Synthesis of naphthyridines and phenanthrolines using catalysts based on transition and rare-earth metals

Liquid-phase condensation of 3-, 4-, and 8-aminoquinolines with aliphatic and aromatic aldehydes catalyzed by transition and rare-earth metal complexes is an efficient method for synthesis of substituted 1,7- and 1,6-naphthyridines and 1,10-phenanthrolines.Institute of Organic Chemistry, Ural Branch, Russian Academy of Sciences, 450054 Ufa; Eastern Scientific-Research Institute of Coal Chemistry, 620219 Sverdlovsk. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 5, pp. 1139–1148, May, 1992.     

氮杂冠醚研究Ⅶ、双仲胺型氮杂冠醚对过渡金属离子的选择性萃取作用

合成了五种新型双仲胺型氦杂冠醚，研究了它们对过渡金属离子进行液—液萃取，并用原子吸收法测定其浓度。实验结果表明：这类冠醚对Ａｇ￣＋、Ｐｄ￣（２＋）、和Ｐｔ￣（４＋）等贵金属离子有较强的选择配位性能，对选择性分离这些金属离子有重要的意义。     

Protection of immobilized sulfhydryl groups against autooxidation by alterations in their microenvironment

Immobilized sulfhydryl groups were prepared by partial thiolation of NH₂-glass beads. The microenvironment of the immobilized SH groups was varied by different chemical modifications of neighboring NH₂ groups. Introduction of a strong charge in the surroundings of immobilized sulfhydryls results in their dramatic stabilization against autooxidation. This effect is due to the salting of O₂ from the surface microlayer of the thiolated beads.     

Formation of Bi-Sb, Bi-Sn, and Bi-Sb-Sn Nanoclusters in Silica Xerogel Matrices from Mixed-Metal Oxide Precursors

Homogeneous mixed-metal oxides of the general formula (Bi/E/Si)O _x , where E represents a dopant element (E=Sb, Sn, or Sb/Sn), can be prepared using typical sol-gel processing techniques. Reduction of the in-situ Bi(III) and E ions by hydrogen affords nanocomposites of Bi-Sb, Bi-Sn, or Bi-Sb-Sn widely dispersed throughout the silica xerogel matrix. The materials prepared have high Bi-E metal loading of 52–60 wt. % containing Bi-E alloy nanoclusters of 12–15 nm average diameter. These results demonstrate a convenient method for the production of practical quantities of nanostructured bismuth alloy ceramic composites at high metal content.     

晋江市潮间带底质,生物体中重金属含量及其分布特征

研究福建省晋江市潮间带底质、生物体内重金属含量的分布特征及其主要影响因素．结果表明：表层底质重金属除总Ｈｇ之外,Ｃｕ、Ｐｂ、Ｃｄ和总Ｃｒ含量在河口、半封闭海湾明显高于紧临台湾海峡的海湾及开敞海区,并且,近年来底质的这些重金属含量大多数呈递增趋势;底质的重金属除总Ｈｇ之外,其他的含量都与底质类型及有机质含量有较好的相关性;３种经济贝类对重金属的富集能力分别为：牡蛎,缢蛏和蛤对Ｃｕ的富集系数分别为ｎ×１０４,ｎ×１０３和ｎ×１０３;３种贝类对Ｐｄ和Ｃｄ的富集系数均为ｎ×１０２．     

环己酮-水分离新方法的研究

针对工业上传统的蒸馏法分离环己酮－水体系能耗过大的问题,研究了含盐类的复合萃取剂对该体系的萃取分离效果。结果表明,ＬｉＣｌ、ＭｇＣｌ２能明显改变环己酮与水之间的互溶度,大幅度提高复合萃取剂对组分的萃取分配系数和选择性系数,达到分离提纯环己酮的目的。进一步研究了萃取工艺参数对分离效果的影响。经初步热量衡算表明：应用本法分离环己酮－水比传统的蒸馏法节省能耗约２５％。     

气相生长碳纤维的制备

以苯和氢气为原料在石墨,陶瓷等基板表面催化热解制取低成本,高性能的气相生长碳纤维（ＶＧＣＦ）,实验考察了催化剂类热解温度、热解时间,苯带入量,载气,基板材料等参数对ＶＧＣＦ生长情况及性能的影响,并提出了碳纤维的生长机理。结果表明,在合适条件下,用直接播种法制得的ＶＧＣＦ直径为０．７￣１０μｍ,长度为１￣５μｍ,采用金属原子溅射沉积的基板可得到均匀稠密的ＶＧＣＦ,直径为３￣８０μｍ,碳纤维的生长过程     

Determination of heavy metal concentration in feed and permeate streams of polymer enhanced ultrafiltration process

Polymer enhanced ultrafiltration (PEUF) is a newly developed method for the removal of heavy metals from aqueous solutions. This method was applied for the removal of mercury and cadmium with the presence of polyethyleneimine (PEI) as a water soluble polymer. After ultrafiltration experiments for metal–polymer mixtures, two separate streams, namely, retentate and permeate, former of which contains mainly metal–polymer complex and free polymer molecules while latter of which mainly contains free metal ions, were obtained. At the end of PEUF experiments, performance of operation was determined by concentration analyses which was achieved by atomic absorption spectroscopy (AAS) applied in a different way for permeate and retentate streams considering the effect of presence of polymer. For mercury analysis, cold vapor AAS was applied. It was observed that the presence of PEI did not affect the atomic absorption signal when 10% HCl was added to the sample solutions. For calcium and cadmium, flame AAS was used. It was observed that change in PEI concentration results in change in measured concentration of calcium and cadmium. Therefore, two new approaches were developed for accurate measurement of concentrations of calcium and cadmium. It was also observed that presence of other metals did not affect the accuracy of the measurement of a particular metal in the concentration range studied.     

5－（4－乙酰氧基苯基），10，15，20－三苯基卟啉金属配合物修饰的铂支撑双层脂膜的IV性质

合成并表征了５－（４－乙酰氧基苯基），１０，１５，２０－三苯基卟啉及其金属配合物，将它们作为修饰物，制得铂支撑的双层脂膜，用循环伏安法研究了抗坏血酸的氧化还原反应，并对其机理作了探讨。     

Oxidative coupling of malononitrile with formation of 1,1,2,3,3-pentacyanopropene salts

A simple and convenient route for the synthesis of 1,1,2,3,3-pentacyanopropene salts is reported. These salts are formed by interaction of malononitrile with SeO₂ in presence of organic N-containing bases or pyridinium salts.