Search Results (18)

This study investigates the impact of sulphuric acid concentration (40% vs. 60%) on the extraction of cellulose nanocrystals (CNCs) from alkali-treated sugarcane bagasse (SCB) and their reinforcement in poly(furfuryl) alcohol (PFA) composites. Probing into the physicochemical changes through scanning electron microscopy (SEM) displayed drastic morphological changes, alkali removal of noncellulosic components followed by sulphuric acid hydrolysis further refined cellulose to nanoscale morphologies. The X-ray diffraction (XRD) study showed that after alkali treatment, the crystallinity was significantly higher (65%), and the crystallinity index of CNCs prepared from 40% H₂SO₄ was greater than the CNCs prepared from 60% H₂SO₄ (61%). Fourier transform infrared spectral and thermogravimetric analysis (TGA) suggested that improving the polymeric performance by the incorporation of a CNC resulted in a decrease in the thermal stability of the modified polyelectrolyte, which was largely attributed to higher sulphate esterification achieved at higher acid concentrations. It is possible to use CNCs to achieve higher mechanical performance while also indicating that optimizing thermal properties and mechanical performance of high-performance materials will require an improved understanding of the microstructural parameters governing the polymer–filler interface. This work demonstrates that acid concentration critically balances CNC crystallinity and thermal performance, offering insights for optimizing sustainable nanocomposites. Full article

Following the vision of the European Commission, organisations and workers establishing Industry 5.0 approaches aspire to more future-proof, resilient, sustainable, and human-centred European industries. In this contribution, we explore how technological innovations that contribute to a “win–win” interaction with involved stakeholders may be advanced in a human-centred and transparent proceeding supported by impartial expert translators who provide information or knowledge-based guidance for decision-makers, initiators and implementers in manufacturing innovation driven by sustainability. We elaborate a stepwise procedure for agreeing on milestones and conjointly treading the path towards solving innovation challenges during a translation process. We exemplify the technological aspects of such a process using an innovation case aiming at identifying parameters for enhancements in a vacuum-bagging process applied to the manufacturing of composite parts from prepregs based on condensation-curing matrix resins made from renewable resources. In detail, we present a straightforward design of an experimental approach varying the dwelling temperature and the temperature ramps during the curing of stacked prepregs. In this way, we demonstrate that for cured composites comprising a poly(furfuryl alcohol)-based matrix, the porosity and connected mechanical properties achieved with autoclave-free curing processes sensitively depend on these process parameters. Applying the resulting data-based model is shown to support decision-making for sustainable composite manufacture. Full article

This work describes the effect of nitrogen and oxygen functional groups on the sorption properties of activated carbons produced from furfuryl alcohol. The poly(furfuryl) alcohol underwent carbonization in nitrogen, ammonia, and ammonia and air (in a 3:2 proportion) atmospheres at 600 °C for 4 h. The resulting materials were subsequently activated in a carbon dioxide atmosphere for 1 h at temperatures of 700 °C, 800 °C, 900 °C, and 1000 °C. The X-ray photoelectron spectroscopy (XPS) findings suggest that ammoxidation is superior to amination in terms of nitrogen doping. The maximum nitrogen concentration achieved after ammoxidation was 25 at.%, which decreased to 4 at.% after activation. Additionally, it was observed that oxygen functional groups have a greater impact on porous structure development compared to nitrogen functional groups. The materials activated through carbonization under an ammonia/air atmosphere attained the highest oxygen concentration of roughly 19 at.% as confirmed by XPS. The materials were evaluated for their sorption capacities for carbon dioxide and ethylene, which were 2.2 mmol/g and 2.9 mmol/g, respectively, at 30 °C. Full article

The present study explores the processability and properties of poly(furfuryl alcohol) (PFA)-based composites and draws comparisons with the industry-standard epoxy resin matrices used in printed circuit board applications. A poly(furfuryl alcohol)-based fiberglass prepreg was used to manufacture composite cores laminated with copper foil, which were then integrated in situ into printed circuit board prototypes through industry-typical manufacturing and assembly processes. Both copper cores and printed boards were tested to characterize the electrical properties and overall quality of the prototypes. The fabrication of the copper cores and manufacturing methods of the printed boards are described, alongside the results from the characterization of the cores and the testing of the printed boards. The inherent advantages and disadvantages of the material are highlighted, and areas of improvement for the processability of the material and reliability of the technology are discussed. Full article

Prepregs are commonly fabricated with non-renewable petroleum-based materials. To reduce the impact of the manufacturing of these materials and to produce more sustainable prepregs, this research aims to manufacture poly(furfuryl alcohol)/wood veneer prepregs and their posterior molding in laminate composites. For this purpose, the vacuum infusion process was used to impregnate the wood veneers, and compression molding was applied to manufacture three- and four-layer laminate composites. Scanning electronic microscopy was used to evaluate the impregnation. the laminate manufacturing and differential scanning calorimetry were used to predict the shelf-life of the prepregs, Fourier-transform infrared was used to evaluate the induced hydrolysis resistance, and thermogravimetric analysis was used to determine the thermal degradation of the laminates. Moreover, water uptake and flexural, compressive, and tensile properties were evaluated. The kinetic models were effective and showed a shelf life for the laminates of approximately 30 days in storage at −7 °C, which is an interesting result for laminates with lignocellulosic materials. FTIR proved the laminates’ excellent resistance to hydrolysis. The water absorption, thermal stability, and mechanical properties did not differ as the amount of wood veneer increased, but these results were up to ~40% higher compared with unidirectional wood laminates found in the literature, which is probably linked to the excellent interface observed with SEM. Full article

Poly(furfuryl alcohol) is a thermostable biobased thermoset. The polymerization of furfuryl alcohol (FA) is sensitive to a number of side reactions, mainly the opening of the furan ring into carbonyl species. Such carbonyls can be used to introduce new properties into the PFA materials through derivatization. Hence, better understanding of the furan ring opening is required to develop new applications for PFA. This article studies the structural discrepancies between a PFA prepared in neat conditions versus a PFA prepared in aqueous conditions, i.e., with more carbonyls, through NMR and MALDI ToF. Overall, the PFA prepared in water exhibited a structure more heterogeneous than the PFA prepared in neat conditions. The presence of ketonic derivatives such as enols and ketals were highlighted in the case of the aqueous PFA. In this line, the addition of water at the beginning of the polymerization stimulated the production of aldehydes by a factor two. Finally, the PFA prepared in neat conditions showed terminal lactones instead of aldehydes. Full article

The use of lignocellulosic fillers in rigid polyurethane foams (RPUFs) has been receiving great attention due to their good mechanical and insulation properties and the high sustainable appeal of the obtained cellular polymers, although high water uptakes are found in most of these systems. To mitigate this detrimental effect, RPUFs filled with wood flour (2.5% wt) were fabricated with the addition of furfuryl alcohol (FA) to create a polymer grafted with the wood filler. Two concentrations of FA (10 wt% and 15 wt%) were investigated in relation to the wood flour, and the RPUFs were characterized for cell morphology, density, compressive properties, thermal stability, and water uptake. The introduction of wood flour as a filler decreased the cell size and increased the anisotropy index of the RPUFs and, in addition to that, the FA grafting increased these effects even more. In general, there were no significant changes in both mechanical and thermal properties ascribed to the incorporation of the fillers. On the other hand, a reduction of up to 200% in water uptake was ascribed to the FA-treated fillers. Full article

The chemistry of biomass-derived furans is particularly sensitive to ring openings. These side reactions occur during furfuryl alcohol polymerization. In this work, the furan ring-opening was controlled by changing polymerization conditions, such as varying the type of acidic initiator or the water content. The degree of open structures (DOS) was determined by quantifying the formed carbonyl species by means of quantitative ¹⁹F NMR and potentiometric titration. The progress of polymerization and ring opening were monitored by DSC and FT-IR spectroscopy. The presence of additional water is more determining on ring opening than the nature of the acidic initiator. Qualitative structural assessment by means of ¹³C NMR and FT-IR shows that, depending on the employed conditions, poly(furfuryl alcohol) samples can be classified in two groups. Indeed, either more ester or more ketone side groups are formed as a result of side ring opening reactions. The absence of additional water during FA polymerization preferentially leads to opened structures in the PFA bearing more ester moieties. Full article

Guanyl-urea phosphate (GUP) was introduced into furfurylated wood in order to improve fire retardancy. Modified wood was produced via vacuum-pressure impregnation of the GUP–furfuryl alcohol (FA) aqueous solution, which was then polymerized at elevated temperature. The water leaching resistance of the treated wood was tested according to European standard EN 84, while the leached water was analyzed using ultra-performance liquid chromatography (UPLC) and inductively coupled plasma–sector field mass spectrometry (ICP-SFMS). This new type of furfurylated wood was further characterized in the laboratory by evaluating its morphology and elemental composition using optical microscopy and electron microscopy coupled with energy-dispersive X-ray spectrometry (SEM-EDX). The chemical functionality was detected using infrared spectroscopy (FTIR), and the fire resistance was tested using cone calorimetry. The dimensional stability was evaluated in wet–dry soaking cycle tests, along with the mechanical properties, such as the Brinell hardness and bending strength. The fire retardancy of the modified furfurylated wood indicated that the flammability of wood can be depressed to some extent by introducing GUP. This was reflected in an observed reduction in heat release rate (HRR₂) from 454.8 to 264.9 kW/m², without a reduction in the material properties. In addition, this leaching-resistant furfurylated wood exhibited higher fire retardancy compared to conventional furfurylated wood. A potential method for producing fire-retardant treated furfurylated wood stable to water exposure has been suggested. Full article

The global “carbon emission peak” and “carbon neutrality” strategic goals promote us to replace current petroleum-based resin products with biomass-based resins. The use of technical lignins and hemicellulose-derived furfuryl alcohol in the production of biomass-based resins are among the most promising ways. Deep understanding of the resulting resin structure is a prerequisite for the optimization of biomass-based resins. Herein, a semiquantitative 2D HSQC NMR technique supplemented by the quantitative ³¹P NMR and methoxyl group wet chemistry analysis were employed for the structural elucidation of softwood kraft lignin-based furfuryl alcohol resin (LFA). The LFA was fractionated into water-insoluble (LFA-I) and soluble (LFA-S) parts. The analysis of methoxyl groups showed that the amount of lignin was 85 wt% and 44 wt% in LFA-I and LFA-S fractions, respectively. The HSQC spectra revealed the high diversity of linkages formed between lignin and poly FA (pFA). The HSQC and ³¹P results indicated the formation of new condensed structures, particularly at the 5-position of the aromatic ring. Esterification reactions between carboxyl groups of lignin and hydroxyl groups of pFA could also occur. Furthermore, it was suggested that lignin phenolic hydroxyl oxygen could attack an opened furan ring to form several aryl ethers structures. Therefore, the LFA resin was produced through crosslinking between lignin fragments and pFA chains. Full article

With increasing demand of alternatives to oil-based lightweight materials, the development of tannin-based foams is getting more and more attention. In this paper, an alternative to traditionally used solvent-evaporation in the production of tannin-foams is presented. Mixing the tannin-furanic resin with different amounts of ionic and non-ionic surfactants at high agitational speed allows for the formation of highly porous, mechanically stable tannin-foams. Investigations on the influence of surfactant type and ingredient ratios on the foaming behavior and properties of the final foams were conducted. Materials obtained via this route do present extraordinary compression resistance (about 0.8 MPa), good thermal insulation (40 mW/m·K) and are suitable as a wastewater treatment agent at the end-of-life. It was shown that during mechanical blowing, homogeneous cross-sections and almost perfectly round pores form, leading to the high compression resistance. Investigations by means of Fourier transform infrared and ¹³C nuclear magnetic resonance spectroscopy show that the milder reaction environment leads to more linear poly(furfuryl alcohol)-tannin chains. This new type of tannin foam allows for use in various different fields of application ranging from durable building insulation to wastewater treatment. Full article

Thermosetting resins, such as poly (furfuryl alcohol), are efficient precursors for preparation of carbon membranes with molecular sieving properties. Polymerization of furfuryl alcohol is catalyzed by Bronsted or Lewis acids. FeCl₃, showing Lewis-acid behavior, is an interesting polymerization catalyst, because it gets reduced into metallic iron during pyrolysis of the resin, promoting transformation of amorphous carbon into graphitic domains. The goal of the present work was to examine whether use of FeCl₃ as a polymerization catalyst of furfuryl alcohol–furfural mixtures could lead to preparation of carbon membranes with improved gas separation performance compared to those prepared with use of p-toluenesulfonic acid. The resins were deposited onto tubular porous ceramic supports and pyrolyzed at temperatures in the range of 500–1000 °C. Material characterization was carried out by X-Ray Diffraction, N₂ physisorption, Raman spectroscopy and Scanning Electron Microscopy. The membrane performance was examined using H₂, CO₂ and CH₄ as probe molecules. It was found that the membranes operate mainly via the molecular sieving mechanism and the use of FeCl₃ instead of p-toluenesulfonic acid does not lead to an improvement in the permeation characteristics of the respective membranes. Full article

This study aims to compare the resistance against subterranean termites of wood–polymer composites produced by in situ polymerization. The biological tests were carried out by choice and no-choice feeding tests. Poly (furfuryl alcohol), poly(styrene) and poly (methyl methacrylate) were studied here. They were impregnated into a Brazilian fast-growing pine wood using a vacuum:pressure method and then cured under simple heating. These treatments were evaluated using chemical (by infrared spectroscopy) and morphological (by scanning electron microscopy) analyses. The termite attack was evaluated by mass loss determination and photography. In general, all the treatments were effective in protecting the fast-growing pine wood. Results obtained by no-choice tests indicated that the treatment solution with 75% of furfuryl alcohol was less effective than the others, which indicates that both choice and no-choice tests may be important in a comprehensive study on the termites resistance of solid woods. Full article

The catalytic performance of a series of 1 wt % Pd/C catalysts prepared by the sol-immobilization method has been studied in the liquid-phase hydrogenation of furfural. The temperature range studied was 25–75 °C, keeping the H₂ pressure constant at 5 bar. The effect of the catalyst preparation using different capping agents containing oxygen or nitrogen groups was assessed. Polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), and poly (diallyldimethylammonium chloride) (PDDA) were chosen. The catalysts were characterized by ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The characterization data suggest that the different capping agents affected the initial activity of the catalysts by adjusting the available Pd surface sites, without producing a significant change in the Pd particle size. The different activity of the three catalysts followed the trend: Pd_PVA/C > Pd_PDDA/C > Pd_PVP/C. In terms of selectivity to furfuryl alcohol, the opposite trend has been observed: Pd_PVP/C > Pd_PDDA/C > Pd_PVA/C. The different reactivity has been ascribed to the different shielding effect of the three ligands used; they influence the adsorption of the reactant on Pd active sites. Full article

We demonstrate an accessible and effective technique for exfoliating graphite foil and graphite powder into graphene in a water solution of inorganic salt. In our research, we report an electrochemical cathodic exfoliation in an aqueous solution of Na₂SO₄. After electro-exfoliation, the resulting graphene was premixed with furfuryl alcohol (FA) and an inorganic template (CaCO₃ and Na₂CO₃). Once FA was polymerized to poly(furfuryl alcohol) (PFA), the mixture was carbonized. Carbon bridges originating in thermally-decomposed PFA joined exfoliated graphene flakes and stabilized the whole sponge-type structure after the nano-template was removed. Gases evolved at the graphite electrode (cathode) played an important role in the process of graphene-flake splitting and accelerated the change of graphite into graphene flakes. Starting graphite materials and graphene sponges were characterized using Raman spectroscopy, SEM, high-resolution transmission electron microscopy (HRTEM), elemental analysis, and low-temperature adsorption of nitrogen to determine their structure, morphology, and chemical composition. The discovered manufacturing protocol had a positive influence on the specific surface area and porosity of the sponges. The SEM and HRTEM studies confirmed a high separation degree of graphite and different agglomeration pathways. Raman spectra were analyzed with particular focus on the intensities of I_D and I_G peaks; the graphene-type nature of the sponges was confirmed. Full article