Synthesis and properties of organosoluble poly(amide imide imide)s based on tetraimide dicarboxylic acid condensed from 4,4′‐(hexafluoroisopropylidene)diphthalic anhydride, 4,4′‐oxydianiline,and trimellitic anhydride and various aromatic diamines

A novel tetraimide dicarboxylic acid was synthesized with the ring‐opening addition of 4,4′‐(hexafluoroisopropylidene)diphthalic anhydride, 4,4′‐oxydianiline, and trimellitic anhydride in a 1/2/2 molar ratio in N‐methyl‐2‐pyrrolidone followed by azeotropic condensation to tetraimide dicarboxylic acid. A series of poly(amide imide imide)s (PAIIs) with inherent viscosities of 0.8–1.1 dL/g were prepared from tetraimide dicarboxylic acid with various aromatic diamines by direct polycondensation. Most of the PAIIs were readily soluble in a variety of amide polar solvents and even in less polar m‐cresol and pyridine. Solvent‐cast films had tensile strengths ranging from 99 to 106 MPa, elongations at break ranging from 8 to 13%, and initial moduli ranging from 2.0 to 2.3 GPa. The glass‐transition temperatures of these PAIIs were recorded at 244–276 °C. They had 10% weight losses at temperatures above 520 °C in air or nitrogen atmospheres. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 1092–1102, 2002     

Synthesis and properties of amine‐containing poly(arylene ether sulfone) as an anion‐exchange matrix

Poly(arylene ether sulfone) (PSF), showing good thermal stability and excellent mechanical properties, was synthesized as an anion‐exchange matrix. It was synthesized by the condensation polymerization between bisphenol A and 4,4′‐dichlorodiphenylsulfone. 1°‐Amine‐containing poly(arylene ether sulfone) (1°‐APSF) was synthesized by the reduction reaction of a nitrated PSF. Then, it was transferred to 3°‐amine‐containing poly(arylene ether sulfone) (3°‐APSF) by the alkylation of the amine of 1°‐APSF. The properties of PSF, 1°‐APSF, and 3°‐APSF were investigated by Fourier transform infrared, ¹H NMR spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. The introduction of the 3°‐amine group into PSF increased the glass‐transition temperature but decreased thermooxidative stability. The ion‐exchange capacities of 1°‐APSF and 3°‐APSF were shown to be 2.24 and 2.86 mequiv/g, respectively. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 4281–4287, 2002     

Synthesis of poly (ether-sulfone-amide)s by palladium-catalyzed polycondensation of aromatic dibromides containing ether sulfone structure,aromatic diamines,and carbon monoxide

A general method for the preparation of aromatic poly (ether-sulfone-amide)s has been developed. Polymerization is based on the palladium-catalyzed polycondensation of aromatic dibromides containing ether sulfone structural units, aromatic diamines, and carbon monoxide. Reactions were carried out in N, N-dimethylacetamide (DMAc) in the presence of palladium catalyst, triphenylphosphine, and 1,8-diazabicyclo [5,4,0]–7–undecene (DBU), and gave a series of poly (ether-sulfone-amide)s with inherent viscosities up to 0.86 dL/g under mild conditions. The polymers were quite soluble in strong acids, dipolar aprotic solvents, and pyridine. Thermogravimetry of the polymers showed excellent thermal stability, indicating that 10% weight losses of the polymers were observed in the range above 470°C in air. The glass transition temperatures of the polymers were around 230°C, which are higher than those of poly (ether-sulfone) analogues. These polymers also showed the good tensile strengths and tensile modulus. © 1994 John Wiley & Sons, Inc.     

Processing polyamides with superheated water

Superheated water (shH₂O) is investigated as a process aid in conventional aliphatic polyamide (PA) systems. The polymers investigated include PA 6 (PA6), PA 6,6 (PA66), PA 6,12 (PA612), and PA 12 (PA12). It is shown that the PA melting and crystallization temperatures are significantly reduced when exposed to shH₂O. For example, the melting temperature of PA6 is depressed from 206 to 153 °C in the presence of shH₂O. A relationship between amide group density and thermal transition temperature reduction is observed. Processing these materials in shH₂O has led to a variety of materials ranging from low‐density foams to higher density locally anisotropic foamed morphologies. In situ observations of PAs melting in the presence of shH₂O are performed using a specially designed reactor. Results from these experiments are used to estimate the diffusion coefficient of shH₂O in PA6. Finally, low‐temperature extrusion is performed with PA6 and shH₂O at temperatures as low as 180 °C and mixture viscosity is estimated. A 20‐fold depression in the melt viscosity of PA6 is observed at 240 °C with shH₂O. © 2018 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2018 , 56, 803–813     

Synthesis of furan dimer‐based polyamides with a high melting point

Polyamide composed of furan dimer, which is prepared from biomass‐derived organic molecule 2‐furfural, is synthesized. The reaction of 2,2′‐furan dimer 5,5′‐dicarbonyl chloride with several 1,ω‐diamines was carried out with a solution or interfacial polycondensation leading to the corresponding polyamide. Measurement of the melting point was performed resulting to exhibit a higher temperature compared with the related polyamide bearing a single furan ring composed of furan‐2,5‐dicarboxylic acid (FDCA). Thermal analyses (TG–DTA) also indicated higher temperatures of decomposition than those of FDCA‐derived polyamide. © 2018 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2018 , 56, 1516–1519     

Palladium‐Catalyzed Direct Cross‐Coupling of Carboranyllithium with (Hetero)Aryl Halides

A palladium‐catalyzed direct C‐arylation reaction of readily available cage carboranyllithium reagents with aryl halides has been developed for the first time. This method is applicable to a wide range of aryl halide substrates including aryl iodides, aryl bromides, and heteroaromatic halides.     

A highly rigid diamine monomer derived from naturally occurring myo‐inositol and its use for polyamide synthesis

A rigid diamine was synthesized from myo‐inositol, a naturally occurring cyclic hexaol, and used as a monomer to synthesize polyamides. myo‐Inositol was treated with 1,1‐dimethoxycyclohexane to yield a bisketal bearing two hydroxyl groups, and from this bisketal, the target diamine was synthesized in three steps: (1) derivation of the diol into the corresponding bistriflate, (2) nucleophilic substitution of the bistriflate with sodium azide yielding a diazide, and (3) reduction of the diazide to the target diamine. The target diamine readily underwent polycondensation with dicarboxylic acid chloride in solution. The resulting polyamides, whose main chain inherited the rigid 5‐6‐5 system from the diamine monomers, have high glass transition temperatures. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2016 , 54, 3436–3443     

Light intensity and image visualization of GDI injector sprays according to nozzle hole arrangements

The light intensity measurement and image visualization of multi-hole injection spray due to different hole arrangements and hole numbers were investigated. The light intensities and behavior characteristics of the GDI spray were analyzed through the axial and diagonal spray penetration, cone angle, and spray area from the spray images by using the image visualization system and image analysis system. The atomization performance of GDI injectors was analyzed by the local and overall Sauter mean diameter (SMD) measurement.     

Shear and extensional rheology of entangled polymer melts: Similarities and differences

This work extends our previous understanding concerning the nonlinear responses of entangled polymer solutions and melts to large external deformation in both simple shear and uniaxial extension. Many similarities have recently been identified for both step strain and startup continuous deformation, including elastic yielding, i.e., chain disentanglement after cessation of shear or extension, and emergence of a yield point during startup deformation that involves a deformation rate in excess of the dominant molecular relaxation rate. At a sufficiently high constant Hencky rate, uniaxial extension of an entangled melt is known to produce window-glass-like rupture. The present study provides evidence against the speculation that chain entanglements tie up into "dead knots" in constant-rate extension because of the exponentially growing chain stretching with time. In particular, it is shown that even Instron-style tensile stretching, i.e., extending a specimen by applying a constant velocity on both ends, results in rupture. Yet, in the same rate range, the same entangled melt only yields in simple shear, and the resulting shear banding is clearly not a characteristic of rupture. Thus, we conclude that chain entanglements respond to simple shear in the manner of yielding whereas uniaxial extension is rather effective in causing some entanglements to lock up, making it impossible for the entanglement network to yield at high rates.     

Contribution à l'étude Électrochimique de Dérivés de l'Acide Mercapto-2 Pyridinecarboxylique-5. II

Abstract

Electrochemical caracteristics of 2-mercaptopyridine-5-carboxylic acid and its methylic ester have been determined using recent polarographic techniques. Measurements have been carried out as a function of parameters such as frequency, others surimposed signals and as a function of concentration and pH. Results are compared to those obtained for selectively methylated on sulfur or nitrogen atoms derivatives. Interpretations of the data are given. The optimal conditions for a quantitative determination by D.C. and differential pulse polarography are fixed.