The overview of the literature reveals the lack of comprehensive study on the effect of clay minerals in flame-retarded polylactic acid (PLA) composites. This research focuses on sepiolite (SEP) and montmorillonite (MMT) clay minerals and their impact on ammonium polyphosphate (APP)-based intumescent flame-retardant (IFR) system in PLA. The effects of the clay mineral types, their surface modification (O-SEP and O-MMT, respectively) and their concentration in PLA/APP composites on the flame-retardant properties were comprehensively evaluated through thermal and flammability tests. Overall, the sepiolite-containing samples showed the greatest decrease in pHRR and THR values at the 3 m/m% loading level. The sepiolites showed stronger interfacial interactions with the PLA matrix than the montmorillonites, and the organomodification proved to improve the compatibility of both types of clay minerals according to the dynamic mechanical analysis (DMA) results. Yet, the organomodification had a contradictory effect on the flame-retardant properties. In the case of sepiolites, it proved to be beneficial as the O-SEP added composite achieved a 60% decrease in the pHRR value and reduced the THR value to 60%. For montmorillonites, the improved compatibility by the organomodification with the PLA matrix seemed to hinder its flame-retardant effectiveness, as the critical point to its flame-retardant mechanism is the rapid migration and accumulation of the clay minerals towards the surface of the polymer.
As polypropylene (PP) has no charring ability on its own due to the lack of hydroxyl functional groups, the flame retardant system needs the addition of carbonizing agent in a relatively great amount. Ammonium-polyphosphate (APP), a conventional flame retardant additive was modified by microencapsulation with a sorbitol-based bioepoxy resin shell to create an intumescent flame retardant system with enhanced charring ability for PP. The flame retardant efficiency of the microencapsulated additive, which contains all the components needed in an effective intumescent flame retardant system, was evaluated in PP matrix at different loadings.When compared to the physical mixture of the component, the microencapsuated form of APP (MCAPP) was found to have improved flame retardant efficiency in PP. The LOI values of the MCAPP containing PP samples increased by 8–11 V/V% besides achieved V-0 classification according to the UL94 test. During cone calorimeter tests, the burning intensity was reduced (peak of heat release rate decreased by 20–35% and shifted in time), increased amount of charred residue was obtained, and based on the calculated Flame Retardancy Index (FRI) “Excellent” fire performance was achieved when MCAPP was used. The improved flame retardant performance is attributed to the effective interaction between the APP core and the readily available carbonizing shell, which promoted the formation of increased amount of char accompanied with improved heat protecting and barrier efficiency.
Poisoning effect of nitrogen on heterogeneous, supported precious metal catalysts, along with their recycling, was further examined in the liquid-phase hydrogenation of 1-methylpyrrole (MP) to 1-methylpyrrolidine (MPD) over rhodium on carbon or γ-alumina, in methanol, under non-acidic conditions, at 25–50 °C and 10 bar. Reusing a spent, unregenerated 5% Rh/C or 5% Rh/γ-Al2O3 catalyst, it was found that the conversion of this model substrate and the activity of the catalyst were strongly dependent on the amount of catalyst, the type of support, the catalyst pre- or after-treatment, the temperature, and the number of recycling, respectively. An unexpected catalytic behaviour of rhodium was observed when it was used in a prehydrogenated form, because no complete conversion of MP was achieved over even the fresh Rh/C or Rh/γ-Al2O3, contrary to the untreated one. In addition, there was a significant difference in the reusability and activity of these rhodium catalysts, depending on their supports (activated carbon, γ-alumina). These diversions were elucidated by applying dispersion (O2- and H2-titration), temperature-programmed desorption of ammonia (NH3-TPD), and transmission electron microscopy (TEM) measurements.
In the flame retardancy of the biopolymer matrix and natural fibre reinforcement containing green composites, researchers face multiple challenges, such as low thermal stability, the candlewick effect of fibres and compatibility issues. Cellulosic fibres have been shown to have char-promoting properties and to advantageously interact with intumescent systems. In this work, melamine-polyphosphate was combined with neat or flame-retardant-treated cellulosic fibres differing in fibre length to obtain intumescent flame retarded poly(lactic acid) composites. The effect of the cellulose fibre length was evaluated in both forms. The structure-property relationships were evaluated by thermal and flammability test methods. It was found that the formation and the structure of the fire-protecting char are influenced by the length of the cellulose fibres, and thus it noticeably affects the effectiveness of the flame-retardant system. Cellulose fibres with an average length of 30–60 µm were found to contribute the best to the formation of an integrated fibrous-intumescent char structure with enhanced barrier characteristics.
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