Isolation, spectra, structure, and ring-opening polymerization of strained macrocyclic aryl(ether ketone) dimer

Macrocyclic arylene ether ketone dimer was isolated from a mixture of cyclic oligomers obtained by the nucleophilic substitution reaction of bisphenol A and 4,4'-difluorobenzophenone and easily polymerized to high molecular weight linear poly(ether ketone). The cyclic compound was characterized by FTIR, H-1- and C-13-NMR, and single-crystal x-ray diffraction. Analysis of the spectral and crystal structure reveals extreme distortions of he phenyl rings attached to the isopropylidene center and of the turning points of the molecular polygons. The release of the ring strain on ring-opening combined with entropical difference between the linear polymer chain and the more rigid macrocycle at temperatures of polymerization may be the proposed motivating factors in the polymerization of this precursor to high molecular weight poly(ether ketone). (C) 1997 John Wiley & Sons, Inc.

Efficient synthesis and facile polymerization of some cyclic bisphenol o-phthalates

A series of new macrocyclic aromatic esters have been efficiently synthesized from o-phthaloyl dichloride and various bisphenols, and unambiguously characterized by a combination of GPC, MS(FAB), FTIR and NMR. These macrocyclic oligomers undergo facile ring-opening polymerization in the presence of anionic initiators to give high molecular weight polyarylates.

Melt functionalization of ethylene-propylene copolymer: Structural investigation

An ethylene-propylene copolymer (EPM) has been functionalized with acrylic acid (AA) by means of a radical-initiated melt process. Different degrees of grafting have been obtained by varying the overall composition of the reaction mixture. The influence of the grafting degree on the structure has been investigated by differential scanning calorimetry (DSC), Fourier-transform infrared analysis (FTIR), and wide-angle x-ray scattering (WAXS) techniques. The results of the structural investigations suggest that the grafting preferentially occurs onto the ethylene sequences of EPM. After acrylic acid was grafted onto EPM, the grafted AA acted as nucleation agent; it caused an increase of crystallization temperature of propylene sequences of EPM-g-AA.

Study on the microstructure and properties of nanosized stannic oxide powders

Stannic oxide xerogel was prepared by a forced hydrolysis method using SnCl4 as the precursor. The average grain sizes of the nanosized stannic oxide powders varied with the sintering temperatures. The powders were characterized by several different physico-chemical techniques. TEM was employed for the direct observation on grain sizes, shape and state of aggregation of the particles. XRD technique was used for the determination of the crystalline structure. Microstructural parameters of average crystallite size () and mean-square root microstrain (epsilon(2)>(1/2)) for the samples were calculated from the broadened values of the half-peak intensity of XRD. The atomic ratio between oxygen and tin in the surface region of the particles was estimated through the analysis of XPS. Attributing to lots of oxygen vacancies in the surface region of the nanoparticulates and the 'trapped electrons' in the vacancies, an ESR signal was observed in the sample sintered at 300 degrees C for 2 h. FTIR of the powders showed that intensity of the transverse optical mode of Sn-O stretching vibration increased with the sintering temperature while the bending vibration of O-Sn-O showed a blue shift. For Raman spectra, very important spectral characteristics such as variations of intensity and width of the bands were observed. A new Raman vibrational band located at 572 cm(-1) was identified in the samples of nanosized stannic oxide powders. Variation of these spectroscopic properties were strongly affected by grain size, shape and state of aggregation of the nanosized particulates.