰ). Investigation of third-order optical nonlinearity shows that it exhibits considerable nonlinear absorptive and self-defocusing effect with α₂=1.75×10^-13m·W^-1 and n₂=3.19×10^-18m²·W^-1. CCDC: 193113.     

Synthesis and magnetic properties of poly(p‐phthaloyl‐disacetylaceton‐ethylenediimine) metal complexes

Macrocyclic Schiff‐base ligand, bisacetylaceton‐ethylenediimine (BAE) and its transition metal complexes M(BAE) (M = Cu²⁺, Ni²⁺) were synthesized. The complexes having characteristics of aromatic systems and well‐defined one‐dimensional structures, reacted with p‐phthaloyl chloride, to obtain polymer complexes. The complexes were characterized by elemental analysis, inductively coupled plasma (ICP), FT‐IR, and thermal analysis and show good thermal stability. ESR spectra analysis discovered that there are free radicals in the chain of polymers, indicating that a weak magnetic spin‐exchange interaction operates between the metal ions and free radicals. It is found that, as the bridging p‐phthaloyl group is able to propagate the magnetic exchange interaction, the polymer complexes show paramagnetic properties by measurement of temperature dependence of the magnetic property, and obey Curie–Weiss law. Copyright © 2001 John Wiley & Sons, Ltd.