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  • 1.
    Maršík, Dominik
    et al.
    Department of Biotechnology, University of Chemistry and Technology, 166 28 Prague, Czech Republic.
    Thoresen, Petter Paulsen
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Maťátková, Olga
    Department of Biotechnology, University of Chemistry and Technology, 166 28 Prague, Czech Republic.
    Masák, Jan
    Department of Biotechnology, University of Chemistry and Technology, 166 28 Prague, Czech Republic.
    Sialini, Pavel
    Central Laboratories, University of Chemistry and Technology, 166 28 Prague, Czech Republic.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Tsikourkitoudi, Vasiliki
    Department of Microbiology, Tumor and Cell Biology, Karolinska Institutet, 171 77 Stockholm, Sweden.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Jarošová Kolouchová, Irena
    Department of Biotechnology, University of Chemistry and Technology, 166 28 Prague, Czech Republic.
    Synthesis and Characterization of Lignin-Silver Nanoparticles2024In: Molecules, ISSN 1431-5157, E-ISSN 1420-3049, Vol. 29, no 10, article id 2360Article in journal (Refereed)
    Abstract [en]

    Metal nanoparticle synthesis via environmentally friendly methods is gaining interest for their potential advantages over conventional physico-chemical approaches. Herein, we propose a robust green synthesis route for lignin-modified silver nanoparticles, utilizing the recovery of lignin as a renewable raw material and exploring its application in valuable areas. Through a systematic approach combining UV-Vis spectroscopy with AAS and DLS, we identified repeatable and scalable reaction conditions in an aqueous solution at pH 11 for homogeneous silver nanoparticles with high uniformity. The TEM median sizes ranged from 12 to 15 nm with circularity between 0.985 and 0.993. The silver nanoparticles yield exceeded 0.010 mol L−1, comparable with traditional physico-chemical methods, with a minimal loss of silver precursor ranging between 0.5 and 3.9%. Characterization by XRD and XPS revealed the presence of Ag-O bonding involving lignin functional groups on the pure face-centered cubic structure of metallic silver. Moreover, the lignin-modified silver nanoparticles generated a localized thermal effect upon near-infrared laser irradiation (808 nm), potentially allowing for targeted applications in the biomedical field. Our study showcases the potential of lignin as a renewable reducing and capping agent for silver nanoparticle synthesis, addressing some shortcomings of green synthesis approaches and contributing to the development of suitable nanomaterials.

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  • 2.
    Moncao, Maxwel
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Paulsen Thoresen, Petter
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Wretborn, Tobias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Lange, Heiko
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Department of Earth and Environmental Sciences, University of Milano-Bicocca, Piazza della Scienza 1, 20126 Milan, Italy; NBFC – National Biodiversity Future Center, 90133 Palermo, Italy .
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    A novel biorefinery concept based on marginally used halophyte biomass2023In: Sustainable Energy & Fuels, E-ISSN 2398-4902, Vol. 7, no 16, p. 3902-3918Article in journal (Refereed)
    Abstract [en]

    Halophytes have major potential in biorefinery as these salt tolerant crops have prospects as an alternative biomass to meet energy demands and provide value-added products with reduced effects in terms of food security and environmental damage when compared to other crops. In this study, we investigated the effects of organosolv pretreatment process parameters on the fractionation of residual fibers from pressed Salicornia ramosissima and how it affects the fractions of cellulose, lignin, and hemicelluloses. Pretreated pulps contained as high as 48.95% w/w cellulose, a 2.9-fold increase from the untreated fibers. The delignification of pulp was as high as 75.01% and hemicellulose removal reached 96.38%. The hemicellulose fractions contained as high as 78.49% oligomers and we identified up to 30.4% linear xylooligosaccharides in the composition. The majority of the fragments of hemicelluloses had molecular weights lower than 1000 Da. Isolated lignin samples had in most cases very low sugar and ash contamination with a reduced molecular weight. The typical G-, S-, and H-type aromatic units were detected in the lignin, together with & beta;-O-4 & PRIME;, & beta;-5 & PRIME;, & beta;-& beta;& PRIME;, and dibenzodioxocine links. The results suggest a novel applicability of S. ramosissima in a biorefinery context with fractionation deriving building blocks for value added products.

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  • 3.
    Paulsen Thoresen, Petter
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Structure and property oriented organosolv lignin extraction2024Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    In this Thesis, organosolv fractionation of softwood (spruce), hardwood (birch and beech), and herbaceous crops (wheat straw) was performed by applying various organosolv process conditions. Among these were a novel steam-explosion/organosolv hybrid mode, and two ternary solvent systems utilizing water/ethanol/acetone, and water/acetone/acetic acid. In addition, the effect of using inorganic acidic catalyst (H2SO4) was investigated for all raw material classes. Also, alkaline catalyst (NaOH) was investigated for wheat straw due to its reported high content of inorganics which presence adds additional structural complexity to the lignocellulosic recalcitrance. Following the organosolv fractionation, structural characterization was performed (content of cellulose, hemicellulose, lignin) in the isolated product fractions. Additionally, in-depth characterization of the isolated lignins was performed by combining Pyrolysis-Gas Chromatography Mass Spectroscopy (Pyr-GC/MS), Gel Permeation Chromatography (GPC), and different modes of Nuclear Magnetic Resonance (NMR; 13C, 1H-13C, 31P). Complementary analytics, such as content of monomeric/oligomeric sugars, dehydration products, total phenolics, and Size-Exclusion Chromatography (SEC) of the isolated product liquor, were performed to provide a comprehensive understanding of the process. Special attention was given the lignin structural changes occurring throughout the organosolv process. This was done as the use of lignin for higher-value application is considered crucial for the economic viability and development of a modern biorefinery. For this reason, significant focus was given to study how the lignin characteristics translate into physical properties such as solubility. The latter property was measured through solubility trials in binary aqueous acetone solutions, as well as solvent-based fractionation (acetone-water system). A coherent picture was aimed for, where structural motifs and lignin characteristics were correlated to reductions/enhancements in solubility at various water contents. To finally bridge this with a potential down-stream application, DPPH radical scavenging was performed in DMSO with and without intercalating Lithium Bromide (LiBr) for a selection of organosolv lignins, as well as their acetone/water fractionated lignins. This was complemented with a UV absorption study of the lignin solutions.The results provide a descriptive span of chemical characteristics related to organosolv lignins, where they range between highly native, to non-native. Whereas the former lignins are largely comprised of inter-unit motifs such as β-O-4’, β-β’ and β-5’, the non-native lignins are instead better characterized by a high content of oxidized sidechains, biaryls and bifurans, as well as showing strong indications of having quaternary cross-linkers originating from ketone functionalities. The ketones are also found to undergo aldol condensation with aldehydes formed throughout the process. Interestingly, these two extremes in lignin characteristics yield highly varying physical properties, where the predominantly native and non-native lignins for example display low and high solubility in pure acetone, respectively. Simultaneously, the latter is more prone towards water-induced precipitation, whereas the former instead require water to display complete (~100%) solubility at specific concentrations. These properties and findings are eventually consistent with recent literature where lignin aggregates also dominate their dissolved state, and the interunit motifs dictate the affinity on forming such aggregates which are important for both their dissolution, precipitation, but also their display of functionality such as antioxidant activity.                    

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  • 4.
    Paulsen Thoresen, Petter
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Lange, Heiko
    Department of Pharmacy, University of Naples’Federico II’, Via Domenico Montesano 49, 80131 Naples, Italy.
    Crestini, Claudia
    Department of Molecular Science and Nanosystems, University of Venice Ca’ Foscari, Via Torino 155, 30170 Venice Mestre, Italy.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Characterization of Organosolv Birch Lignins: Toward Application-Specific Lignin Production2021In: ACS Omega, E-ISSN 2470-1343, Vol. 6, no 6, p. 4374-4385Article in journal (Refereed)
    Abstract [en]

    Organosolv pretreatment represents one of the most promising biomass valorization strategies for renewable carbon-based products; meanwhile, there is an overall lack of holistic approach to how extraction conditions affect the suitable end-usages. In this context, lignin extracted from silver birch (Betula pendula L.) by a novel hybrid organosolv/steam-explosion treatment at varying process conditions (EtOH %; time; catalyst %) was analyzed by quantitative NMR (1H–13C HSQC; 13C NMR; 31P NMR), gel permeation chromatography, Fourier transform infrared (FT-IR), Pyr-gas chromatography–mass spectroscopy (GC/MS), and thermogravimetric analysis, and the physicochemical characteristics of the lignins were discussed regarding their potential usages. Characteristic lignin interunit bonding motifs, such as β-O-4′, β-β′, and β-5′, were found to dominate in the extracted lignins, with their abundance varying with treatment conditions. Low-molecular-weight lignins with fairly unaltered characteristics were generated via extraction with the highest ethanol content potentially suitable for subsequent production of free phenolics. Furthermore, β-β′ and β-5′ structures were predominant at higher acid catalyst contents and prolonged treatment times. Higher acid catalyst content led to oxidation and ethoxylation of side-chains, with the concomitant gradual disappearance of p-hydroxycinnamyl alcohol and cinnamaldehyde. This said, the increasing application of acid generated a broad set of lignin characteristics with potential applications such as antioxidants, carbon fiber, nanoparticles, and water remediation purposes.

  • 5.
    Paulsen Thoresen, Petter
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Lange, Heiko
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Department of Earth and Environmental Sciences, University of Milano-Bicocca, Piazza della Scienza 1, 20126 Milan, Italy; NBFC – National Biodiversity Future Center, 90133 Palermo, Italy.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Covalently bound humin-lignin hybrids as important novel substructures in organosolv spruce lignins2023In: International Journal of Biological Macromolecules, ISSN 0141-8130, E-ISSN 1879-0003, Vol. 233, article id 123471Article in journal (Refereed)
    Abstract [en]

    Organosolv lignins (OSLs) are important byproducts of the cellulose-centred biorefinery that need to be converted in high value-added products for economic viability. Yet, OSLs occasionally display characteristics that are unexpected looking at the lignin motifs present. Applying advanced NMR, GPC, and thermal analyses, isolated spruce lignins were analysed to correlate organosolv process severity to the structural details for delineating potential valorisations. Very mild conditions were found to not fractionate the biomass, causing a mix of sugars, lignin-carbohydrate complexes (LCCs), and corresponding dehydration/degradation products and including pseudo-lignins. Employing only slightly harsher conditions promote fractionation, but also formation of sugar degradation structures that covalently incorporate into the oligomeric and polymeric lignin structures, causing the isolated organosolv lignins to contain lignin-humin hybrid (HLH) structures not yet evidenced as such in organosolv lignins. These structures effortlessly explain observed unexpected solubility issues and unusual thermal responses, and their presence might have to be acknowledged in downstream lignin valorisation.

  • 6.
    Paulsen Thoresen, Petter
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Lange, Heiko
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Department of Earth and Environmental Sciences, University of Milano-Bicocca, Piazza della Scienza 1, 20126 Milan, Italy.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Role and importance of solvents for the fractionation of lignocellulosic biomass2023In: Bioresource Technology, ISSN 0960-8524, E-ISSN 1873-2976, Vol. 369, article id 128447Article, review/survey (Refereed)
    Abstract [en]

    Lignocellulosic biomass is one of the most important renewable materials to replace carbon-based fossil resources. Solvent-based fractionation is a promising route for fractionation of biomass into its major components. Processing is governed by the employed solvent-systems properties. This review sheds light on the factors governing both dissolution and potential reactivities of the chemical structures present in lignocellulose, highlighting how proper understanding of the underlying mechanisms and interactions between solute and solvent help to choose proper systems for specific fractionation needs. Structural and chemical differences between the carbohydrate-based structural polymers and lignin require very different solvents capabilities in terms of causing and eventually stabilizing conformational changes and consequent activation of bonds to be cleaved by other active components in the. A consideration of potential depolymerization events during dissolution and energetic aspects of the dissolution process considering the contribution of polymer functionalities allow for a mapping of solvent suitability for biomass fractionation.

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  • 7.
    Paulsen Thoresen, Petter
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Recent advances in organosolv fractionation: Towards biomass fractionation technology of the future2020In: Bioresource Technology, ISSN 0960-8524, E-ISSN 1873-2976, Vol. 306, article id 123189Article, review/survey (Refereed)
    Abstract [en]

    Organosolv treatment is among the most promising strategies for valorising lignocellulosic biomass and could facilitate the transition towards enhanced utilization of renewable feedstocks. However, issues such as inefficient solvent recycle and fractionation has to be overcome. The present review aims to address these issues and discuss the role of the components present during organosolv treatment and their influence on the overall process. Thus, the review focuses not only on how the choice of solvent and catalyst affects lignocellulosic fractionation, but also on how the choice of treatment liquor influences the possibility for solvent recycling and product isolation. Several organic solvents have been investigated in combination with water and acid/base catalysts; however, the lack of a holistic approach often compromises the performance of the different operational units. Thus, an economically viable organosolv process should optimize biomass fractionation, product isolation, and solvent recycling.

  • 8.
    Thoresen, Petter Paulsen
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Delgado Vellosillo, Irene
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Lange, Heiko
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Department of Earth and Environmental Sciences, University of Milano-Bicocca, Piazza della Scienza 1, 20126 Milan, Italy; NBFC − National Biodiversity Future Center, 90133 Palermo, Italy.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Furan Distribution as a Severity Indicator upon Organosolv Fractionation of Hardwood Sawdust through a Novel Ternary Solvent System2024In: ACS Sustainable Chemistry and Engineering, E-ISSN 2168-0485, Vol. 12, no 4, p. 1666-1680Article in journal (Refereed)
    Abstract [en]

    Beech sawdust was treated with a ternary solvent system based on binary aqueous ethanol with partial substitution of ethanol by acetone at four different water contents (60, 50, 40, and 30%v/v). In addition to standard, i.e., noncatalyzed treatments, the application of inorganic acid in the form of 20 mm H2SO4 was evaluated. The various solvent systems were applied at 180 °C for 60 min. The obtained biomass fractions were characterized by standard biomass compositional methods, i.e., sugar monomer and oligomer contents, dehydration product contents of the aqueous product, and lignin, cellulose, and hemicellulose contents in isolated solid fractions. More advanced analyses were performed on the lignin fractions, including quantitative 13C NMR analyses, 1H–13C HSQC analysis, size exclusion chromatography, and pyrolysis-GC/MS, and the aqueous product, in the form of size exclusion chromatography and determination of total phenol contents. The picture emerging from the thorough analytical investigation performed on the lignin fractions is consistent with that resulting from the characterization of the other fractions: results point toward greater deconstruction of the lignocellulosic recalcitrance upon higher organic solvent content, replacing ethanol with acetone during the extraction, and upon addition of mineral acid. A pulp with cellulose content of 94.23 wt % and 95% delignification was obtained for the treatment employing a 55/30/15 EtOH/water/acetone mixture alongside 20 mm H2SO4. Furthermore, the results indicate the formation of two types of organosolv furan families during treatment, which differ in the substitution of their C1 and C5. While the traditional lignin aryl–ether linkages present themselves as indicators for process severity for the nonacid catalyzed systems, the distribution of these furan types can be applied as a severity indicator upon employment of H2SO4, including their presence in the isolated lignin fractions.

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  • 9.
    Thoresen, Petter Paulsen
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Fahrni, Jonas
    RISE Processum AB, Department Biorefinery and Energy, Division of Bioeconomy and Health, Research Institute of Sweden, 981 22 Örnsköldsvik, Sweden.
    Lange, Heiko
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Department of Earth and Environmental Sciences, University of Milano-Bicocca, Piazza della Scienza 1, 20126 Milan, Italy; NBFC – National Biodiversity Future Center, 90133 Palermo, Italy.
    Hertzog, Jasmine
    Université de Lorraine, LCP-A2MC, 57000 Metz, France.
    Carre, Vincent
    Université de Lorraine, LCP-A2MC, 57000 Metz, France.
    Zhou, Ming
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Trubetskaya, Anna
    Department of Bioscieces, Nord University, 7713 Steinkjer, Norway.
    Aubriet, Frederic
    Université de Lorraine, LCP-A2MC, 57000 Metz, France.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Gustafsson, Tomas
    RISE Processum AB, Department Biorefinery and Energy, Division of Bioeconomy and Health, Research Institute of Sweden, 981 22 Örnsköldsvik, Sweden.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    On the understanding of bio-oil formation from the hydrothermal liquefaction of organosolv lignin isolated from softwood and hardwood sawdust2023In: Sustainable Energy & Fuels, E-ISSN 2398-4902, Vol. 7, no 22, p. 5361-5373Article in journal (Refereed)
    Abstract [en]

    Conversion of organosolv lignins isolated with and without an inorganic acid catalyst (H2SO4) from hard- and softwood (birch and spruce) into bio-oil through hydrothermal liquefaction has been investigated. Furthermore, fractions of the isolated bio-oils were catalytically deoxygenated to improve the bio-oil properties. As elucidated through NMR, both biomass source and extraction mode influence the bio-oil product distribution. Depending on whether the lignins carry a high content of native structures, or are depolymerized and subsequently condensed in the presence of sugar dehydration products, will dictate heavy oil (HO) and light oil (LO) distribution, and skew the HO product composition, which again will influence the requirements upon catalytical deoxygenation.

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  • 10.
    Wu, Zhipeng
    et al.
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Machine Elements.
    Paulsen Thoresen, Petter
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Shi, Yijun
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Machine Elements.
    Facile Synthesis of Lignin-Castor Oil-Based Oleogels as Green Lubricating Greases with Excellent Lubricating and Antioxidation Properties2023In: ACS Sustainable Chemistry and Engineering, E-ISSN 2168-0485, Vol. 11, no 34, p. 12478-12858Article in journal (Refereed)
    Abstract [en]

    In this study, a facile synthesis method was employed to create lignin-castor oil-based oleogels by modifying organic lignin with two silane coupling agents. The resulting oleogels demonstrated outstanding lubricating and antioxidation properties, establishing them as promising green lubricating greases. Compared with the pure castor oil, the oxidation induction time (OIT) value of the synthesized oleogels was significantly increased from 20 s (pure castor oil) to 1959 s (oleogel with 20 wt % lignin), indicating an effective improvement of the oxidation resistance. The steel contacts lubricated by the synthesized oleogel also had lower wear than those lubricated by pure castor oil, signifying the better lubricating properties of oleogels. The oleogel with 20 wt % lignin showed the lowest wear, which was around 64% lower than that of pure castor oil. The exceptional performance and environmentally sustainable composition of these oleogels, with the biomass content exceeding 80%, allow them to be used as green lubricating greases for industrial applications. Overall, this study provides valuable insights into the development of high-performance, eco-friendly lubricants.

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