一种含有咔唑功能基团的有机聚磷腈的合成与表征

采用传统的亲核取代反应的方法合成了一种新有含有咔唑侧基的有机磷腈高分子，并用红外、＾１Ｈ核磁、紫外、热失重、差热分析了其结构，它的玻璃化转变温度为９１．６℃，大大低于聚乙烯咔唑的玻璃化转变温度。     

含咔唑生色团的三聚磷腈分子玻璃的合成

含咔唑生色团的三聚磷腈分子玻璃的合成;三聚磷腈;后重氮偶合;咔唑;光折变分子玻璃     

聚酚氧磷腈的合成及其热分解过程

聚酚氧磷腈的合成及其热分解过程胡源１桂宙１藤本康弘２范维澄１田村昌三３（１中国科学技术大学合肥２３００２６；２日本劳动省产业安全研究所；３日本东京大学）聚磷腈是一类骨架由磷和氮原子交替排列的无机高分子化合物。由于磷原子上有两个可取代的基团，赋予了它可...     

聚双(6-咔唑基己氧基)磷腈的合成

以PCl5和NH4Cl为原料采用"一步法"合成了线型聚二氯磷腈(4);4与6-咔唑基己醇发生亲核取代反应合成了聚双(6-咔唑基己氧基)磷腈(5),其结构经1H NMR,31P NMR,IR和GPC表征。热分析结果表明,5具有良好的热稳定性和较高的玻璃化温度。     

含咔唑生色团的聚磷腈的合成与表征

通过后重氮偶合方法制备了一种含咔唑双功能生色团的聚磷腈光折变高分子,并用1H-NMR3、1P-NMRI、R、UV-vis、GPC以及DSC、TG等测试手段对聚合物进行了分析和表征。1H-NMR、IR、UV-vis谱图表明对硝基偶氮苯基团连接在咔唑环上。31P-NMR谱图上的单峰说明聚二氯磷腈分子链上的氯已经全部被咔唑基团取代,而且后功能化反应条件没有破坏磷腈主链结构。GPC测得聚磷腈的Mw=1.28×104。热分析结果显示聚磷腈的Tg=20℃,并在300℃开始分解。     

β－萘酚取代聚磷腈的合成与表征

β－萘酚取代聚磷腈的合成与表征徐师兵，郑福安，杨永刚（华东理工大学高分子材料所，上海，２００２３７）（吉林大学理论化学研究所）关键词聚氯化磷腈，Ｎ－二氯磷酰Ｐ－三氯单磷腈，β－萘酚取代聚磷腈无机高分子聚氯化磷腈中的氯原子具有很高的反应活性，它可与许多...     

一种新型有机无机杂化聚磷腈高分子的制备及表征

通过两步亲核取代反应制备了一种新型有机一无机杂化聚磷腈高分子—丙烯胺苯酚双取代聚磷腈。运用红外光谱、氢核磁共振谱、磷核磁共振谱证实了聚合物的化学组成。热失重研究表明该聚合物具有较好的热稳定性和较高的残留率,800℃时,残炭率高达48.2％。聚合物侧链上的烯丙基基团可通过热引发交联,进一步提高其热稳定性和残炭率。     

β-萘酚取代聚磷腈的合成与表征

The method of preparing N-dichlorophosphoryl-P-trichloromonophosphazene as monomer from PCl5 and(NH4)2 SO4 in 1, 1, 2, 2-tetrachloroethane was investigated. Polydichlorophosphazene can be obtained from the polycondensation of this monomer and poly (β-naphthyloxy) phosphazen (I) was prepared from polydichlorophosphazene and sodium β-naphthyloxy.At the same time, the IR, 31P NMRof the title polymers were determined.The glass transition and viscous flow temperatures determined by TBAare-83℃ and 19℃respectively. Decomposition temperature measured by TGis 338℃.The Mn of Iestimated by VPOis 4110.     

聚对苯基苯酚取代磷腈的合成与表征

环状三聚六氯化磷腈在α-氯代萘中开环聚合得到聚氯化磷腈.后者与对苯基苯酚钠反应合成了标题聚合物.测定了该聚合物的IR、~1H NMR谱.GPC估计其数均分子量为6×10~4.扭辫分析表明,该聚合物的玻璃化转变温度与粘流温度分别为0℃和130℃,硫化温度为210℃.     

聚[二(对丙酸钠苯氧基)]磷腈合成方法的改进

本文以THF为反应溶剂制备聚[二(对丙酸钠苯氧基)]磷腈,降低了实验成本,提高的反应产率,并对制备的聚合物进行了IR,31PNMR、1HNMR表征,及TGA,GPC分析。     

Photostimulated SRN 1 Reactions of Benzyl Chloride with Carbazolyl Nitrogen Anion

In recent years, the studies of the radical chain nucleophilic substitution reaction (S.. I )have been active area in both mechanism and organic synthesis'-'. The main steps of thismechanism are sketched in scheme 1.As nucleophile, various anions have been used in S.l reaction. However, thestudies of the reactions of organic nitrogen anions are not so much reported'. We have'reported that photostimulated reactions of carbazolyl nitrogen, anion with aryl handes indimethyl sulfoxide by S.l mec…     

Polyurethanes with Pendant Hydroxyl Groups: Synthesis and Characterization

Communication: Phenoxycarbonyloxymethyl ethylene carbonate 4 was synthesized from glycerol carbonate and phenyl chloroformate. Polyurethanes with pendant hydroxyl groups were obtained from polycondensation reactions of this AA* monomer with diamines. These polymers contain primary as well as secondary hydroxyl groups. The obtained polyurethanes are amorphous materials. The glass transition temperature decreases with increasing number of methylene groups between the urethane groups.

As the number of methylene groups increases between the urethane groups, the glass transition temperature of the polymer decreases.     

Synthesis and Characterization of Cobalt-Cage Complexes with Pendant Phenol Groups

The synthesis and characterization of four compounds formed from the reductive amination of m- and o-hydroxybenzaldehyde to (1,8-diamino-3,6,10,13,16,19-hexaazabicyclo[6.6.6]eicosane)cobalt(III) are presented. These compounds are the mono- and dialkylated derivatives of the starting cobalt complex. The X-ray crystal structures of each compound, as its fully protonated chloride salt, have been obtained and are reported. The pK(a)'s of the compounds were determined by nonlinear least-squares analysis of data from potentiometric titrations and UV/vis spectrophotometry. The K(a)'s of the phenol groups of the compounds are reduced by roughly 1 order of magnitude compared to their analogous organic phenols. In the solid state, the compounds with one pendant phenol group (2, 4) are yellow and adopt the ob(3) conformation of their ethylene diamine rings in their crystal structures, while the compounds with two pendant phenol groups (3, 5) are orange and have the lel(3) conformation in their crystal structures. Solid-state reflectance UV/vis spectroscopy confirms these structural differences. In water, all four compounds form orange solutions and adopt the lel(3) conformation, as indicated by comparison of UV/vis spectroscopy and cyclic voltammetry properties with the literature.     

Synthesis and Characterization of Novel Glycerol‐Derived Polycarbonates with Pendant Hydroxyl Groups

Summary: A novel type of glycerol‐derived, water‐soluble polycarbonate with pendant, primary hydroxyl groups was prepared from 2‐(2‐benzyloxyethoxy)trimethylene carbonate (BETC). Ring‐opening polymerization of BETC and 2,2‐dimethyltrimethylene carbonate (DTC) gave narrow distribution of homopolymers or random copolymers with high molecular weights. The protecting benzyl groups were removed by catalyzed hydrogenation at atmosphere H₂ pressure to give hydroxyl polycarbonates without observable changes on the polymer backbone and molecular weight distribution. The hydrophilicity of the copolymers increases with the increase in the hydrophilic glycerol‐derived carbonate content.

Synthesis of the glycerol‐derived polycarbonate.     

Synthesis and Characterization of Functionalized Polyaniline Having Methyl Violet as Pendant Groups

Methyl violet–substituted polyaniline is prepared by oxidative polymerization of aniline in an aqueous acidic media using tosic acid as dopant and ammonium persulphate as oxidant. Substitution of methyl violet (dye moieties) on polyaniline backbone takes place in the presence of butyl lithium. The structures of methyl violet–substituted polyanilinewas elucidated by Fourier transform infrared (FT-IR), fluorescence spectra, XRD and differential scanning calorimetery (DSC). Molecular weight is determined by gel permeation chromatography (GPC) and viscosity method. Conductivity and band gap of methyl violet–substituted polyaniline was computed by a two-probe conductometer.     

Synthesis and Characterization of Novel Aliphatic Polycarbonates Bearing Pendant Allyl Ether Groups

To fulfill the diverse requirements in surgery and medicine, biomedical polymers have been drawing interests and attentions increasingly since the last decade1. In these fields, aliphatic carbonates have been proved to be a kind of material with excellent…     

Synthesis and Characterization of Six New Carbazolyl Porphyrins

Novel 4-(N-carbazole methyl) benzoic acid and N-carbazolacetic acid are synthesized, then six new carbazolyl porphyrins are synthesized by bonding these acids to hydroxy porphyrin or amido porphyrin via acyl chloride or N,N′-dicyclohexylcarbodiimide (DCC)–dimethylaminopyndine methods. The formations of these title compounds, as well as their intermediates are characterized by ¹H NMR, mass spectrometry, Fourier transform–infrared, and elemental analysis.     

新型侧基含磷共聚酯的合成、表征及性能

以精制对苯二甲酸（TPA）、乙二醇（EG）和含磷反应型阻燃剂9,10-二氢-9-氧杂-10-[2,3-二（2-羟基乙氧基）羰基丙基]-10-磷杂菲-10-氧化物为原料,利用熔融缩聚法合成了含磷量分别为0．35％、0．65％的阻燃聚酯。通过熔融纺丝法将聚酯制成纤维及织物,研究了纤维的染色性能,并通过极限氧指数法和垂直燃烧法研究了织物的阻燃性能。FT-IR和NMR研究结果表明：阻燃共聚酯含磷量为0．35％时,其氧指数（LOI）达31．5％,并无熔滴、烟雾产生,具有优异的阻燃性能和抗熔滴性能。DSC、TG和XPS的研究结果表明：侧基舍磷单元的引入降低了聚酯的Tg和Tm,较低的Tm将有利于材料加工性能的改善;阻燃聚酯侧基上的P-C、P-O键易断裂并挥发至气相中,从而降低了聚酯热稳定性,阻燃聚酯可能以气相阻燃机理为主发挥阻燃作用。此外,含磷共聚酯纤维具有较优异的染色性能。     

Synthesis and Modification of Functional Polycarbonates with Pendant Allyl Groups

Functional aliphatic polycarbonates with pendant allyl groups were synthesised by copolymerization of carbon dioxide and allyl glycidyl ether (AGE) in the presence of a catalyst system based on ZnEt₂ and pyrogallol at a molar ratio 2 : 1. The functionality of some polycarbonates was reduced by replacing a part of allyl ether with saturated glycidyl ether, i.e., butyl glycidyl ether (BGE) or isopropyl glycidyl ether (IGE). Polycarbonates obtained by the copolymerization of AGE and CO₂ or by the terpolymerization of AGE, IGE and CO₂ were oxidized with m‐chloroperbenzoic acid to their respective poly(epoxycarbonate)s. The influence of the AGE/ΣGE ratio in the polycarbonates, the polymer concentration in the reaction solution and the duration of the reaction on the conversion of allyl groups into glycidyl ones was examined. A tendency to gelation of the initial and oxidized polycarbonates during storage was observed. The initial polycarbonates and their oxidized forms were degraded in aqueous buffer of pH = 7.4 at 37°C. The course of hydrolytic degradation was monitored by the determination of mass loss.