Phosphonium-modified layered silicate epoxy resin nanocomposites were evaluated by testing the thermal/thermo-mechanical properties (differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), torsional pendulum, Sharpy toughness), flammability (limiting oxygen index LOI) and fire behavior (cone calorimeter with different irradiations). The morphology of the composites was determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The drying conditions of phosphonium-modified layered silicate were varied in order to improve the nanocomposite formation and properties. The results were compared with using a commercial ammonium- modified montmorillonite. Enhanced nanocomposite formation was found for the commercial systems due to the amount of excess surfactant, but this effect was overcompensated through the advanced morphology of the phosphonium-modified systems. Several fire retardancy mechanisms and their specific influence on the different fire properties, such as ignitability, flammability, flame spread, total heat release (fire load), and the production of CO and smoke were discussed comprehensively. The main mechanism of layered silicate is a barrier formation influencing the flame spread in developing fires. Several minor mechanisms are significant, but important fire properties such as flammability or fire load are hardly influenced. Hence combinations with aluminum hydroxide and organo-phosphorus flame retardants were evaluated. The combination with aluminum hydroxide was a promising approach since it shows superposition in properties such as the fire load and only in some properties very little antagonism. The combination with an organo-phosphorus flame retardant disillusions, since it was characterized mainly by antagonism
The influence of different organobentonites on the decomposition and the combustion behaviour of an epoxy resin were examined. The epoxy resin is a cationically polymerised cycloaliphatic epoxy resin flexibilised with poly(tetrahydrofuran) (PTHF), with hydroxyl endgroups. The bentonite was modified with either an ammonium or a phosphonium salt. The thermal decomposition of the PTHF induced by the initiator, used for the cationic polymerisation, did neither take place for the nanocomposite based on the ammonium bentonite nor for that based on the phosphonium bentonite. This improved decomposition characteristic lead to a larger time to ignition for both kinds of nanocomposites compared to the not modified polymer, which is not the case for other polymer/clay nanocomposites described in the literature. The fire behaviour was investigated using limiting oxygen index (LOI), a horizontal burner test and a cone calorimeter. The forced flaming conditions in the cone calorimeter were varied using different external heat fluxes between 30 and 70 kW · m−2. The fire behaviour of the nanocomposites was improved in comparison to the polymer, and phosphonium bentonite was superior to ammonium bentonite. The main mechanism is a barrier formation resulting in a reduction of the fire growth rate, which was more pronounced in the case of high external heat fluxes.
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An overview about the use of nanoparticles in epoxy resins is given. Deaggregated fumed silica, sol gel materials and other spheroidic nanoparticles improved the abrasion resistance and the mechanical properties of filled epoxides, and several properties can be improved by specific particles. Combustion properties, strength and permeation can be improved by organically modified layered silicates. The proper characterisation of the nanocomposites is still an art. TEM analysis of the cured materials and light scattering with 3D cross‐correlation for the liquid samples were sufficient methods for the characterisation of filled epoxides.
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