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Abstract  

Translational diffusion of poly-2,5-(1,3-phenylene)-1,3,4-oxadiazole (PMOD) in solution in 96% sulphuric acid was studied, and intrinsic viscosity was measured at different stages of thermal degradation. Polymer solution has previously been subjected to heating at temperature ranging from 75 to 104C and then investigated at 26C. A monotonic decrease in intrinsic viscosity and the molecular mass, M, of degraded products with increasing degradation temperature was detected. The rate constant of the degradation process has been obtained from the change in M of the degradation products with time at a fixed solution temperature, and the activation energy of the process was calculated by using the temperature dependence of the rate constant. The activation energy (E =1028 kJ–1 ) is close to that obtained previously for the hydrolysis of poly-2,5-(1,4-phenylene)-1,3,4-oxadiazole (PPOD) in sulphuric acid (106 kJ–1 ), the rate constant being approximately twice in the value.

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Journal of Thermal Analysis and Calorimetry
Authors:
L. Barral
,
J. Cano
,
J. López
,
I. López-Bueno
,
P. Nogueira
,
C. Ramírez
,
A. Torres
, and
M. Abad

Abstract  

The effect of thermal degradation on the mechanical behaviour of a system containing both tetraglycidyl-4-4′-diaminodiphenylmethane (TGDDM) and a multifunctional novolac glycidyl ether (EPN) resins, cured with 4,4′-diaminodiphenylsulphone (DDS) has been studied using dynamic mechanical analysis (DMA) and tensile tests. Different curing paths using the isothermal time-temperature-transformation (TTT) diagram for this system were designed, obtaining thermosetting materials with different conversions. The influences of the degree of cure and of the aging temperature were also studied. The results showed different trends in the dynamic mechanical properties and an increase in the stiffness of the material with increasing aging time. Changes were faster and more intense with the higher temperature.

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Abstract  

Styrene and montmorillonite organically modified with imidazolium surfactants (MMT) at various alkyl chain lengths (C12, C16 and C18) were used to prepare the corresponding PS/MMT/C12, PS/MMT/C16 and PS/MMT/C18 nanocomposites by in situ polymerization. XRD and TEM analyses evidenced the formation of both intercalated and exfoliated structures. The glass transition temperatures (T g) of nanocomposites, as well as that of neat PS, were obtained by DSC measurements. The thermal degradations were carried out in the scanning mode, in both inert and oxidative environments, and the initial temperatures of decomposition (T i) and the apparent activation energies of degradation (E a) were determined. Due to an oxidative degradation mechanism, the T i and E a values in air atmosphere were lower than those under nitrogen. The results indicated that nanocomposites are more thermally stable than polystyrene, and suggested an increasing degree of exfoliation as a function of alkyl chain length of surfactant, associated with enhancing thermal stability.

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Abstract  

The thermal degradation of the aliphatic polyamides 6 and 66 was investigated by means of the combined techniques TA-MS and TA-FTIR. The analyses were performed in three different devices. Sample mass ranged from 13 mg to 1 g and heating rates of 2.6 and 10 K min–1 were used in both air and nitrogen atmospheres. The most important decomposition products were caprolactam for PA 6 and cyclopentanone for PA 66. Evolution of NH3 and HCN was registered. The findings of the two hyphenated techniques led to the same results and complemented each other well. The evolved products were captured and analyzed off-line by GC/MS for further confirmation of results.

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A combination system of thermogravimetric/differential thermal analysis (TG-DTA) and Fourier-transform infrared absorption spectroscopy (FT-IR) was described. This simultaneous TG-DTA/FT-IR technique gave spectroscopic and weight loss information about the thermal degradation process of engineering polyesters; poly(ethylene terephthalate)(PET) and poly(butylene terephthalate)(PBT). The evolved gases from PET were benzoic acid, carbon dioxide and carbon monoxide, while those from PBT were terephthalic acid esters and benzoic acid esters.

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Abstract  

Wood has been treated with guanidine phosphate, guanidine nitrate, guanidine carbonate and guanidine chloride to impart flame retardancy. The samples were subjected to differential thermal analysis (DTA) and thermogravimetry (TG) from ambient temperature to 800°C in air to study their thermal behaviors. From the resulting data, kinetic parameters for different stages of thermal degradation were obtained following the method of Broido. For the decomposition of wood and flame retardant wood, the activation energy was found to decrease from 116 to 54 kJ mol–1; the char yield was found to increase from 5.6 to 34.9%, LOI from 18 to 41.5, which indicated that the flame retardancy of treated wood was improved. Effects of the different compounds on the degradation and flammability of wood have also been proposed.

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Abstract  

The thermal behavior of poly(methyl methacrylate) (PMMA) was studied in the presence of AlBr3 using TG-DTA-DTG, IR and Py-GC-MS techniques. Degradation products were identified. It was found that PMMA started degrading at a lower temperature due to the generation of free radicals (Br), being the product of decomposition of AlBr3. Despite early destabilization of the system, stabilization zone was also highlighted. Flammability test was conducted to check the affectivity of AlBr3. Degradation mechanism has been proposed. Pyrolysis of the system (PMMA–AlBr3) was also monitored by heating it at different temperatures.

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Abstract  

Flow birefringence (FB) has been investigated in solutions of products of hydrolytic degradation of poly(naphthoyleneimide benzimidazole) (PNIB) in 96% sulphuric acid PNIB solutions have previously been subjected to heating at various temperatures from 65 to 120°C and then investigated at 22°C by FB and viscometry. A monotonic decrease in intrinsic viscosity and the molecular weightM of thermal degradation products with increasing degradation temperature was detected. At the same time, the shear optical coefficients in series of products with decreasingM first increases and then, at treatment temperatures exceeding 90°C, decreases with decreasing [ν] in accordance with decreasingM of the product. Possible reasons for the detected anomaly have been discussed.

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Abstract  

The thermal mechanical properties and degradation behaviors were studied on fibers prepared from two high-performance, heterocyclic polymers, poly(p-phenylenebenzobisthiazole) (PBZT) and poly(p-phenylenebenzobisoxazole) (PBZO). Our research demonstrated that these two fibers exhibited excellent mechanical properties and outstanding thermal and thermo-oxidative stability. Their long-term mechanical tensile performance at high temperatures was found to be critically associated with the stability of the C—O or C—S linkage at the heterocyclic rings on these polymers' backbones. PBZO fibers with the C—O linkages displayed substantially higher thermal stability compared to PBZT containing C—S linkages. High resolution pyrolysis-gas chromatography/mass spectrometry provided the information of the pyrolyzates' compositions and distributions as well as their relationships with the structures of PBZT and PBZO. Based on the analysis of the compositions and distributions of all pyrolyzates at different temperatures, it was found that the thermal degradation mechanisms for both of these heterocyclic polymers were identical. Kevlar®-49 fibers were also studied under the same experimental conditions in order to make a comparison of thermo-oxidative stability and long-term mechanical performance at high temperatures with PBZO and PBZT fibers. The data of two high-performance aromatic polyimide fibers were also included as references.

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Abstract  

The thermal analysis methods (TG, DTG and DTA) were used for the investigation of the thermal degradation of some recent manufactured tanned leathers, leathers that are supports of cultural or historical objects (leather from book covers (XVII-XIX centuries); leather from an Austrian belt (Franz Joseph period), Cordoba leather (XVII century), lining leathers), recent and patrimonial parchments and recent extracted collagen (sorts of collagen obtained from bovine leather at different pH-values, bovine collagen with different hydration degree). At progressive heating, all investigated materials exhibit two main successive processes, associated with the dehydration and thermo-oxidative degradation. Each analyzed material has a characteristic thermal analysis curve (TG, DTG and DTA) that can be considered a material 'fingerprint'. This result suggests the use of the thermal analysis methods to identify of leathers from which the patrimonial objects are manufactured. The rate of thermo-oxidation of recent manufactured tanned leathers is substantially higher than the rate of the same process corresponding to naturally aged leathers that exhibit values of the thermo-oxidation rate appropriate to those obtained for parchments and collagens. The rate of thermo-oxidation of leather can thus be used as a criterion to distinguish between recent manufactured leather and patrimonial one.

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