杂环苄基锡二氨基硫脲席夫碱配合物的合成

二氨基硫脲与芳香醛(酮)反应,合成了3个三齿Schiff碱配体;配体与二苄基二氯化锡或三苄基氯化锡反应合成了6个未见文献报道的三齿配体杂环有机锡(Ⅳ)配合物,其结构经1H NMR, IR和元素分析表征.     

双烷基及双（β－烷氧羰乙基）锡聚胺的合成及性质的研究

利用界面缩聚技术，将二烷基或二（烷氧羰已基）二氯化锡与有机二胺反应，制成了５８种有机锡聚胺大分子化合物，研究了部分聚胺对ＰＶＣ树脂热稳定性的影响，取得了有意义的结果。     

混合二烃基二氯化锡与2-羟基-1-萘醛缩苯胺类席夫碱配合物的合成与表征

由混合二烃基二氯化锡 (RR′Sn Cl2 )与 2 -羟基 - 1 -萘醛缩苯胺类席夫碱反应 ,合成了 1 8种新的有机锡配合物。经元素分析 ,IR、1 H NMR、1 3 C NMR和 TG- DSC测定 ,确认配合物为有机锡与席夫碱的 1 2 1加成物 ,配体以酚羟基氧原子和锡原子配位。     

混合二烃基二氯化锡与2-羟基-1-萘醛缩苯胺类席夫碱配合物的合成与表征

由混合二烃基二氯化锡(RR′SnCl₂)与2-羟基-1-萘醛缩苯胺类席夫碱反应,合成了18种新的有机锡配合物。经元素分析,IR、¹H NMR、¹³CNMR和TG-DSC测定,确认配合物为有机锡与席夫碱的121加成物,配体以酚羟基氧原子和锡原子配位。     

双烷基及双（β—烷氧羰乙基）锡聚铵的合成及性质的研究

利用界面缩聚技术，将二烷基或二（烷氧羰乙基）二氯化锡与有机二胺反应，制成了５８种有机锡聚胺大分子化合物，研究了部分聚胺对ＰＶＣ树脂热稳定性的影响，取得了有意义的结果。     

杂环苄基锡氨基硫脲席夫碱配合物的合成与表征

二苄基二氯化锡和三苄基氯化锡分别与水杨醛缩氨基硫脲,含羟基芳香醛(酮)缩氨基硫脲的席夫碱钠盐反应,合成了10种新的有机锡配合物,其结构经1H NMR,119Sn NMR,IR和元素分析表征。结果表明,中心锡原子均为五配位杂单环结构。     

含杂环羧酸基二苄基锡(Ⅳ)配合物的合成与表征

以二苄基二氯化锡和杂环羧酸钠为原料合成了十种新的有机锡配合物(PhCH₂)₂Sn(O₂CR)_nCl_2-n(n=1或2，R=杂环)。用元素分析、IR、 ¹H NMR和TG表征了配合物的组成和结构。     

混合二烃基二氯化锡与水杨醛缩苯胺类Schiff碱配合物的合成和表征

由混合二烃基二氯化锡与水杨醛缩苯胺类Schiff碱反应,合成了24种新的有机锡配合物。经元素分析、NMR、TG-DSC测定和X射线粉末衍射分析,确定有14种是有机锡与Schiff碱的1:1配合物,10种是1:2配合物。配体是以酚羟基氧原子与锡原子配位,摩尔电导率测定表明这些配合物均为非电解质。     

气相色谱-质谱法同时测定聚氯乙烯塑料制品中的10种有机锡化合物

采用气相色谱-质谱法(GC-MS)同时快速有效地测定了聚氯乙烯（PVC）塑料制品中的二丁基氯化锡、单丁基氯化锡、三乙基氯化锡、三苯基氯化锡、三丁基氯化锡、三丙基氯化锡、二苯基氯化锡、四丁基锡、二辛基氯化锡和单苯基氯化锡等10种有机锡化合物。使用四氢呋喃溶解PVC样品,甲醇沉淀样品中的聚合物,超声萃取其中的有机锡化合物,将提取液衍生化后用正己烷萃取,采用GC-MS总离子流和选择离子进行定性定量测定。对衍生化时间、衍生化pH值、衍生化试剂用量、沉淀试剂用量等样品前处理条件进行了优化,并进行了线性关系、回收率、精密度等考察。结果表明,方法的线性范围为0.5～50 mg/L,线性相关系数为0.9978～0.9997。10种有机锡化合物的回收率及相对标准偏差(n=9)分别为84.23%～109.1%和4.24%～10.75%。所建立的方法能很好地应用于PVC塑料制品中有机锡化合物的检测。     

三苄基锡二硫代氨基甲酸酯的合成

三苄基锡二硫代氨基甲酸酯的合成尹汉东马春林＊张如芬（聊城师范学院化学系聊城２５２０５９）关键词三苄基氯化锡，二硫代氨基甲酸盐，合成１９９７－０７－１０收稿，１９９７－０９－０９修回山东省自然科学基金资助项目三烃基锡衍生物是一类具有较强生物活性的有机锡...     

Synthesis and properties of soluble,fluorescent polyesters and polyethers with substituted m‐terphenyl segments in the main chain

A new series of rigid polyesters and semiflexible polyethers were synthesized from 4,4″‐dihydroxy‐5′‐phenyl or anthracenyl‐m‐terphenyl. The polymers were characterized by viscometry, Fourier transform infrared, NMR, X‐ray, differential scanning calorimetry, thermomechanical analysis, thermogravimetric analysis, ultraviolet–visible, and luminescence spectroscopy. The polyesters were amorphous, whereas some of the polyethers showed a low degree of crystallinity. All the polymers displayed an enhanced solubility even in 1,1,2,2‐tetrachloroethane and tetrahydrofuran. The glass‐transition temperatures were 123–146 °C for the polyesters and 45–117 °C for the polyethers. The polymers were stable up to 213–340 °C and afforded anaerobic char yields of 36–62% at 800 °C. Their optical properties were investigated both in solution and in the solid state. They showed ultraviolet fluorescence, violet‐blue fluorescence, or both with emission maxima at 333–487 nm. The polymers with anthracenyl pendent groups exhibited higher fluorescence quantum yields and emission maxima redshifted compared with the corresponding polymers with phenyl pendent groups. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 2381–2391, 2000     

Pyrolyse-gas-chromatographische und pyrolyse-massenspektrometrische Untersuchungen an polymeren Kronenethern

Zusammenfassung Pyrolyse-Gas-Chromatographie und Pyrolyse-Massenspektrometrie dienen zur Charakterisierung erstmalig hergestellter Polymeren mit Polyethern als Ankergruppen. Zu den untersuchten Polymeren gehören: mit cyclischen Polyethern und nichtcyclischen Ethern substituiertes Polystyrol, mit cyclischen Polyethern substituiertes Kieselgel und Polykondensate, hergestellt aus cyclischen Polyethern und Vernetzern. Die Pyrolyse-Gas-Chromatogramme zeigen für den jeweiligen Polymertyp charakteristische Spektren und gestatten eine eindeutige Zuordnung der Art der Matrix und Ankergruppen sowie der Verknüpfung von Ankergruppe und Matrix. Die Pyrolyse-Massenspektren liefern schnelle qualitative Aussagen über Zusammensetzung und pyrolytisches Abbauverhalten der Polymeren. Mit den vorliegenden Ergebnissen kann der Syntheseweg von Polymeren mit cyclischen Polyethern als Ankergruppen beurteilt und gegebenenfalls modifiziert werden. Auch eine einfache Identifizierung unbekannter Polymeren ist möglich.

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Pyrolysis gas-chromatographic and pyrolysis mass-spectrometric examinations of polymeric crown ethers

Summary Pyrolysis gas-chromatography and pyrolysis mass-spectrometry are useful to characterize polymers with polyethers as anchor groups, which are synthesized for the first time. The analysed polymers are: polystyrene substituted with cyclic polyethers and non-cyclic ethers, silica gel substituted with cyclic polyethers and polycondensates synthesized from cyclic polyethers and cross-linking reagents. The pyrolysis gas-chromatograms show characteristic spectra for the respective type of polymer and make possible a definite classification of the type of the matrix and anchor groups as well as of the cross-linking of anchor group and matrix. Pyrolysis mass-spectra provide rapid qualitative information on composition and thermal breakdown mechanism of the polymers.The results given allow the evaluation of the efficiency of the synthesis way used for polymers with cyclic polyethers as anchor groups and may be used to modify the syntheses. They also allow a simple identification of unknown polymers.

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Für finanzielle Unterstützung danken wir der Deutschen Forschungsgemeinschaft, Bonn-Bad Godesberg.     

Synthesis and characterization of fluorine-containing aromatic polyethers from tetrafluoroisophthalonitrile and bisphenols

New aromatic polyethers having inherent viscosities of 0.43–0.91 dL/g were synthesized by the phase-transfer catalyzed polycondensation of tetrafluoroisophthalonitrile with various hisphenols in a nitrobenzene-water system. All the polyethers were amorphous and soluble in N-methyl-2-pyrrolidone and nitrobenzene. They were cast into transparent and flexible films from the solutions. These polymers had glass transition temperatures around 130°C and dia not lose weight below 400°C in either air or nitrogen.     

同时溶解和ICP-AES同时测定焊锡材料中的铅、锡和银

铅锡银合金被广泛应用在焊料、耐磨合金等领域,对它们的检测目前主要有容量法[1]、原子光谱法[2,3]等。在该合金分析中,样品中铅锡银的溶解是分析中最重要的步骤,目前常用的样品溶解方法有:稀王水溶解铅锡法[2]、浓硫酸浓硝酸溶解锡银法[1]、稀硝酸溶解银法[4]。无论哪一种样品     

含茋生色团聚醚的合成与热致液晶行为

β 氯乙基缩水甘油醚 (GCE)和GCE/羟丁基乙烯基醚 (HBVE)分别通过阳离子聚合、光引发共聚合 ,获得两种聚醚 ,然后再分别与 4 硝基 4′ 羟基 (NHS)反应 ,制备了两种侧链含生色团的液晶聚合物(PSEG、PSV) .用FTIR、1H NMR和EA对其化学结构及生色团含量进行了表征 ,以POM、DSC、TGA和WAXD对聚合物介晶相转变温度、织构、热稳定性及相行为进行了研究 .结果表明 ,这类聚合物属向列型热致双向性液晶 ,液晶相转变温度较低、范围较宽 ;聚合物热稳定性较好 ,开始分解温度在 30 0℃以上 .     

锡石墨炉原子化机理研究

本文考察了盐酸、硫酸、硝酸、亚硒酸及硼酸中锡的石墨炉原子吸收特性,对锡在不同基体中的原子化过程进行了初步探讨。发现硼酸是石墨炉法测定锡时的一种较好的化学改进剂;1%的硼酸加入可克服一定含量的硫酸与盐酸的干扰。并利用XRD与XPS对硼酸与锡共存时的石墨表面进行了结构与状态分析。提出了硼酸与锡共存时,锡的原子化历程。     

Biodegradable and Biocompatible Silatrane Polymers

In this study, new biodegradable and biocompatible amphiphilic polymers were obtained by modifying the peripheral hydroxyl groups of branched polyethers and polyesters with organosilicon substituents. The structures of the synthesized polymers were confirmed by NMR and GPC. Organosilicon moieties of the polymers were formed by silatranes and trimethylsilyl blocks and displayed hydrophilic and hydrophobic properties, respectively. The effect of the ratio of hydrophilic to hydrophobic organosilicon structures on the surface activity and biological activity of macromolecules was studied, together with the effect on these activities of the macromolecules’ molecular weight and chemical structure. In particular, the critical micelle concentrations were determined, the effect of the structure of the polymers on their wetting with aqueous solutions on glass and parafilm was described, and the aggregation stability of emulsions was studied. Finally, the effect of the polymer structures on their antifungal activity and seed germination stimulation was examined.     

Soluble rigid–flexible polyethers containing bis(biphenyl)anthracene or bis(styryl)anthracene units in the main chain for light-emitting applications

New rigid–flexible polyethers containing bis(biphenyl)anthracene or bis(styryl)anthracene units in the main chain were synthesized and characterized by viscosimetry, thermal and mechanical analysis, NMR, UV-vis, and luminescence spectroscopy. The polyethers containing bis(styryl)anthracene units in the main chain form free-standing films either from solution casting or after melt pressing at temperatures where they are thermally stable. The length of the flexible spacer influences the thermal and mechanical behavior of these polymers. The isotropization temperature as well as the glass transition temperature show an odd–even effect depending on the spacer segment length. Films with high modulus at room temperature and glass transition temperatures in the range 74–103°C were obtained using dynamic mechanical analysis. These polymers show bright-yellow photoluminescence with maximum at 580 nm in solution. In the solid state, the luminescence maximum is either red or blue shifted depending on the number of the methylene units in the aliphatic segment. The polyethers containing bis(biphenyl)anthracene units in the main chain are blue-light-emitting polymers with photoluminescence maxima at 435 and 455 nm in solution. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 3826–3837, 1999     

含偶氮苯生色团的聚醚的合成与热致液晶性质

β－氯乙基缩水甘油醚（ＧＣＥ）和ＧＣＥ／羟丁基乙烯基醚（ＨＢＶＥ）分别通过阳离子聚合、光引发共聚合,获得两种聚醚,然后再分别与４－硝基－４’－羟基偶氦苯（ＮＨＡ）反应,制备了两种侧链含偶氦苯生色团的液晶聚合物（ＰＡＥＧ、ＰＡＶ）。用ＦＴＩＲ、＾１Ｈ－ＮＭＲ和ＥＡ对其化学结构及生色团含量进行了表征,以ＰＯＭ,ＤＳＣ、ＴＧＡ和ＷＡＸＤ对聚合物介晶相转变温度、织构、热稳定性及相行为进行了研究。结果表明,     

Distannylated Bithiophene Imide: Enabling High‐Performance n‐Type Polymer Semiconductors with an Acceptor–Acceptor Backbone

A distannylated electron‐deficient bithiophene imide (BTI‐Tin) monomer was synthesized and polymerized with imide‐functionalized co‐units to afford homopolymer PBTI and copolymer P(BTI‐BTI2), both featuring an acceptor–acceptor backbone with high molecular weight. Both polymers exhibited excellent unipolar n‐type character in transistors with electron mobility up to 2.60 cm² V^?1 s^?1. When applied as acceptor materials in all‐polymer solar cells, PBTI and P(BTI‐BTI2) achieved high power‐conversion efficiency (PCE) of 6.67 % and 8.61 %, respectively. The PCE (6.67 %) of polymer PBTI, synthesized from the distannylated monomer, is much higher than that (0.14 %) of the same polymer PBTI*, synthesized from typical dibrominated monomer. The 8.61 % PCE of copolymer P(BTI‐BTI2) is also higher than those (<1 %) of homopolymers synthesized from dibrominated monomers. The results demonstrate the success of BTI‐Tin for accessing n‐type polymers with greatly improved device performance.