Eco-friendly materials need "green" fire-retardancy treatments, which offer opportunity for new wood nanotechnologies. Balsa wood (Ochroma pyramidale) was delignified to form a hierarchically structured and nanoporous scaffold mainly composed of cellulose nanofibrils. This nanocellulosic wood scaffold was impregnated with colloidal montmorillonite clay to form a nanostructured wood hybrid with high flame-retardancy. The nanoporous scaffold was characterized by scanning electron microscopy and gas adsorption. Flame-retardancy was evaluated by cone calorimetry, whereas thermal and thermo-oxidative stabilities were assessed by thermogravimetry. The location of well-distributed clay nanoplatelets inside the cell walls was confirmed by energy-dispersive X-ray analysis. This unique nanostructure dramatically increased the thermal stability because of thermal insulation, oxygen depletion, and catalytic charring effects. A coherent organic/inorganic charred residue was formed during combustion, leading to a strongly reduced heat release rate peak and reduced smoke generation.
Here we investigate the relationship between thermomechanical properties and chemical structure of well-characterized lignin-based epoxy resins. For this purpose, technical lignins from eucalyptus and spruce, obtained from the Kraft process, were used. The choice of lignins was based on the expected differences in molecular structure. The lignins were then refined by solvent fractionation, and three fractions with comparable molecular weights were selected to reduce effects of molar mass on the properties of the final thermoset resins. Consequently, any differences in thermomechanical properties are expected to correlate with molecular structure differences between the lignins. Oxirane moieties were selectively introduced to the refined fractions, and the resulting lignin epoxides were subsequently cross-linked with two commercially available polyether diamines (Mn = 2000 and 400) to obtain lignin-based epoxy resins. Molecular-scale characterization of the refined lignins and their derivatives were performed by 31 P NMR, 2D-NMR, and DSC methods to obtain the detailed chemical structure of original and derivatized lignins. The thermosets were studied by DSC, DMA, and tensile tests and demonstrated diverse thermomechanical properties attributed to structural components in lignin and selected amine cross-linker. An epoxy resin with a lignin content of 66% showed a Tg of 79 °C from DMA, Young’s modulus of 1.7 GPa, tensile strength of 66 MPa, and strain to failure of 8%. The effect of molecular lignin structure on thermomechanical properties was analyzed, finding significant differences between the rigid guaiacyl units in spruce lignin compared with sinapyl units in eucalyptus lignin. The methodology points toward rational design of molecularly tailored lignin-based thermosets.
Clay aerogels are foam-like materials with potential to combine high mechanical performance with fire retardancy. However, the compression strength of these aerogels is much lower than theoretically predicted values. High-strength aerogels with more than 95% porosity were prepared from a ternary material system based on poly(vinyl alcohol), montmorillonite clay platelets, and cellulose nanofibrils. A hydrocolloidal suspension of the three components was subjected to freeze-drying so that a low-density aerogel foam was formed. Cell structure was studied by field-emission scanning electron microscopy. Interactions at the molecular scale were observed by X-ray diffraction and Fourier transform infrared spectroscopy. Cross-linking was carried out using glutaraldehyde or borax, and moisture stability was investigated. These biobased ternary aerogels showed compression strength much better than that of previously studied materials and also showed strength higher than that of high-performance sandwich foam cores such as cross-linked polyvinyl chloride foams.
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