A bio-based polymeric matrix was developed by the copolymerization of a vegetable oil-based epoxy, epoxidized linseed oil (ELO), with dodecenyl succinic anhydride (DDSA). To obtain eco-friendly bio-composites, this matrix was combined with a natural filler: spruce bark powder (SB) with its hydrochar (HC) in various proportions ranged from 1 to 30 wt.%. The reactivities of these formulations were studied by DSC analysis that highlighted that both fillers have a high catalytic effect on the ELO–DDSA crosslinking reaction. The complementary studies by TGA, DMA, tensile tests, water absorption and Shore tests had shown that both HC and SB bring improvements to the mechanical properties of the composites, fulfilling multiple roles: (i) Both act as co-reactants in the copolymerization mechanism; (ii) HC acts as reinforcement, consolidating the network and providing stiffness and rigidity; and (iii) SB acts as plasticizer for reducing the brittle character of the epoxy resins.
Thiswork is focused on the development of sustainable biocomposites based on epoxy bioresin reinforced with a natural porous material (hydrochar, HC) that is the product of spruce bark wastes subjected to hydrothermal decomposition. To identify the influence of hydrochar as a reinforcing material on the designed composites, seven formulations were prepared and tested. An aromatic epoxy monomer derived from wood biomass was used to generate the polymeric matrix, and the formulations were prepared varying the filler concentration from 0 to 30 wt %. The reactivity of these formulations, together with the structural, thermal, and mechanical properties of bio-based resin and biocomposites, are investigated. Surprisingly, the reactivity study performed by differential scanning calorimetry (DSC) revealed that HC has a strong impact on polymerization, leading to an important increase in reaction enthalpy and to a decrease of temperature range. The Fourier Transform Infrared Spectroscopy (FT-IR) investigations confirmed the chemical bonding between the resin and the HC, while the dynamic mechanical analysis (DMA) showed increased values of crosslink density and of storage moduli in the biocomposites products compared to the neat bioresin. Thermogravimetric analysis (TGA) points out that the addition of hydrochar led to an improvement of the thermal stability of the biocomposites compared with the neat resorcinol diglycidyl ether (RDGE)-based resin (T5% = 337 °C) by ≈2–7 °C. Significantly, the biocomposites with 15–20 wt % hydrochar showed a higher stiffness value compared to neat epoxy resin, 92SD vs. 82SD, respectively.
In the context of sustainable use of resources, hydrothermal conversion of biomass has received increased consideration. As well, the hydrochar (the solid C-rich phase that occurs after the process) has caused great interest. In this work, spruce bark (Picea abies) wastes were considered as feedstock and the influence of hydrothermal process parameters (temperature, reaction time, and biomass to water ratio) on the conversion degree has been studied. Using the response surface methodology and MiniTab software, the process parameters were set up and showed that temperature was the significant factor influencing the conversion, while residence time and the solid-to-liquid ratio had a low influence. Furthermore, the chemical (proximate and ultimate analysis), structural (Fourier-transform infrared spectroscopy, scanning electron microscopy) and thermal properties (thermogravimetric analysis) of feedstock and hydrochar were analyzed. Hydrochar obtained at 280 °C, 1 h processing time, and 1/5 solid-to-liquid ratio presented a hydrophobic character, numerous functional groups, a lower O and H content, and an improved C matter, as well as a good thermal stability. Alongside the structural features, these characteristics endorsed this waste-based product for applications other than those already known as a heat source.
The conversion of lignocellulosic waste ascends as a promising path to generate new materials with wide industrial and environmental uses. Pyrolytic biochar (PBc), hydrochar (Hc), and activated hydrochar (AcHc) produced from the waste of Picea Abies bark were considered bio-based sorbents for lead uptake from aqueous effluents. PBc was obtained through slow pyrolysis (550 °C), while Hc resulted under hydrothermal conversion (280 °C). In order to enhance the specific surface, Hc was subjected to a physical activation, resulting AcHc. All three carbonaceous materials were prepared through relatively simple processes from a readily locally available resource. The carbonaceous materials were characterized using infrared spectroscopy and scanning electron microscopy. The Pb (II) removal has been tested in batch mode on a synthetic monocomponent wastewater matrix, as well as on a real mine drainage effluent. A significant effect of pH was observed, while the equilibrium was achieved in a short time, about 60 min for PBc and Hc and 120 min for AcHc. Langmuir model predicted a maximum adsorption capacity of 15.94 mg/g for PBc, 9.99 mg/g for Hc, and 37.46 mg/g for AcHc. All materials studied had good uptake capacities for lead with no drastic effect of typical coexisting species.
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