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Brito Jr. C.A.R.,Brazilian Technological Institute of Aeronautics | Fleming R.R.,Brazilian Technological Institute of Aeronautics | Pardini L.C.,DCTA IAE | Alves N.P.,Quimlab Cientifica Ltda

This paper presents results from thermal analysis of polyacrylonitrile (PAN) plasticized with glycerin, where effects from the high purity glycerin (glycerol) and other additives to glycol were studied. Using differential scanning calorimetry (DSC) at high heating rate (90 °C/min) and inert atmosphere, we observed a decrease in the melting temperature of PAN (from 290 °C to 217 °C) owing to the presence of glycerol. The Kissinger's method was used to investigate the kinetics of thermal degradation for acrylonitrile (AN) with vinyl acetate (AV). The apparent activation energy for the copolymer AN/AV was calculated as 149 kJ.mol-1. The AV comonomer resulted in a lower degradation enthalpy for the copolymer AN/AV (353 J.g-1) compared with the comonomers comprising a precursor PAN for carbon fibers (988 J.g-1). Source

Ribeiro R.F.,Brazilian Technological Institute of Aeronautics | Pardini L.C.,Brazilian Technological Institute of Aeronautics | Alves N.P.,Quimlab Cientifica Ltda | Junior C.A.R.B.,Federal University of Maranhao

A low cost and environmental friendly extrusion process of the Polyacrylonitrile (PAN) polymer was viabilized by using the 1,2,3-propanetriol (glycerol) as a plasticizer. The characterization of the fibers obtained by this process was the object of study in the present work. The PAN fibers were heat treated in the range of 200 °C to 300 °C, which is the temperature range related to the stabilization/oxidation step. This is a limiting phase during the carbon fiber processing. The characterization of the fibers was made using infrared spectroscopy, thermal analysis and microscopy. TGA revealed that the degradation of the extruded PAN co-VA fibers between 250 °C and 350 °C, corresponded to a 9% weight loss to samples analyzed under oxidizing atmosphere and 18% when the samples were analyzed under inert atmosphere. DSC showed that the exothermic reactions on the extruded PAN co-VA fibers under oxidizing synthetic air was broader and the cyclization started at a lower temperature compared under inert atmosphere. Furthermore, FT-IR analysis correlated with thermal anlysis showed that the stabilization/oxidation process of the extruded PAN fiber were coherent with other works that used PAN fibers obtained by other spinning processes. Source

Brito C.A.R.,University | Pardini L.C.,IAE | Alves N.P.,Quimlab Cientifica Ltda

This paper summarizes the conventional spinning processes used to obtain polyacrylonitrile (PAN). A brief history of the development of PAN fiber is presented. The employability of PAN fibers is attributed mainly to the textile sector and aviation (as main precursor for carbon fibers). Currently, the wet spinning process became the only means of industrial production of PAN fibers, which employs DMF (dimethylformamide) as the main solvent for this technique of spinning. We describe a new method of spinning of PAN with no need of using highly toxic solvents. This innovative technology enables spinning by melting PAN using glycerin (from biodiesel production) as the primary plasticizer. Source

Fleming R.,Brazilian Technological Institute of Aeronautics | Pardini L.C.,Brazilian Technological Institute of Aeronautics | Alves N.,Quimlab Cientifica Ltda | Garcia E.,Quimlab Cientifica Ltda | Brito Jr. C.,University Uni

Polyacrylonitrile fiber encompasses a broad range of products based on acrylonitrile (AN) which is readily copolymerized with a wide range of ethylenic unsaturated monomers giving rise to polymers with different characteristics and applications. Such products can be designed for cost-effective, flame and heat resistant solutions for the textile industry, aircraft and automotive markets. In the present work acrylonitrile was copolymerized with vinylidene chloride (VDC) by conventional suspension polymerization process via redox system, with an initial content of 10%/mass of the VDC monomer. The copolymer average molecular weight was obtained by Gel Permeation Chromatography (GPC) and by intrinsic viscosity analysis. To control the polymerization process continuously, qualitative and quantitative analysis of the chloride content in the PAN AN/VDC copolymer structure was accomplished by using X-ray fluorescence and potentiometric titration techniques. A good correlation was found between these two techniques, leading to a straightforward verification of VDC in the polymer structure. The thermal behavior of PAN AN/VDC copolymer was performed by Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA). The results showed that VDC monomers exhibited a nearly stoichiometric reaction with acrylonitrile, copolymerizing about 90% of its initial mass. VDC changed significantly the polyacrylonitrile thermal behavior, decreasing the polymer degradation temperature by about 40-50°C. Source

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