We discussed about the influence of extraction mode on the flaxseed gums composition and their thermal stabilities. In order to do so, flaxseed gum was extracted by both classical magnetic stirring method and ultrasonic-assisted extraction (UAE). As a function of time, protein content, gum yield, pH values were evaluated and samples were characterized by 1H and 13C nuclear magnetic resonance (NMR) experiments as well as scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The flaxseed gum extracted in aqueous solution correspond to a mixture of different components, including polysaccharides, proteins and sometimes lignan derivatives. It is found that the protein and gum contents increase with the extraction duration for both the ultrasonic assisted and the traditional extraction while the pH decreases at the same time. As expected, compared to traditional magnetic stirring method, ultrasonic assisted extraction method can significantly enhance the yield of polysaccharides, lignans and proteins. The variation of pH is correlated to the increase of lignan molecules in the extracted samples. For thermic methods, SEM experiments showed that lignan derivatives which ester-bonded to polysaccharides associated to proteins are responsible to the formation of globular aggregates. Supplementary rod-like molecular organization were obtained from UAE and questions on the nature of the amphiphilic mesogen carbohydrate structures.
The substitution of toxic precursors such as bisphenol A by renewable and safer molecules has become a major challenge. To overcome this challenge, the 12 principles of green chemistry should be taken into account in the development of future sustainable chemicals and processes. In this context, this paper reports the highly efficient synthesis of oligo-isosorbide glycidyl ethers from bio-based starting materials by a rapid one-pot heterogeneous ultrasound-assisted synthesis. It was demonstrated that the use of high-power ultrasound in solvent-free conditions with sodium hydroxide microbeads led for the first time to a fully epoxidated prepolymer with excellent epoxy equivalent weight (EEW). The structure of the epoxy precursor was characterized by FT-IR, NMR spectroscopy and high-resolution mass spectrometry (HRMS). The efficiency of the ultrasound-assisted synthesis was attributed to the physical effects caused by micro-jets on the surface of the solid sodium hydroxide microspheres following the asymmetrical collapse of cavitation bubbles.
In the present work, an innovative range of foams based on flax gum-filled epoxy resin was developed, reinforced or not by flax fibers. Foams and composites with different gum and epoxy resin contents were produced and their mechanical and thermal performances were characterized. To enhance the organic flax gum filler’s cross-linking, we exploited the oxidized components’ reactivity with the amine hardener (isophorone diamine). We compared the materials obtained with those derived from the native components. The flax gum and fibers were primarily characterized by chemical analysis, NMR, and FTIR to evaluate the mild oxidation of the native materials. The formation of chemical bonds between the oxidized polymer chains, epoxy resin, and hardener was evidenced by FTIR, and the materials were then studied by SEM and X-ray computed micro-tomography (CT) and submitted to mechanical and thermal tests. The relevance of the oxidation treatment was highlighted through a significant increase in density and mechanical performance (+36% and +81%, respectively, for the 100% flax gum material). The positive effect of the flax fibers on homogeneity evidenced through micro-CT analysis was also clearly addressed. This set of promising results paves the way for the future development of fully flax-based insulation composite materials.
In the present work, an innovative range of foams, based on flax gum-filled epoxy resin was developed, reinforced or not by flax fibers. Foams and composites with different gum and epoxy resin contents were produced and characterized for mechanical and thermal performances. To enhance the organic flax gum filler's cross-linking, we exploited the oxidized components' reactivity with the amine hardener (isophorone diamine). We compared the materials obtained with those derived from the native components. Flax gum and fibers were primarily characterized by chemical analysis, NMR, and FTIR to evaluate the mild oxidation of native materials. The formation of chemical bonds between oxidized polymer chains, epoxy resin, and hardener has been evidenced by FTIR, and the materials were then studied by SEM, X-ray computed micro-tomography (CT), and submitted to mechanical and thermal tests. The relevance of oxidation treatment was highlighted, through a significant increase in density and mechanical performances (+36% and +81%, respectively for the 100% flax gum material). The positive effect of flax fibers on homogeneity evidenced through micro-CT analysis was also clearly addressed. This set of promising results paves the way for future development of fully flax-based insulation composite materials.