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Possibility of imide structure formation under microwave irradiation of molecules containing anhydride and isocyanate functional groups was investigated. The microwave-assisted polycondensation of aromatic diisocyanates and dianhydrides for preparation of polyimides was studied. The effect of microwave irradiation time and power, solvent nature, solid content of monomers, effect of catalyst, effect of polymerization reactor material and possibility of pressure development during polymerization, on the inherent viscosity of prepared polyimides were discussed. Experimental results showed that polymers obtained via this method had superior inherent viscosity and yield in comparison to the polymers obtained via conventional solution method. 相似文献
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Rangwalla H Schwab AD Yurdumakan B Yablon DG Yeganeh MS Dhinojwala A 《Langmuir : the ACS journal of surfaces and colloids》2004,20(20):8625-8633
A new and direct approach to verify surface heterogeneity as the microscopic origin of contact-angle hysteresis is demonstrated. IR-visible sum-frequency-generation spectroscopy (SFG) was used to selectively probe the molecules at the interface of an alkyl-side-chain polymer [poly(vinyl n-octadecyl carbamate-co-vinyl acetate)] with water. The spectra indicate that in contact with water, the polymer surface is heterogeneous (having areas of differing surface energies). This evidence of surface heterogeneity supports the hysteresis observed in the advancing and receding contact angles of the polymer surface with water. The same measurements made for the chemically and structurally similar surface of an octadecyltrichlorosilane self-assembled monolayer indicates a homogeneous surface at the water interface. In this case, contact-angle hysteresis measurements implicate surface roughness as the cause of hysteresis. Atomic force microscopy measurements of roughness for these surfaces further support our conclusions. The polymer-water interface was probed using SFG at above-ambient temperatures, and an order-to-disorder transition (ODT) of alkyl side chains at the interface was observed, which closely follows the melting of crystalline side chains in the bulk. This transition explains the increased wettability of the polymer, by water, when the temperature is raised above the bulk melting temperature. Furthermore, the irreversibility of this ODT suggests that the disordered polymer-water interface is the thermodynamic equilibrium state, whereas the before-heating structure of this interface is a kinetically hindered metastable state. 相似文献
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Harp GP Rangwalla H Yeganeh MS Dhinojwala A 《Journal of the American Chemical Society》2003,125(37):11283-11290
Surface-sensitive infrared-visible sum frequency generation spectroscopy (SFG) in total internal reflection geometry has been used to study the structure of poly(vinyl n-octadecyl carbamate-co-vinyl acetate) (PVNODC) or poly(octadecyl acrylate) (PA-18) in contact with a deuterated or hydrogenated polystyrene (dPS or hPS) layer. SFG spectra from the PVNODC (or PA-18)/hPS interface show methyl and methylene peaks corresponding to PVNODC (or PA-18) and phenyl peaks corresponding to the PS. Analysis suggests that the methyl groups are tilted at angles less than 30 degrees with respect to the surface normal. The presence of a strong methylene peak suggests the PVNODC alkyl side chains contain more gauche defects at the PS/PVNODC interface in comparison to PVNODC (or PA-18)/air interfaces. On heating, the SFG intensity from the PS/PA-18 interface drops sharply near the bulk melting temperature (T(m)) of PA-18. Interestingly, a similar drop in SFG signal is also observed for the PS phenyl groups. This demonstrates the ability of the phenyl group at the PS/PA-18 interface to rearrange itself upon the solid-to-liquid transition of the PA-18 alkyl side chain, at a temperature well below the bulk PS glass transition temperature. For PS/PVNODC interfaces, the drop in SFG intensity is gradual and in agreement with the three broad transitions of PVNODC observed in the bulk. 相似文献
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Biodegradable polyurethane elastomers with potential for applications in medical implants with tunable degradation rate and physical properties were synthesized from reaction of epoxy terminated polyurethanes (EUP) with 1,6-hexamethylene diamine (HMDA) as curing agent. Poly(ε-caprolactone) (PCL) and poly(ethylene glycol) (PEG) as well as 1,6-hexamethylene diisocyanate (HDI) were used for preparation of isocyanate terminated polyurethanes which were subsequently blocked with glycidol to prepare EUPs. All materials were characterized by conventional methods, and their properties were studied fully. Results showed that elastomers based on PEG exhibit superior degradation rate and inferior mechanical properties in comparison to elastomers based on PCL. Optimum degradation rate and mechanical properties were obtained from elastomers made from mixture of PCL and PEG base EUPs. 相似文献
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Efficient oxidation of alcohols with tert-butyl hydroperoxide catalyzed by Mo(CO)6 supported on multiwall carbon nanotubes modified with 4-aminopyridine is reported. The effect of various parameters such as catalyst amount, solvent and oxidant was studied. The catalyst, [Mo(CO)5@APy-MWCNT], showed high activity not only in the oxidation of benzylic and linear alcohols but also in the oxidation of secondary alcohols. The catalyst can be reused several times without significant loss of its activity. 相似文献
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Mohammad Taghi Taghizadeh Nazanin Yeganeh Mostafa Rezaei 《Journal of Thermal Analysis and Calorimetry》2014,118(3):1733-1746
A peak deconvolution procedure used for the analysis of data corresponding to simultaneous overlapping processes begins with separation of individual processes using functions such as Gaussian, Lorentzian, Weibull, and Fraser–Suzuki (FS) followed by application of kinetic analysis methods to the separated peaks. We propose a coupled peak deconvolution procedure to link the parameters of the FS functions of similar peaks in two DTG curves obtained at different linear heating rates, so that the coordinates of each peak can be obtained in a constrained manner. The proposed technique is a kinetic deconvolution method rather than a pure mathematical deconvolution technique. To analyze individual peaks in our study, the non-parametric kinetic and Freidman’s isoconversional methods have been applied to determine kinetic triplet of each process. This technique has been tested with both simulated and experimental data. Using this technique, the effects of molecular weight and degree of hydrolysis of polyvinyl alcohol (PVA) samples on reaction mechanism and activation energy of thermal degradation were studied. The presence of acetate group in the PVA samples causes thermal stability, decreases the rate of main reactions, and increases the activation energy. The results of this study may help tailor heat-resistant materials with proper choice of polymer characteristics. 相似文献
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Mohammad Yeganeh Ghotbi Mohd Zobir bin Hussein Asmah Hj Yahaya 《Journal of Physics and Chemistry of Solids》2009,70(6):948-93
Intercalation of d-gluconate into the interlamellae of zinc-aluminum-layered double hydroxide for the formation of a food additive-inorganic layered nanohybrid was accomplished by both direct (co-precipitation) and indirect (ion-exchange) methods. Powder X-ray diffraction (PXRD) together with CHNS and Fourier transform infrared (FTIR) analyses showed that the hybridization of d-gluconate with pure phase and good crystallinity was successfully accomplished by a direct method within ranges of pH 7.5-10, Zn to Al initial molar ratio of 2-5 and DG concentration of 0.05-0.3 M. The same nanohybrid compound was also prepared using an indirect ion-exchange method by contacting the pre-prepared LDH with 0.1 M DG for 80 min. The basal spacing of the nanohybrid synthesized by the direct method ranged between 9 and 12.0 Å while that synthesized by the indirect ion-exchange method was 14.0 Å. The crystallinity of the latter was higher than the former and it inherited the crystallinity of the precursor. This work shows that a food additive, such as d-gluconate, can be hybridized into an inorganic host for the formation of a new nanohybrid compound, which can be used to regulate the release of acidity in the food industry. 相似文献