Polymer-Metal Complexes: Synthesis and Characterization of Poly-(2-Hydroxy-4-acryloxyacetophenone-semicarbazone) Metal Complexes

Abstract

2-Hydroxy-4-acryloxyacetophenone (HAAP) was synthesized and polymerized in 2-butanone using benzoyl peroxide as initiator at 65 °CC. Poly(2-hydroxy-4-acryloxyacetophenone-semicarbazone) (HAAPS) was prepared from poly(HAAP) and semicarbazide hydrochloride and was characterized by IR and NMR spectral studies. The molecular weights of the polymer was determined by gel permeation chromatography. Cu(II) and Ni(II) chelates of poly(HAAPS) were synthesized. Thermogravimetric analysis of the polychelates have been carried out. Elemental analysis of the poly chelates suggest a metal to ligand ratio as 1:2. The polychelates were also characterized by infrared, electronic spectral studies, magnetic, and conductivity measurements.     

Synthesis and Characterization of Poly-[2-methoxy-4,6-di(2,7-Naphthyloxy)-s-triazine]

Abstract

Poly[2-methoxy-4,6-di (2,7-naphthyloxy)-s-triazine] was synthesized by interfacial polycondensation of 2-methoxy-4,6-dichloro-s-triazine with 2,7-dihydroxy-naphthalene. The polymer was characterized by IR and UV spectra, dynamic mechanical analysis, differential scanning calorimetry, and thermogravimetric analysis. The polymer was fractionated by the fractional precipitation method and the fractions were characterized by viscometry and membrane osmometry. The polymer has a T^g of 175°C and is found to be stable up to 300°C in air. The polymer sample is found to degrade in air in two steps, and the energy of activation for the first step is around 25 kcal/mol.     

聚-2-氨基吡啶电化学合成及性质

报导了在 0.43 mol•dm－3 C6H6N2和0.01 mol•dm－3 NaOH中用循环伏安法合成聚-2-氨基吡啶. 聚-2-氨基吡啶在1.0 mol•dm－3 ZnCl2(pH=4.99)溶液中的循环伏安图上有三对氧化-还原峰.旋转环-盘实验的结果表明,在 2-氨基吡啶聚合的初期有中间体生成.由红外光谱可知，聚-2-氨基吡啶具有头-尾相接的结构.聚-2-氨基吡啶平均粒子大小约893 nm， 平均粒子间距约 255 nm. 由聚-2-氨基吡啶正极和锌负极及2.5 mol•dm－3 ZnCl2溶液和 3.0 mol•dm－3 NH4Cl (pH=5.5) 溶液构成的电池，其放电曲线类似于Li-SOCl2, 放电曲线的中间区域非常平稳.     

The Synthesis of Poly(Dimethylsiloxane-b-Isobutylene-b-Dimethylsiloxane) and Poly-(Dimethylsiloxane-b-Isobutylene-b-Dimethylsiloxane) from Alcohol-Telechelic Polyisobutylenes

The purpose of these studies was to combine polydimethylsiloxane (PDMS) and polyisobutylene (PIB) sequences into novel triblock, PDMS-b-PIB-b-PDMS, and multiblock, (-PDMS-b-PIB-b-PDMS-)n, copolymers. The key toward syntheses was the definition of conditions for the initiation of living anionic polymerization of hexamethyl-cyclotrisiloxane (D₃) at the CH₂OLi termini of well-defined tele-chelic PIB sequences. Subsequent deactivation of living D₃ polymerization charges with Me₃ SiCl yielded the target triblock whereas stoichiometric amounts of Me₂ SiCl₂ gave the multiblock copolymer.     

Co(AMP)2Cl2的合成及表征

氯化钴;二甲氧基嘧啶胺;固态配合物;Co(AMP)2Cl2的合成及表征     

Template Synthesis of Polyaniline in the Presence of Poly-(2-acrylamido-2-methyl-1-propanesulfonic Acid)

A template oxidative polymerization of aniline in aqueous solutions containing poly-(2-acrylamido-2-methyl-1-propanesulfonic acid) and ammonium persulfate yields a polyaniline complex with the polyacid soluble in water. According to the data of spectral measurements, the process of polymerization is of a pronounced autocatalytic nature. The consequences of this are both the formation of a nonuniform distribution of oxidized and nonoxidized fragments of the polymer chain and the formation of a macroscopic scale of redox nonuniformities in the reaction volume during the process of polymerization. The spectra of absorption of the polyaniline/polyacid films on transparent glass electrodes with a conductive layer of SnO₂ and the data of potentiodynamic measurements in the potential region 0–1.0 V (Ag/AgCl) are typical for polyaniline with moderate electroconduction.     

聚丙烯酸[2,5-双(对甲氧基苯甲酰氧基)苄酯]及聚甲基丙烯酸[2,5-双(对甲氧基苯甲酰氧基)苄酯]的合成

周其凤等曾报道聚丙烯酸［２,５－双（对甲氧基苯甲酰氧基）节酯］［１］和聚甲基丙烯酸［２,５－双（对甲氧基苯甲酰氧基）苄酯］［２］的合成．但后来的研究发现,在合成单体的条件下出现的一种未见报道的异常反应［３］使产物成分复杂化,因此当时报道的聚合物可能不是聚丙烯酸［２,５－双－（对甲氧基苯甲酰氧基）苄酯］或聚甲基丙烯酸［２,５－双（对甲氧基苯甲酰氧基）苄酯］,而可能是共聚物．针对这一问题,我们重新设计了合成路线以避免发生上述副反应,成功地合成了丙烯酸或ａ－甲基丙烯酸［２,５－双－（对甲氧基苯甲酰氧基…     

聚丙烯酰胺/聚异丙基丙烯酰胺互穿网络水凝胶的制备与性能

采用分步法用电子加速器辐射合成了聚丙烯酰胺(PAAm)/聚异丙基丙烯酰胺(PNIPAAm)互穿网络水凝胶,并考察了温度、pH值、离子强度对其溶胀性能的影响.研究表明:互穿水凝胶具有温度敏感性,且其体积相变与互穿网络中PAAm和PNIPAAm含量有关,随着网络中PAAm含量的增加水凝胶的体积相变趋于平缓,可以通过改变PAAm和PNIPAAm的组成比来控制水凝胶的体积相变行为.此外,互穿水凝胶还具有pH敏感性和一定的抗盐性.     

Synthesis and Characterization of Fluorodinitroamine,FN(NO2)2

NF₃ and N(NO₂)₃ are known compounds, whereas the mixed fluoronitroamines, FN(NO₂)₂ and F₂NNO₂, have been unknown thus far. One of these, FN(NO₂)₂, has now been prepared and characterized by multinuclear NMR and Raman spectroscopy. FN(NO₂)₂ is the first known example of an inorganic fluoronitroamine. It is a thermally unstable, highly energetic material formed by the fluorination of the dinitramide anion using NF₄⁺ salts as the preferred fluorinating agent.     

Synthesis and Characterization of Fluorodinitroamine,FN(NO2)2

NF₃ and N(NO₂)₃ are known compounds, whereas the mixed fluoronitroamines, FN(NO₂)₂ and F₂NNO₂, have been unknown thus far. One of these, FN(NO₂)₂, has now been prepared and characterized by multinuclear NMR and Raman spectroscopy. FN(NO₂)₂ is the first known example of an inorganic fluoronitroamine. It is a thermally unstable, highly energetic material formed by the fluorination of the dinitramide anion using NF₄⁺ salts as the preferred fluorinating agent.     

聚γ-巯丙基硅氧烷钯(0)配合物的合成及催化性能研究

γ－巯丙基三乙氧基硅烷依次与气相法二氧化硅，氯化钯作用，然后用水合肼还原，合成了新配合物聚γ－巯丙基硅氧烷钯。该配合物是丙烯酰胺及丙烯酸丁酯的Ｈｅｃｋ芳基化反应的有效催化剂，为立体选择性地２Ｅ－不饱酰胺及不饱和酯提供了简便且实用的方法。     

Synthesis and Characterization of 2,5-Bis(2-pyridyl)thiophene

2-[2-(Trimethylsilyl)ethynyl] pyridine ( 6 ) was prepared in 95% yield by reaction of 2-bromopyridine with trimethylsilylacetylene in triethylamine in the presence of bis(triphenylphosphine)Palladium(II) chloride and Copper(I) iodide. Desilylation of ( 6 ) by refluxing with sodium hydroxide in methanol (yield 95%) of 2-ethynylpyridine ( 5 ). Oxidative coupling of ( 5 ) in pyridine by oxygen in the presence of Copper(I) chloride gives 70% yield of 1,4-bis(2-pyridyl)1,3-butadiyne ( 4 ). Reaction of 4 with sodium sulfide affords 100% of 2,5-bis(2-pyridyl) thiophene ( 1 ).     

Synthesis and Characterization of Alkyltris(2-pyridyl)phosphonium Salts

Alkytris(2-pyridyl)phosphonium salts [(2-Py) ₃ PR]X 1 [1a, R = Et, X = Br; 1b, R = Pr, X = Br; 1c, R = Bu, X = Br; 1d, R = CH₂Ph, X = Br; 1e, R = CH ₂ Ph, X = Cl] were synthesised from (2-Py) ₃ P and an excess of RCl. 1c and 1e were found to rapidly decompose in hot acetone to 2,2′-bipyridinium(+1) bromide 2 and (2-Py)P(O)(CH ₂ Ph)C(OH)Me ₂ 3, respectively. A reaction mechanism for both products is proposed. All compounds were fully characterized, including X-ray crystallography for 1a and 3 with 1a being the first representative of this class of compounds characterized by this technique.     

官厅水库蓝绿藻及藻毒素初步研究

聚苹果酸最初是由微生物学家在研究青霉菌的过程中发现的,聚苹果酸的人工合成由逐步聚合法开始,但由于苹果酸单体具有3种功能基,因此得到的是支化的聚苹果酸,随后人们改用苄酯基保护一端羧基的苹果酸单体,以DCC为缩合剂,进行缩聚,但这种方法只能得到聚苹果酸低聚物。     

(EnH2)2Ge2S6的合成与结构表征

用溶剂热方法制备了(EnH2)2Ge2S6单晶.单晶X射线衍射分析结果表明,(EnH2)2Ge2S6属单斜晶系,P2(1)/n空间群,晶胞参数a=0.67125(5)nm,b=1.12290(4)nm,c=1.07518(4)nm,β=92.288(2)°,Z=2.利用DSC及TG分析研究了其热稳定性,结果表明,该化合物在200℃以下能够稳定存在.     

Synthesis and Biomedical Properties of Poly-[(Ethylene-Vinylalcohol)-g-Acrylamide]

This paper deals with the graft copolymerization of acrylamide (AM) onto ethylene-vinyl alcohol copolymer (EVAL) film initiated by cerium(IV) ion. It was found that both the chemical and diffusion factors had influences on the graft reaction. The reaction was initiated on the surface and then penetrated inward as the grafting percentage was increased. The permeability of urea through the grafted EVAL film was improved compared to that of the original film as was the blood compatibility.     

聚-ω-(甲硒基)十一烷基硅氧烷钯(O)配合物的合成与催化性能

ω-氯代十一烷基三乙氧基硅烷依次用气相法二氧化硅固载、与甲硒基钠和氯化钯作用,再用水合肼还原,合成了气相法二氧化硅负载的聚-ω-(甲硒基)十一烷基硅氧烷钯(0)配合物.该钯(0)配合物对丙烯腈和丙烯酸与芳基碘的Heck芳基化反应具有很高的催化活性,为各种肉桂腈和肉桂酸的立体选择合成提供了方便实用的新途径.