Synthesis and Characterization of Novel Poly(Arylene Ether)s from 4,4′‐Thiodiphenol

Four novel perfluoroalkylated poly(arylene ether)s have been synthesized successfully using four perfluoroalkyl‐activated bisfluoro monomers. These polymers are synthesized through nucleophilic displacement of the fluorine atoms on the benzene ring with 4,4′‐thiodiphenol and are named as 1a, 1b, 1c and 1d, respectively. The polymers obtained by displacement of the fluorine atoms exhibit weight‐average molar masses up to 3.9×10⁴ g · mol^?1 in Gel permeation chromatography. These poly(arylene ether)s showed very high thermal stability up to 548°C for 10% weight loss in TGA under nitrogen and high glass transition temperature (T_g) up to 178°C in DSC depending on the repeat unit structures. The glass transition temperatures taken as peak in tan δ in DMA measurements are in good agreement with the DSC T_g values. All the polymers synthesized are soluble in a wide range of organic solvent such as CHCl₃, CHCl₂, THF, NMP, DMF and toluene. Transparent thin films of these polymers cast from THF exhibited tensile strengths up to 72 MPa, modulus up to 1.69 GPa with low elongation at break depending on their exact repeating unit structures. Rheological properties showed ease of processability of these polymers with no change in melt viscosity with temperature.     

Synthesis and Characterization of Fluorine-containing Poly（ether ether ketone）s

<正>Poly(ether ether ketone)s(PEEK) are a class of high performance engineering thermoplastics known for their excellent thermal,mechanical,and electrical properties.This class of advanced materials has currently received considerable attention for potential application in aerospace,electronics,automobile and     

Synthesis and Characterization of Poly(ether imide)s Containing m-Methyl and Phthalazinone Moieties

Aromatic polyimides are distinguished for their excellent mechanical and thermal properties in many engineering fields1. However, aromatic polyimides are normally insoluble in common organic solvents, which restricts their applications in some fields. Many efforts have been taken to improve their solubility. Introducing bulky side groups and non-coplanar structure into polymers bone chains is a good way to obtain the polymers with excellent mechanical and thermal properties2. In this paper…     

Synthesis and Water Uptake of Sulfonated Poly （phthalazinone ether sulfone ketone）/Polyacrylic Acid Proton Exchange Membranes

Proton exchange membrane fuel cell (PEMFC) is extremely attractive as power sources for transportation, power stations and portable electrical devices, because of their efficiency, cleanliness and quiet1. The heart of PEMFC is proton exchange membranes (P…     

Synthesis and Characterization of Novel Poly(Arylene Ether)s from 1,3‐bis(4‐Hydroxyphenyl) Benzene

Abstract

Several poly(aryl ether)s have been prepared by the condensation of 1,3‐bis(4‐hydroxy phenyl) benzene with different trifluoromethyl activated bis‐fluoro compounds. IR, ¹H and ¹³C NMR, and elemental analyses have established the resulting polymer structures. The properties of the polymers have been evaluated by DSC, TGA, dynamic mechanical analysis (DMA) and stress–strain analysis. The polymers 1a and 1c showed semi‐crystalline behavior as evident by sharp crystalline melting peaks at 299°C and 330°C along with glass transitions at 202°C and 216°C, respectively. The polymers showed very good thermal stability in air, high modulus, and high tensile strength with low elongation at break.     

Synthesis and Characterization of Poly(ether ether ketone)s with (2,5‐dihydroxy)phenyl Side Group

A new monomer, (2,5‐dimethoxy)phenylhydroquinone (DMPH), was prepared in a two‐step synthetic procedure. One aromatic poly(ether ether ketone)s with 2,5‐dimethoxy phenyl side group (DMP‐PEEK) was synthesized via an aromatic nucleophilic substitution reaction with 4,4′‐difluorobenzophenone (DFB). Poly(ether ether ketone)s with 2,5‐dihydroxy phenyl side group (DHP‐PEEK) was obtained via hydrolysis of methoxy group on the DMP‐PEEK. Both of the high molecular weight polymers could be obtained despite the steric effect of the bulky pendant groups. The two polymers have good solubility at room temperature.     

Synthesis and Characterization of Poly（ether amide）s Containing Bisphthalazinone and Ether Linkages

A novel aromatic diacid, 4, 4′-bis[2-(4-carboxyphenyl)phthalazin- 1-one-4-yl]-bisphenyl ether III, containing bisphthalazinone and ether linkages was prepared from nucleophilic substitution of p-chlorobenzonitrile with the bisphenol-like monomer I, followed by alkaline hydrolysis of the intermediate dinitrile II. A series of poly(ether amide)s containing bisphthalazinone and ether linkages derived from diacid III and aromatic diamines were synthesized by one-step solution condensation polymerization using triphenyl phosphite and pyridine as condensing agents. Moreover, the properties of poly(ether amide)s including thermal stability,solubility and crystallinity were also studied.     

Synthesis and modification of oligo(aryloxycyclotriphosphazenes) based on 4,4′-dihydroxydiphenyl-2,2-propane

Oligo(aryloxyphosphazenes) are synthesized on the basis of diphenylolpropane and hexachlorocyclotriphosphazene via the phenolate method. Corresponding functional derivatives are obtained through treatment of the oligomers with methacryloyl chloride, glycidyl methacrylate, and epichlorohydrin. GPC data indicate that modification is accompanied by an increase in the molecular mass of the oligomers. Epoxidation of a specially synthesized hexaallyloxy derivative of oligo(aryloxycyclotriphosphazene) with m-chloroperbenzoic acid proceeds incompletely to yield an oligomer with a content of epoxy groups below 6%. All of the compounds are characterized with the use of ³¹P and ¹H NMR spectroscopy.     

Synthesis and Characterization of Ion-exchange Sulfonated Poly （ether sulfone）

N,N'-Bis(3-hydroxyphenyl)-1,8,4,5-naphthalenetetracarboxylic bisimide was prepared from the reaction of 1,8,4,5-naphthalenetetrcarboxylic acid dianhydride and 2-aminophenol in N, N-dimethylformamide. Polymerization of this bisimide with 4,4'-difluorodiphenylsulfone and disodium 3,3'-disulfonate4,4'-difluorodiphenylsulfone gave ion-exchange sulfonated poly(ether sulfone). The structure of the title compound was characterized with 1H-NMR and its polymer was characterized with FT-IR.     

Preparation and Characterization of Chitosan Composite Membranes Crosslinked by Carboxyl-capped Poly（ethylene glycol）

In this study a series of chemically crosslinked chitosan/poly（ethylene glycol） （CS/PEG） composite membranes were prepared with PEG as a crosslinking reagent other than an additional blend. First, carboxyl-eapped poly（ethylene glycol） （HOOC-PEG-COOH） was synthesized. Dense CS/PEG composite membranes were then prepared by casting/evaporation of CS and HOOC-PEG-COOH mixture in acetic acid solution. Chitosan was chemically crosslinked due to the amidation between the carboxyl in HOOC-PEG-COOH and the amino in chitosan under heating, as confirmed by FTIR analysis. The hydrophilicity, water-resistance and mechanical properties of pure and crosslinked chitosan membranes were characterized, respectively. The results of water contact angle and water absorption showed that the hydrophilicity of chitosan membranes could be significantly improved, while no significant difference of weight loss between pure chitosan membranes and crosslinked ones was detected, indicating that composite membranes with amidation crosslinking possess excellent water resistanance ability. Moreover, the tensile strength of chitosan membranes could be significantly enhanced with the addition of certain amount of HOOC-PEG-COOH crosslinker, while the elongation at break didn＇t degrade at the same time. Additionally, the results of swelling behaviors in water at different pH suggested that the composite membranes were pH sensitive.     

Synthesis and Properties of Novel Poly（amine ether）s

Using aromatic bis（4-bromophenyl） ether and various aromatic diamines as the monomers, a series of novel poly（amine ether）s （PAEs） have been synthesized via palladium-catalyzed aryl amination, which is the Hartwig-Buchwald polycondensation reaction. Their structures were characterized by means of elemental analysis, FT-IR, 1^H NMR and UV-Vis spectroscopy. The results show a good agreement with the proposed structures. Their general properties were studied by DSC and TG and it＇s obvious that they show high glass transition temperatures （Tg〉200 ℃）, good thermal stability with high decomposition temperatures （TD〉500℃） and excellent solubility. The mechanical behavior of these polymers suggested that they could be considered a new class of high-performance polymers.     

Synthesis and Characterization of Poly (Ether Sulfone Ketone) Containing the Phthalazinone Moiety

IntroductionHeterocyclicpolymersareaclassofpolymersthatusuallyshowexcellentthermalstabilityandhavereceivedconsiderableattentionashigh-modulusplastics.Theycanbesynthesizedbythereactionofheterocyclichandesoractivatedarylhandeswithahis(phenolate)anioninanucleophilicdisplacementreaction.Manydifferenttypesofhightemperatureheterocyclicpolymers,suchaspoly(etherimide)s,poly(aryletherbenzoxazole)s,poly(etherketone)shavebeensynthesizedbythismethodl-3.Inthispaper,anovelpoly(ethersulfoneketone)withC-Nbon…     

Synthesis and Characterization of a Series of New Functional Poly(ferrocenylenesilanes) for Nonlinear Optics

ＩｎｔｒｏｄｕｃｔｉｏｎＰｏｌｙ(ｆｅｒｒｏｃｅｎｙｌｓｉｌａｎｅｓ)ａｒｅａｎｏｖｅｌｃｌａｓｓｏｆｔｒａｎｓｉｔｉｏｎｍｅｔａｌｏｒｇａｎｏｍｅｔａｌｌｉｃｐｏｌｙｍｅｒｓｗｉｔｈａｂａｃｋｂｏｎｅｃｏｎｓｉｓｔｉｎｇｏｆａｌｔｅｒｎａｔｉｎｇｆｅｒｒｏｃｅｎｅａｎｄｏｒｇａｎｏｓｉｌａｎｅｕｎｉｔｓ .Ｈｉｇｈｍｏｌｅｃｕｌａｒｗｅｉｇｈｔｐｏｌｙ(ｆｅｒｒｏｃｅｎｙｌｅｎｅｓｉｌａｎｅｓ)ｗａｓｆｉｒｓｔｓｙｎ ｔｈｅｓｉｚｅｄｖｉａｔｈｅｒｍａｌｒｉｎｇ ｏｐｅｎｉｎｇｐｏｌｙｍｅｒｉｚａｔｉ…     

Synthesis and Characterization of Poly(hydrogen halide) Halogenates (–I)

Herein, we report the synthesis and characterization of a variety of novel poly(hydrogen halide) halogenates (−I). The bifluoride ion, which is known to have the highest hydrogen bond energy of ≈160 kJ mol⁻¹, is the most famous among many examples of [X(HX)_n]⁻ anions (X=F, Cl) known in the literature. In contrast, little is known about poly(hydrogen halide) halogenates containing two different halogens, ([X(HY)_n]⁻). In this work we present the synthesis of anions of the type [X(HY)_n]⁻ (X=Br, I, ClO₄; Y=Cl, Br, CN) stabilized by the [PPh₄]⁺ and [PPN]⁺ cation. The obtained compounds have been characterized by single-crystal X-ray diffraction, Raman spectroscopy and quantum-chemical calculations. In addition, the behavior of halide ions in hydrogen fluoride was investigated by using experimental and quantum-chemical methods in order to gain knowledge on the acidity of hydrogen halides in HF.     

Synthesis and Characterization of Biodegradable Poly(ϵ-caprolactone)-b-Poly(L-lactide) and Study on Their Electrospun Scaffolds

A series of multi-block copolymers, poly(L-lactide)-b-poly (?-caprolactone) (PLLA-b-PCL) were synthesized. The first step of the synthesis consisted of the transesterification between the PLLA and 1,4-Butanediol, followed by the copolymerization of PLLA-diols and PCL, using isophorone diisocyanate (IPDI) as a coupling agent. The synthesized polymers were characterized by Fourier transform infrared (FTIR) spectra, differential scanning calorimetry (DSC) and wide angle X-ray diffraction (WAXD). PLLA/PCL block copolymers were electrospun into ultrafine fibers. The morphology of the electrospun fibrous scaffolds were investigated by Scanning Electron Microscopy (SEM). Results showed that the morphology and diameter of the fibers were affected by the electrospinning solution concentrationan and different weight ratio of PLLA/PCL. These electrospun PLLA-b-PCL fibrous membranes exhibited good flexibility and deformability. In comparison with the electrospun PLLA membrane, the electrospun fibrous membranes of PLLA-b-PCL demonstrated an enhanced elongation with still high tensile strength and Young's modulus to be beneficial for tissue engineering scaffolds.     

Synthesis and Characterization of Tris(2,2′-bipyridine) and tris(1,10-phenanthroline) Copper(II) Hexafluorophosphate. Crystal Structure of the Phenanthroline Complex

The tris-(bidentate)chelate complexes [Cu(NN)₃](PF₆)₂ where NN=2,2'-bipyridine or 1,10-phenanthroline have been isolated as secondary products in the reaction between the dimers [{Cu(NN)}₂(μ-OH)₂](PF₆)₂·2H₂O and di-2-pyridylketone. the X-ray crystal structure of [Cu(phen)₃](PF₆)₂ showed a distorted octahedral C ₂ geometry around teh metal atom, with two Cu-N distances being much longer than the other four. Magnetic susceptibility measurements (in the 4.4-290K range) correspond, in both cases, to a d⁹ configuration without significant magnetic interaction. A signal (g=2.102) was observed in the EPR spectrum of the bipy complex and the two axial components were resolved for the phen complex, with g_||=2.249, g_⊥=2.083 and A_||=137 x 10^-4cm^-1. In this case also a signal at g=2.128 is observed.     

Synthesis and characterization of poly(phthalazinone biphenyl ether sulfone ketone)s from 4,4′-dichlorobenzophenone

A series of poly(aryl ether sulfone ketone)s containing phthalazinone and biphenyl moieties were synthesized by aromatic nucleophilic displacement polycondensation of 4-(4-hydroxylphenyl)(2H)-phthalazin-1-one (DHPZ), 4,4′-dichlorobenzophenone (DCB), 4,4′-dichlorodiphenyl sulfone (DCS) and 4,4′-biphenol (BP) in different molar ratios. The obtained copolymers were characterized by different instrumental techniques (FTIR, TGA, DSC, WAXD, etc.). The inherent viscosities of these polymers were in the range of 0.43–0.56 dL g⁻¹. They were amorphous and had good solubility in polar aprotic organic solvents. The copolymers exhibited high glass transition temperatures (T _gs) between 225°C and 256°C and excellent thermal stability up to 517–526°C (thermal decomposition temperatures for 5% weight loss, T _{d, 5%}) in nitrogen. The tensile strength and elongation at break of the polymers ranged from 63 MPa to 71 MPa and from 18% to 21%, respectively. The processability of the material was effectively improved by the introduction of biphenyl group into polymer backbone.     

Synthesis, Characterization and Crystal Structure of (2,2′-Bipyridine)(μ-maleato)copper(II) Dihydrate

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Synthesis and characterization of complexes of the first transition series cations with 2,2′-biimidazole and 2,2′-biimidazolate

Mononuclear [M(hfacac)₂(H₂biim)] complexes, where M = Mn^II, Fe^II, Co^II, Ni^II, Cu^II or Zn^II, hfacac = hexafluoroacetylacetonate, H₂biim = 2,2-biimidazole; dinuclear K₂[M₂(acac)₄(-biim)] (M = Cu^II or Zn^II) and tetranuclear K₂[M₄(acac)₈( ₄-biim)] (M = Co^II or Ni^II) complexes have been prepared and characterized by chemical analysis, conductance measurements, i.r., electronic and e.p.r. spectroscopies and by magnetic susceptibility measurements (in the 2–300 K range). Mn^II, Fe^II and Co^II are in a high spin state. The e.p.r. spectra of Cu^II and Mn^II compounds have been recorded.