@article {1847, title = { Characterization and 3D printability of poly (lactic acid)/acetylated tannin composites }, journal = { INDUSTRIAL CROPS AND PRODUCTS }, volume = {149}, year = {2020}, abstract = {

In this study, a three-dimensional (3D) printing filament prepared from poly (lactic acid) (PLA) and acetylated tannin via a twin-screw extruder was reported. The impact of acetylated tannin loading content on the final properties of the resulting composite materials and their 3D printability were investigated. The experimental results indicate that PLA can be compounded with up to 20 wt\% acetylated tannin without any obvious deterioration in the tensile property. The resulting composites acquired better degradation rate in aquatic system compared with neat PLA, especially in alkaline medium. Moreover, all composites are printable and showed generally good printing quality with brown color, however, this is limited to temperatures reasonably below 220 degrees C to avoid printing defects, especially at high loadings of acetylated tannin.

}, url = {https://hal.univ-lorraine.fr/LERMAB-UL/hal-02508080}, author = {J.J. LIAO and N. BROSSE and A. PIZZI and S. HOPPE and X.J. ZHOU and G.B. DU} } @article {1859, title = { Effect of vacuum hot pressing on the bonding quality and heat transfer performance of plywood }, journal = { EUROPEAN JOURNAL OF WOOD AND WOOD PRODUCTS }, volume = {78}, year = {2020}, pages = {441-447}, abstract = {

Vacuum technology was applied to the hot-pressing technology of plywood production with phenolic resin (PF). For plywood with the same number of layers, veneers were hot-pressed with conventional and vacuum hot-pressing processes respectively at the same hot-pressing time. Varying layers (3, 9 and 15-layers) and spread quantities (220 g m(-2), 260 g m(-2), 300 g m(-2)) were applied. Heat transfer performance of the assembly, polymerization extent of PF, and bonding quality of plywood were examined by thermocouple and humidity sensors, Fourier transform infrared spectroscopy (FTIR), fluorescence microscope and bonding strength measurement. The results indicated that, compared to conventional hot pressing, the temperature of the central layer of the assembly vacuum hot-pressed was significantly increased by about 20-30 degrees C and the adhesive cured more quickly. The hot-pressing method had a significant influence on the bonding strength of plywood, with an enhancement of the bonding strength to wood failure ratio of 48.37\% and 33.55\%, respectively. The adhesive between adjacent laminates formed a continuously dense layer with more connection points, leading to excellent mechanical meshing and high bonding quality. In addition, vacuum hot pressing can eliminate the influence of adhesive position on bonding strength and make the mechanical properties of plywood tend to be uniform in thickness direction. Under the experimental conditions, the variable energy cost of 15-ply plywood with 1 m(3) produced by vacuum hot pressing was 3.83\% less than that of conventional hot pressing, and the plywood could still maintain good bonding strength at low spread quantity.

}, author = {L. HONG and Q. HE and Z.H. JU and H.Y. ZHANG and N. BROSSE and X.N. LU} } @article {1846, title = { Facile preparation of high anti-fungal performance wood by high voltage electrostatic field (HVEF) }, journal = { JOURNAL OF CLEANER PRODUCTION }, volume = {260}, year = {2020}, abstract = {

In this study, in order to improve the anti-fungal performance of wood material, a facile, efficient and eco-friendly method was proposed for wood modification under the synergistic effect of silver particles and high voltage electrostatic field (HVEF) treatment. Poplar wood, a vulnerable to decay species, was hot-pressed by silver electrode plates and exposed simultaneously to HVEF. The chemical characteristics and anti-fungal performance of treated wood were investigated in details. Under HVEF treatment, silver particles were triggered to different oxidized forms and bound with polar groups in the wood cell wall. Decreased O/C element ratio and -OH groups and increased C-H and C=O bonds in treated wood were observed by the X-ray photoelectron spectra (XPS) and fourier transform infrared (FTIR) spectroscopy. After 24h of HVEF treatment, high concentration (10.71\%) of well-distributed silver particles appeared in mapping graphs. Laboratory anti-fungal tests showed that mass losses of treated wood samples decreased significantly (\<1\%) after exposing to rot fungi. The highest leaching percentage of silver in treated samples was 3.94\%. These results indicated that the synergistic effect of silver particles and HVEF treatment enhanced the fungal-resistance performance of wood. Moreover, this approach could be regarded as a facile, efficient and eco-friendly modification to broaden the outdoor-use potential of wood.

}, url = {https://hal.univ-lorraine.fr/hal-02508085}, author = {Q. HE and T.Y. ZHAN and H.Y. ZHANG and Z.H. JU and L. HONG and N. BROSSE and X.N. LU} } @article {1875, title = { Hydrothermal conversion of wood, organosolv, and chlorite pulps }, journal = { BIOMASS CONVERSION AND BIOREFINERY }, volume = {10}, year = {2020}, pages = {1-13}, abstract = {

In this work, beech wood has been submitted to fractionation and hydrothermal liquefaction in order to produce fermentable carbohydrates. Fractionation either by ethanol organosolv or by sodium chlorite/acetic acid (SC/AA) treatment allowed obtaining delignification yields of 50 and 91 wt.\% respectively. The recovered pulps were then submitted to liquefaction in hot-compressed water (HCW). Three temperatures were studied: 180, 200, and 220 degrees C during 2 h. The same experiments were conducted on untreated beech and model cellulose (Avicel PH-101). Product yields and total carbohydrates were determined. The liquefaction products, i.e., solid residue, water-soluble compounds, and permanent gas, were analyzed respectively by X-ray diffraction (XRD), high-performance anion-exchange chromatography with pulsed amperometric detector (HPAEC-PAD), and gas chromatography (GC). SC/AA treatment allowed a high recovery of hemicelluloses and for this reason, xylose content was significantly higher than for the organosolv pulp. The maximum yields of total carbohydrates (based on the initial carbohydrates in wood), found when the liquefaction temperature was 220 degrees C, increased from 9.0 wt.\% for the raw beech to 13.5 and 33.7 wt.\% for the organosolv and SC/AA pulps respectively.

}, url = {https://hal.univ-lorraine.fr/hal-02125963}, author = {F. BUENDIA-KANDIA and N. BROSSE and D. PETITJEAN and G. MAUVIEL and E. RONDAGS and E. GUEDON and A. DUFOUR} } @article {1855, title = { Nanocellulose: From Fundamentals to Advanced Applications }, journal = { FRONTIERS IN CHEMISTRY }, volume = {8}, year = {2020}, pages = {392}, abstract = {

Over the past few years, nanocellulose (NC), cellulose in the form of nanostructures, has been proved to be one of the most prominent green materials of modern times. NC materials have gained growing interests owing to their attractive and excellent characteristics such as abundance, high aspect ratio, better mechanical properties, renewability, and biocompatibility. The abundant hydroxyl functional groups allow a wide range of functionalizations via chemical reactions, leading to developing various materials with tunable features. In this review, recent advances in the preparation, modification, and emerging application of nanocellulose, especially cellulose nanocrystals (CNCs), are described and discussed based on the analysis of the latest investigations (particularly for the reports of the past 3 years). We start with a concise background of cellulose, its structural organization as well as the nomenclature of cellulose nanomaterials for beginners in this field. Then, different experimental procedures for the production of nanocelluloses, their properties, and functionalization approaches were elaborated. Furthermore, a number of recent and emerging uses of nanocellulose in nanocomposites, Pickering emulsifiers, wood adhesives, wastewater treatment, as well as in new evolving biomedical applications are presented. Finally, the challenges and opportunities of NC-based emerging materials are discussed.

}, url = {https://hal.univ-lorraine.fr/LERMAB-UL/hal-02649346}, author = {D. TRACHE and A.F. TARCHOUN and M. DERRADJI and T.S. HAMIDON and N. MASRUCHIN and N. BROSSE and M.H. HUSSIN} } @article {1850, title = { One-step compatibilization of poly(lactic acid) and tannin via reactive extrusion }, journal = { MATERIALS \& DESIGN }, volume = {191}, year = {2020}, abstract = {

The compatibility issue between poly(lactic acid) (PLA) and tannin is a big challenge for preparing PLA/tannin biocomposites with enhanced properties. In this work, composites with enhanced properties have been accomplished using an efficient one-step reactive extrusion method with the help of methylene diphenyl diisocyanate (p-MDI) or 3-aminopropytriethoxysilane (APS). The extent of compatibility achieved via the one-step was evaluated by tensile, morphological, rheological, and thermal properties. The obtained results indicated that the adhesion promoters, especially p-MDI, contributed efficiently to an improved tensile behavior of the resulting composites with a tough tensile-fracture surface compared with incompatibilized PLA/tannin composite. Moreover, these composites displayed a plateau-like rheological behavior, enhanced complex viscosity, higher melting and thermal degradation temperature. This approach can be potentially adapted to other PLA/biopolymers composite systems.

}, url = {https://hal.inria.fr/hal-02495239/}, author = {J.J. LIAO and N. BROSSE and S. HOPPE and G. DU and X.J. ZHOU and A. PIZZI} } @article {1877, title = { Steam Explosion of Beech Wood: Effect of the Particle Size on the Xylans Recovery }, journal = { WASTE AND BIOMASS VALORIZATION }, volume = {11}, year = {2020}, pages = {625-633}, abstract = {

In this work, the effect of particle size and severity factors was investigated to find the optimum condition of steam explosion pretreatment on xylan recovery of beech wood. The beech wood particles with sizes of 0.16, 1, or 2 mm were steamed at 150-210 degrees C for 2.5-15 min before an explosive decompression. The results showed that the maximum xylan recovery was about 10\% w/w wood with low concentrations of the inhibitors, which were obtained when the particle size is 1 mm and R-0=3.65 (190 degrees C, 10 min). The smallest particle size may result in overcooking of biomass, leads to easily and high degradation of hemicelluloses sugars, whereas the largest particle sizes may result in incomplete autohydrolysis in biomass and lower extractability of hemicelluloses sugars. The obtained optimum condition for xylan recovery will improve the subsequent utilization (such as in food industry and other chemical products), prior to subsequent transformation of steam explosion pretreated wood (bioethanol and pellet).

}, url = {https://hal.univ-lorraine.fr/LERMAB-UL/hal-02125966}, author = {E. SIMANGUNSONG and I. ZIEGLER-DEVIN and L. CHRUSCIEL and P. GIRODS and N.J. WISTARA and N. BROSSE} } @article {1844, title = { Toward the cottonization of hemp fibers by steam explosion. Flame-retardant fibers }, journal = { INDUSTRIAL CROPS AND PRODUCTS }, volume = {151}, year = {2020}, abstract = {

The goal is to produce cottonized hemp fibers with improved thermal stability. It was first found that the fine hemp fibers produced from technical non-retted hemp fibers by steam explosion exhibited an enhanced thermal stability. An efficient and low-cost process was developed using a mixture of urea/etidronic acid in aqueous solution in order to achieve a high phosphorus content and produce flame retardant fibers by chemical grafting. ICP, P-31 and C-13 NMR, SEM, thermogravimetric, Pyrolysis-Combustion Flow Calorimetry analyses and a flame test were used to characterize the grafted fibers. Fibers modified with relatively high P and N contents have been produced (approximate to 6 wt \% and approximate to 4 wt \% respectively) but lower grafting rates (P approximate to 0.5 \% and N approximate to 0.35 \%) are sufficient to produce non-flammable fibers. A synergistic effect between N and P has been proposed to induce the formation of a stable char.

}, url = {https://hal.univ-lorraine.fr/LERMAB-UL/hal-02676818}, author = {M. MOUSSA and R. EL-HAGE and R. SONNIER and L. CHRUSCIEL and I. ZIEGLER-DEVIN and N. BROSSE} } @article {1842, title = { Dynamically Cross-Linked Tannin as a Reinforcement of Polypropylene and UV Protection Properties }, journal = {POLYMERS}, volume = {11}, year = {2019}, abstract = {

Tannins were used as reinforcing components for polypropylene with anti-UV properties via dynamic curing extrusion. The influence of cross-linked tannins in different weight fraction and their anti-UV capacity on morphological, mechanical, rheological, crystallize and thermal properties were studied. The experimental results indicated that the cross-linked tannins improve Young\&$\#$39;s modulus, crystallinity, and thermal stability and reinforce the internal network of polypropylene. After UV accelerated weathering, polypropylene had fewer surface cracks, lower carbonyl index, fewer crystallinity decreases and less mechanical properties loss with increasing tannin content.

}, url = {https://hal.archives-ouvertes.fr/hal-01977584}, author = {J.J. LIAO and N. BROSSE and A. PIZZI and S. HOPPE} } @article {1791, title = { High voltage electric discharges treatment for high molecular weight hemicelluloses extraction from spruce }, journal = { CARBOHYDRATE POLYMERS }, volume = {222}, year = {2019}, abstract = {

The aim of this work is to extract hemicelluloses polymers from spruce sawdust using High Voltage Electrical Discharges (HVED) pretreatment. HVED pretreatment was carried out in order to improve deconstruction of the wood matrix and to allow easier release of high molecular mass hemicelluloses. The results revealed the advantage of HVED activation step in the process of extraction. The yield of hemicellulose extraction increased with HVED treatment time. In fact, after 4 ms of HVED treatment time in 1M NaOH solution, the yield obtained was higher as compared to the untreated sample (19 mg/g of dry matter and 15.8 mg/g of dry matter respectively). The molecular weights of extracted hemicelluloses are very high (55 kDa and 47 kDa for 4 ms of HVED-treatment in 1M NaOH solution and water respectively). The use of different mediums of extraction with HVED pretreatment have revealed a selective solubilization of spruce hemicelluloses.

}, url = {https://hal.univ-lorraine.fr/LERMAB-UL/hal-02290577}, author = {M. CHADNI and N. GRIMI and I. ZIEGLER-DEVIN and N. BROSSE and O. BALS} } @article {1843, title = { Influence of high voltage electrostatic field (HVEF) on bonding characteristics of Masson (Pinus massoniana Lamb.) veneer composites }, journal = { EUROPEAN JOURNAL OF WOOD AND WOOD PRODUCTS }, volume = {77}, year = {2019}, pages = {105-114}, abstract = {

For the first time, it was experimented with high voltage electrostatic field (HVEF) for the optimization of the bonding process of urea formaldehyde (UF) resin to wood. Varying HVEF treatment times (0-8min) and intensities (5-20kV) were applied. Wood surface characteristics, polymerization extent of UF, and bonding interphase of UF to wood were examined by electron spin resonance (ESR) spectroscopy, dynamic contact angle goniometers, Fourier transform infrared spectroscopy (FTIR), X-ray densitometer, fluorescence microscope and bonding strength measurement. The results indicated that HVEF treatments applied to wood veneer induced a decrease in contact angles and an increase in the free radicals of wood, and surface energy varied with treatment times and intensities. These varieties were because triggered free electrons, broken chemical bonds and new ions appeared on the wood surface with HVEF treatment. An aggregated performance was obviously obtained in micrographs and vertical density profiles (VPDs). It was explained that resin penetration into wood structure was significantly shallow, and resin concentration and density at bonding interphase were more enhanced than the control. This is due to the increment of surface energy and lower contact angles providing more chances for possible reactions of wood surface with the UF resin. Resin penetration depth and density varied with different treatment times and intensities. Increased cross-linking extent of UF was obtained under varied conditions of HVEF treatment. The bonding strength was measured as a function of treatment times and intensities respectively; it increased by 85\% and the wood failure ratio significantly increased by 70\% under HVEF treatment (20kV, 8min) due to the aggregation performance and more cross-linked UF resin. It was manifested that both treatment time and intensity play a significant role in HVEF treatment, and HVEF treatment has a significant influence on the characteristics of the wood surface and the bonding properties of wood composites.

}, url = {https://hal.univ-lorraine.fr/hal-02289753}, author = {Q. HE and T.Y. ZHAN and Z.H. JU and H.Y. ZHANG and L. HONG and N. BROSSE and X.N. LU} } @article {1841, title = { Lignin-Based Carbon Nanofibers as Electrodes for Vanadium Redox Couple Electrochemistry }, journal = {NANOMATERIALS}, volume = {9}, year = {2019}, abstract = {

Three different types of lignin (kraft, organosolv and phosphoric acid lignin) were characterized and tested as precursors of electrospun nanofibers. Polyethylene oxide (PEO) was added as a plasticizer and dimethyl formamide (DMF) employed as a solvent. It was found that the molecular weight of lignin was the key parameter to understand the differences of the mechanical stability of the resultant fiber mats. In the case of kraft lignin (KL), the influence of some changes in the synthetic process was also tested: applied voltage, pretreatment in air or not, and the addition of a small amount of Ketjen black. After pyrolysis in nitrogen flow, the obtained carbon nanofibers (CNFs) were characterized by different techniques to analyze their differences in morphology and surface chemistry. Vanadium electrochemistry in 3M sulfuric acid was used to evaluate the different CNFs. All fibers allowed electrochemical reactions, but we observed that the oxidation of V(II) to V(III) was very sensitive to the nature of the raw material. Materials prepared from kraft and phosphorus lignin showed the best performances. Nevertheless, when 1 wt.\% of Ketjen black was added to KL during the electrospinning, the electrochemical performance of the sample was significantly improved and all targeted reactions for an all-vanadium redox flow battery were observed. Therefore, in this work, we demonstrated that CNFs obtained by the electrospinning of lignin can be employed as electrodes for vanadium electrochemistry, and their properties can be tuned to improve their electrochemical properties.

}, url = {https://hal.univ-lorraine.fr/hal-02125947}, author = {J.F. VIVO-VILCHES and A. CELZARD and V. FIERRO and I. ZIEGLER-DEVIN and N. BROSSE and A. DUFOUR and M. ETIENNE} } @inbook {1835, title = { Organosolv Processes }, booktitle = {BIOREFINERIES}, volume = {166}, number = {Advances in Biochemical Engineering-Biotechnology}, year = {2019}, pages = {153-176}, abstract = {

Biofuels and chemicals can be produced from lignocellulosic feedstocks using biotechnological processes. The effective utilization of carbohydrates from biomass for the production of biofuels necessitates the development of pretreatment technologies to enhance their enzymatic digestibility. Among all the various pretreatment methods currently studied and developed, the organosolv processes, in which organic solvents or aqueous organic solvent mixtures are used as the pretreatment medium, appear to be specially promising in the context of the biorefinery because (1) they produce cellulosic pulp with a good enzymatic digestibility for monomeric glucose production and (2) they allow a clean fractionation of the major biomass components (cellulose, lignin, and hemicelluloses) into three process streams. In this chapter we give an updated overview of organosolv methods using conventional solvents and ionic liquids which have recently gained considerable interest as solvents for lignocellulosic biomass and pretreatment.

}, author = {N. BROSSE and M.H. HUSSIN and A.A. RAHIM} } @article {1805, title = { Polypropylene Blend with Polyphenols through Dynamic Vulcanization: Mechanical, Rheological, Crystalline, Thermal, and UV Protective Property }, journal = {POLYMERS}, volume = {11}, year = {2019}, abstract = {

Tannin and lignin were blended with polypropylene (PP) through dynamic vulcanization technique. Their influence of mechanical property, crystallinity, thermal stability, as well as ultraviolet (UV) protection property on the PP matrix was investigated and compared with native tannin and lignin. According to our experimental results, tannin and lignin undergo dynamic vulcanization and were more compatible with the PP matrix. Besides, tannin and vulcanized tannin can perform as nucleating agents of PP because of their relatively small particle size. Moreover, vulcanized tannin/lignin have a better performance on the thermal stability of PP compared with native tannin/lignin, especially PP/vulcanized lignin blend. Furthermore, vulcanized tannin/lignin present better UV protective performance, concluded from fewer changes on surface morphology, carbonyl index, crystallinity, viscosity, and tensile property.

}, url = {https://hal.univ-lorraine.fr/LERMAB-UL/hal-02196798}, author = {J.J. LIAO and N. BROSSE and A. PIZZI and S. HOPPE and X.D. XI and X.J. ZHOU} } @article {1778, title = { Reinforced lignin-phenol-glyoxal (LPG) wood adhesives from coconut husk }, journal = { INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES }, volume = {141}, year = {2019}, pages = {185-196}, abstract = {

Lignin was extracted from coconut husk via alkaline pulping, either Kraft or soda. The isolated lignin samples were classified as hydroxy-benzaldehyde, vanillin, and syringaldehyde type according to Fourier-transform Infrared Spectroscopy, H-1 and C-13 Nuclear Magnetic Resonance (NMR) spectra. Soda lignin (SL) showed higher thermal stability and glass transition temperature (T-g) than Kraft lignin (KL) as proven by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC), respectively. The soda-lignin-phenol-glyoxal (SLPG) resins with the optimum percentage of lignin substitution at 30\% showed improved solid content and gel time in comparison to 30\% of Kraft-lignin-phenol-glyoxal (KLPG) and phenol-glyoxal (PG) resin. The good mechanical properties in SLPG is due to the higher amount of molecular weight as well as higher phenolic and G-type unit in lignin that improve the properties of 30\% SLPG adhesive. Moreover, the addition of layered double hydroxides (LDH) as reinforced filler up to 15\%-30\% SLPG adhesive blend shows a great performance (especially mechanical properties) as compared to 30\% SLPG adhesive alone.

}, url = {https://hal.univ-lorraine.fr/hal-02289744}, author = {N.A. AZIZ and A.F.A. LATIP and L.C. PENG and N.H. ABD-LATIF and N. BROSSE and R. HASHIM and M.H. HUSSIN} } @article {1795, title = { Robust and durable bonding performance of bamboo induced by high voltage electrostatic field treatment }, journal = { INDUSTRIAL CROPS AND PRODUCTS }, volume = {137}, year = {2019}, pages = {149-156}, abstract = {

To enhance the bonding performance of bamboo, the high voltage electrostatic field (HVEF) treatment was used for flattened moso bamboo (Phyllostachys pubescens). Three bonding types including bamboo skin-bamboo skin (BS-BS), bamboo skin-bamboo pith (BS-BP) and bamboo pith-bamboo pith (BP-BP) were tested. Surface characteristics of HVEF-treated bamboo composites were analyzed by the electron spin resonance (ESR), X-ray photoelectron spectra (XPS), Fourier transform infrared spectroscopy (FTIR), fluorescence microscopy and vertical density profile (VDP). Mechanical properties, including bonding strength, modulus of rupture (MOR), modulus of elasticity (MOE) and boiling peeling rate of treated-bamboo composites were tested as well. The results of ESR, XPS and FTIR showed that significantly increased free radicals, broken chemical bonds and oxygen-containing groups (-OH, C=O and C-O) were obtained. These variations were attributed to the fact that triggered electrons were able to break oxygen and water molecules in the atmosphere under HVEF treatment and more broken chemical bonds (oxygen atoms and ions) appeared and reacted with bamboo surface. Higher change ratios involved in BS compared with BP were due to higher components of cellulose and lignin. HVEF treatment induced a significant decrease on adhesive penetration depth and an increment on density at bonding interphase. The highest decrease of adhesive penetration depth and increment of density at bamboo interphase were obtained in BS-BS while the least was BP-BP. All the bonding performance significantly enhanced after HVEF-treatment. The most robust and durable bonding performances were obtained in BS-BS type, and BP-BP showed the most increment extents of bamboo failure ratio. Results of this study revealed that: HVEF treatment was an effective approach for enhancing bonding properties of both bamboo skin and pith.

}, url = {https://hal.univ-lorraine.fr/hal-02289743}, author = {Q. HE and T.Y. ZHAN and H.Y. ZHANG and Z.H. JU and L. HONG and N. BROSSE and X.N. LU} } @article {1811, title = { The structural characterization and antioxidant properties of oil palm fronds lignin incorporated with p-hydroxyacetophenone }, journal = { INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES }, volume = {130}, year = {2019}, pages = {947-957}, abstract = {

This study reports on the effects of unmodified autohydrolyzed ethanol organosolv lignin (AH EOL) and modified autohydrolyzed ethanol organosolv lignin on the structural characteristics and antioxidant properties upon incorporation of p-hydroxyacetophenone (AHP EOL). The lignin samples isolated from black liquor of oil palm fronds (OPF) were evaluated and compared using various complementary analyses; FTIR, H-1 and C-13 NMR spectroscopy, 2D-NMR spectroscopy (FIMBC and HSQC), CHN, GPC, HPLC and thermal analyses (TGA and DSC). Chemically modified organosolv lignin (AHP EOL) provided lignin with lower molecular weight (M-W), which has smaller fragments that leads to higher solubility rate in water in comparison to unmodified organosolv lignin, AH EOL (D-AHP EOL: 19.8\% \> D-AH EOL: 14.0\%). It was evident that the antioxidant properties of modified organosolv lignin has better reducing power in comparison to the unmodified organosolv lignin. Therefore, the functionalization of lignin polymers enhanced their antioxidant properties and structural features towards a various alternative approach in lignin-based applications.

}, url = {https://hal.univ-lorraine.fr/hal-02296950}, author = {N.H. ABD-LATIF and A.A. RAHIM and N. BROSSE and M.H. HUSSIN} } @article {1734, title = { Acetyl Groups in Typha capensis: Fate of Acetates during Organosolv and Ionosolv Pulping }, journal = {POLYMERS}, volume = {10}, year = {2018}, abstract = {

During biomass fractionation, any native acetylation of lignin and heteropolysaccharide may affect the process and the resulting lignin structure. In this study, Typha capensis (TC) and its lignin isolated by milling (MWL), ionosolv (ILL) and organosolv (EOL) methods were investigated for acetyl group content using FT-Raman, H-1 NMR, 2D-NMR, back-titration, and Zemplen transesterification analytical methods. The study revealed that TC is a highly acetylated grass; extractive free TC (TCextr) and TC MWL exhibited similar values of acetyl content: 6 wt \% and 8 wt \% by Zemplen transesterification, respectively, and 11 wt \% by back-titration. In contrast, lignin extracted from organosolv and [EMIm][OAc] pulping lost 80\% of the original acetyl groups. With a high acetyl content in the natural state, TC could be an interesting raw material in biorefinery in which acetic acid could become an important by-product.

}, url = {https://hal.univ-lorraine.fr/LERMAB-UL/hal-02297011}, author = {I.G. AUDU and N. BROSSE and H. WINTER and A. HOFFMANN and M. BREMER and S. FISCHER and M.P. LABORIE} } @article {1724, title = { Biochemical characterization of the skeletal matrix of the massive coral, Porites australiensis - The saccharide moieties and their localization }, journal = { JOURNAL OF STRUCTURAL BIOLOGY }, volume = {203}, year = {2018}, pages = {219-229}, abstract = {

To construct calcium carbonate skeletons of sophisticated architecture, scleractinian corals secrete an extra cellular skeletal organic matrix (SOM) from aboral ectodermal cells. The SOM, which is composed of proteins, saccharides, and lipids, performs functions critical for skeleton formation. Even though polysaccharides constitute the major component of the SOM, its contribution to coral skeleton formation is poorly understood. To this end, we analyzed the SOM of the massive colonial coral, Porites australiensis, the skeleton of which has drawn great research interest because it records environmental conditions throughout the life of the colony. The coral skeleton was extensively cleaned, decalcified with acetic acid, and organic fractions were separated based on solubility. These fractions were analyzed using various techniques, including SDS-PAGE, FT-IR, in vitro crystallization, CHNS analysis, chromatography analysis of monosaccharide and enzyme-linked lectin assay (ELLA). We confirmed the acidic nature of SOM and the presence of sulphate, which is thought to initiate CaCO3 crystallization. In order to analyze glycan structures, we performed ELLA on the soluble SOM for the first time and found that it exhibits strong specificity to Datura stramonium lectin (DSL). Furthermore, using biotinylated DSL with anti-biotin antibody conjugated to nanogold, in situ localization of DSL-binding polysaccharides in the P. australiensis skeleton was performed. Signals were distributed on the surfaces of fiber-like crystals of the skeleton, suggesting that polysaccharides may modulate crystal shape. Our study emphasizes the importance of sugar moieties in biomineralization of scleractinian corals.

}, url = {https://hal.archives-ouvertes.fr/hal-02122753/}, author = {T. TAKEUCHI and L. PLASSERAUD and I. ZIEGLER-DEVIN and N. BROSSE and C. SHINZATO and N. SATOH and F. MARIN} } @article {1716, title = { Potential of a short rotation coppice poplar as a feedstock for platform chemicals and lignin-based building blocks }, journal = { INDUSTRIAL CROPS AND PRODUCTS }, volume = {123}, year = {2018}, pages = {698-706}, abstract = {

In the context of a biorefinery, the potential of the short rotation coppice \"poplar with bark\" as a feedstock for the acid-catalyzed ethanol-water Organosolv process and furthermore for possible applications of the biomass components was investigated aiming at optimal separation of the non-standardized woody biomass. The study was supported and evaluated by an experimental design (Box-Behnken). The statistical analysis showed an increase in lignin yield with rising process intensity with an optimum for precipitated lignin yield of 42\%. A change in downstream processing from lignin precipitation by simple dilution of the reaction water to stripping of the ethanol provided a 10\% higher lignin yield. Molecular weight distribution of the lignin samples as well as the number of aliphatic OH-groups within the lignin molecules decreased with intensified conditions whereas the phenolic group content increased. The cellulose content in the fibre fraction is hardly influenced by the pulping conditions, lignin and hemicellulose removal lead to a raising cellulose recovery.

}, author = {V. ROHDE and T. HAHN and M. WAGNER and S. BORINGER and B. TUBKE and N. BROSSE and N. DAHMEN and D. SCHMIEDL} } @article {1732, title = { Production of oil palm (Elaeis guineensis) fronds lignin-derived non-toxic aldehyde for eco-friendly wood adhesive }, journal = { INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES }, volume = {113}, year = {2018}, pages = {1266-1272}, abstract = {

Lignocellulosic materials can significantly contribute to the development of eco-friendly wood adhesives. In this work, glyoxal-phenolic resins for plywood were prepared using organosolv lignin, which was isolated from black liquor recovered from organosolv pulping of oil palm fronds (OPF) and considered to be an alternative to phenol. Glyoxal, which is a dialdehyde obtained from several natural resources, was used as substitute for formaldehyde. The structure of organosolv lignin and the resins were characterized by FTIR and NMR, and for thermal stability by TGA and DSC. The resins were further studied for their viscosity, pH, solids content and gel times. The resins performance as wood adhesive was further established from mechanical test in terms of tensile strength and modulus of elasticity (MOE) to obtain the optimum ratios of organosolv lignin, which replaces phenol in organosolv lignin phenol glyoxal (OLPG) resins. The adhesive composition having 50\% (w/w) of phenol substituted by organosolv lignin, termed as 50\% OLPG showed highest adhesive strength compared to phenol formaldehyde (PF) commercial adhesive.

}, author = {M.H. HUSSIN and N.A. SAMAD and N.H. ABD-LATIF and N.A. ROZULI and S.B. YUSOFF and F. GAMBIER and N. BROSSE} } @article {1739, title = { Toward the cottonization of hemp fibers by steam explosion - Part 1: defibration and morphological characterization }, journal = { TEXTILE RESEARCH JOURNAL }, volume = {88}, year = {2018}, pages = {1047-1055}, abstract = {

Fine hemp fibers (cottonized hemp) were processed using steam explosion. The quantification of the defibration rate was performed by image processing. Based on this method, the hemp defibration was optimized using a response surface methodology based on three-variable central composite design for the production of elementary fibers with low variability. Optimal parameters for the steam processes were as follows: time=4.1min; temperature=191?. Biomass was impregnated with a solution of NaOH (8\%) before treatment, leading to a defibration rate of 91.2\%, which is producing approximate to 50\% fibers with length \<3mm, in good agreement with the experimental data. Damaged fibers originating from the conjugated effect of steam explosion and alkali hydrolysis were also observed.

}, url = {https://hal.univ-lorraine.fr/hal-02289748}, author = {T. SAUVAGEON and J.M. LAVOIE and C. SEGOVIA and N. BROSSE} } @article {1660, title = { Modification of oil palm fronds lignin by incorporation of m-cresol for improving structural and antioxidant properties }, journal = { INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES }, volume = {104}, year = {2017}, pages = {251-260}, abstract = {

Lignin extracted from oil palm fronds (OPF) underwent chemical modification by incorporating m-cresol into the lignin matrix. This study reports on the physicochemical properties and antioxidant activity of unmodified autohydrolyzed ethanol organosolvlignin (AH EOL) and the modified autohydrolyzed ethanol organosolv lignin (AHC EOL). The lignin samples were analyzed by FFIR, H-1 and C-13 NMR spectroscopy, 2D NMR: HSQC spectroscopy, CHN analysis, molecular weight distribution analysis; GPC and thermal analysis; DSC and TGA. The lignin modification has reduced the hydrophobicity of its complex structure by providing better quality lignin with smaller fragments and higher solubility rate in water (D-AHCEOL.: 42\%\> D-AHEOL: 25\%). It was revealed that the modification of lignin has improved their structural and antioxidant properties, thus venture their possible applications.

}, url = {https://hal.univ-lorraine.fr/hal-01765057}, author = {N.A. SA{\textquoteright}DON and A.A. RAHIM and M.N.M. IBRAHIM and N. BROSSE and M.H. HUSSIN} } @article {1673, title = { A Multitechnique Characterization of Lignin Softening and Pyrolysis }, journal = { ACS SUSTAINABLE CHEMISTRY \& ENGINEERING }, volume = {5}, year = {2017}, pages = {6940-6949}, abstract = {

The understanding of lignin softening and pyrolysis is important for developing lignocellulosic biorefinery in order to produce carbon fibers, polymers additives, green aromatics, or biofuels. Protobind lignin (produced by soda pulping of a wheat straw) was characterized by thermogravimetry, calorimetry (for glass transition temperature and heat of pyrolysis reactions), in situ H-1 NMR (for the analysis of the mobility of protons upon lignin thermal conversion), and solution-state C-13 and P-31 NMR (determination of functional groups in lignin). In situ rheology reveals the real-time viscoelastic behavior of lignin as a function of temperature. Upon heating, lignin undergoes softening, through glass transition overlapped with depolymerization, and is followed by the solidification of the softened material by cross-linking reactions. The lignin residues were quenched within the rheometer at the midpoint temperatures of softening and solidification regions and were further analyzed by elemental analysis, GPC-UV of acetylated THE soluble fractions, FTIR, solid C-13 NMR, and laser desorption ionization (LDI) combined with very high-resolution mass spectrometry (HRMS). We present the first report on lignin biochars analysis by LDI-HRMS. NMR and FTIR analyses provide the evolution of functional moieties in lignin residues. C-13 NMR, GPC-UV, and LDI FTICRMS analyses depict the depolymerization mechanism combined with cross-linking and demethoxylation reactions. An overall physical and chemical mechanism for the thermal conversion of alkali lignin is proposed based on these complementary analyses.

}, url = {https://hal.univ-lorraine.fr/hal-01575541}, author = {B. SHRESTHA and Y. LE-BRECH and T. GHISLAIN and S. LECLERC and V. CARRE and F. AUBRIET and S. HOPPE and P. MARCHAL and S. PONTVIANNE and N. BROSSE and A. DUFOUR} } @article {1659, title = { Pretreatment of trace element-enriched biomasses grown on phytomanaged soils for bioethanol production }, journal = { INDUSTRIAL CROPS AND PRODUCTS }, volume = {107}, year = {2017}, pages = {63-72}, abstract = {

Phytotechnologies are a set of sustainable, ecological options notably for alleviating pollutant linkages induced by contaminated soils. However, concerns exist regarding the processing of trace elements (TE)-enriched biomass and the fate of TEs in the end-products. The fractionation of phytoremediation TE-enriched non-woody lignocellulosic (tobacco) and woody (birch, willow) phytoremediation-borne biomasses was studied using ethanol organosolv, soda and dilute acid pretreatments. TE distribution in the process fractions (pulp, liquid effluents and lignin) was further examined. In dilute acid conditions, a wood pretreatment performed at 170 degrees C in the presence of 2\% w/w of sulfuric acid allowed an efficient extraction of the metals in the water effluent (approximate to 90\% for Mn and Zn) producing a clean pulp. A soda pretreatment resulted in a low metal extractability, especially at high temperature. At 170 degrees C or above with 15\% w/w of NaOH, metals were mostly recovered in the cellulosic pulp (70\%- 98\%). Using organosolv pulping, the TE contents were in the decreasing order: pulp \>\> water stream \> lignin. The TE organosolv extraction in the liquid phase varied depending on the TE metal and on the species but was generally low. Metal extractability increased with the water content in the solvent of the organosolv pulping but decreased with temperature. Enzymatic hydrolyses of TE-enriched and metal-free pulps were investigated and it was concluded that the TE concentrations had little or no effect on polysaccharide enzymatic hydrolysability by cellulases. The final destination of the various fractions for valorization in a biorefinery setting is discussed, regarding their TE content.

}, url = {https://hal.archives-ouvertes.fr/hal-01538463}, author = {M. ASAD and Z. MENANA and I. ZIEGLER-DEVIN and V. BERT and M. CHALOT and R. HERZIG and M. MENCH and N. BROSSE} } @article {1657, title = { The capability of ultrafiltrated alkaline and organosolv oil palm (Elaeis guineensis) fronds lignin as green corrosion inhibitor for mild steel in 0.5 M HCl solution }, journal = { MEASUREMENT }, volume = {78}, year = {2016}, pages = {90-103}, abstract = {

The inhibitive effect of ultrafiltrated oil palm fronds (OPF) lignins on the corrosion of mild steel in 0.5 M HCl solution has been investigated by electrochemical impedance spectroscopy (EIS), potentiodynamic polarization (PP) and weight loss measurement. The presence of smaller lignin fractions reduces remarkably the corrosion rate of mild steel. The highest corrosion inhibition efficiency for all ultrafiltrated lignins were attained at maximum concentration of 500 ppm (IEP.Soda: 87\% \> IEP.Organosolv: 83\% \> IEP.Kraft: 81\%). The results from this corrosion test clearly reveal that all ultrafiltrated lignins behaved as a mixed-type inhibitor with predominant anodic (organosolv lignin) or cathodic (alkaline lignin) effectiveness. It was deduced that the inhibition process was spontaneous and the inhibitors were mainly physically adsorbed onto the mild steel surface.

}, author = {M.H. HUSSIN and A.A. RAHIM and M.N.M. IBRAHIM and N. BROSSE} } @article {1600, title = { Characterization of biomass char formation investigated by advanced solid state NMR }, journal = { CARBON }, volume = {108}, year = {2016}, pages = {165-177}, abstract = {

Char is produced during pyrolysis of biomass and it could be valorised as soil amendment, activated carbon or to produce syngas or heat by further oxidation. The mechanisms of biochars formation have to be better understood in order to tailor their properties. For this purpose, the pyrolysis of biomass was conducted in a fixed bed reactor allowing a good control of pyrolysis conditions. Miscanthus and the macromolecules extracted from this same biomass (holocellulose, cellulose, ethanol organosolv lignin) were pyrolysed to various final temperatures (200-500 degrees C). The chemical moieties formed in the chars were studied by solid state C-13 NMR. A Cross Polarization method at the Magic Angle Spinning with Adiabatic Passage though Hartmann-Hahn conditions (CP/MAS APHH) has been found to give similar spectra than the Direct Polarization quantitative method in much shorter acquisition times. A quantitative study on the formation of aromatic structures in the network of the macromolecules in miscanthus and in the fractionated macromolecules was conducted. It is shown that below 300 degrees C xylan is the main source of aromatic formation while above this temperature the aromatization of cellulose occurs. The interactions between lignin and carbohydrates inside the network of biomass for aromatic structures formation are discussed.

}, url = {https://hal.univ-lorraine.fr/hal-01599591}, author = {Y. LE-BRECH and J. RAYA and L. DELMOTTE and N. BROSSE and R. GADIOU and A. DUFOUR} } @article {1639, title = { Effect of Potassium on the Mechanisms of Biomass Pyrolysis Studied using Complementary Analytical Techniques }, journal = { CHEMSUSCHEM }, volume = {9}, year = {2016}, pages = {863-872}, abstract = {

Complementary analytical methods have been used to study the effect of potassium on the pyrolysis mechanisms of cellulose and lignocellulosic biomasses. Thermogravimetry, calorimetry, high-temperature H-1 NMR spectroscopy (in situ and real-time analysis of the fluid phase formed during pyrolysis), and water extraction of quenched char followed by size-exclusion chromatography coupled with mass spectrometry have been combined. Potassium impregnated in cellulose suppresses the formation of anhydrosugars, reduces the formation of mobile protons, and gives rise to a mainly exothermic signal. The evolution of mobile protons formed from K-impregnated cellulose has a very similar pattern to the evolution of the mass loss rate. This methodology has been also applied to analyze miscanthus, demineralized miscanthus, miscanthus re-impregnated with potassium after demineralization, raw oak, and Douglas fir. Hydrogen mobility and transfer are of high importance in the mechanisms of biomass pyrolysis.

}, url = {https://hal.univ-lorraine.fr/hal-01416493}, author = {Y. LE-BRECH and T. GHISLAIN and S. LECLERC and M. BOUROUKBA and L. DELMOTTE and N. BROSSE and C. SNAPE and P. CHAIMBAULT and A. DUFOUR} } @article {1616, title = { Extraction and Characterization of Fibers from Palm Tree }, journal = { BIORESOURCES }, volume = {11}, year = {2016}, pages = {7016-7025}, abstract = {

The characterization of fibers extracted from leaflet, the empty fruit bunches, leaf sheath, and spath of palm tree was performed. The fibers were extracted using three different procedures through chemical and / or enzymatic methods. The raw fibers studied have xylose contents between 13-22\% and glucose content between 30\% and 45\%. The microfibrillar angle (MFA) values are in the order: bunch \> spath \> leaf sheath \>\> leaflet. Spath and leaf sheath, which naturally occur in a woven form present poor mechanical strength but could be readily used to produce cheap composites. Leaflet fibers extracted from date palm tree exhibiting a low MFA (16 degrees), a high cellulose content, and cellulose crystallinity present the highest ultimate tensile strengths (approximate to 1250 N.mm(-2)).

}, url = {https://hal.inria.fr/hal-01492068}, author = {I. TAHRI and I.Z. DEVIN and J. RUELLE and C. SEGOVIA and N. BROSSE} } @article {1652, title = { Mechanisms of biomass pyrolysis studied reactor with advanced gas analysis by combining a fixed bed }, journal = { JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS }, volume = {117}, year = {2016}, pages = {334-346}, abstract = {

Slow pyrolysis of different biomasses (miscanthus, douglas fir and oak) was conducted in a U-shape fixed bed reactor combined to (1) on-line analysis of the vapors (primary tar) by soft photoionisation mass spectrometry (single photoionisation time-of-flight mass spectrometer, SPI-TOFMS), (2) quantitative off-line analysis of condensed vapors by GC*GC/MS-FID and (3) permanent gas analysis. The U-shape fixed bed reactor allows controlling external mass transfers, temperature of the bed, quenching char at targeted temperatures and quantifying mass balances. The mass yields in solid, condensable products and gas are studied between 200 degrees C and 500 degrees C. The soft on-line photoionisation analysis leads to a more interpretable mass spectra with few fragment ions and gives the evolution of the main markers of volatiles produced in real-time as a function of the temperature. The chemical structure of the markers analyzed on-line by SPI-TOFMS is assigned by GC*GC/FID-MS analysis. The mechanisms of hemicelluloses, cellulose and lignin pyrolysis in the complex network of biomass (including minerals catalytic effect) are discussed.

}, url = {https://hal.univ-lorraine.fr/hal-01923764}, author = {Y. LE-BRECH and L.Y. JIA and S. CISSE and G. MAUVIEL and N. BROSSE and A. DUFOUR} } @article {1598, title = { Physicochemical of microcrystalline cellulose from oil palm fronds as potential methylene blue adsorbents }, journal = { INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES }, volume = {92}, year = {2016}, pages = {11-19}, abstract = {

The present study sheds light on the physical and chemical characteristics of microcrystalline cellulose (MCC) isolated from oil palm fronds (OPF) pulps. It was found that the OPF MCC was identified as cellulose II polymorph, with higher crystallinity index than OPF alpha-cellulose (CrIOPFMCC: 71\%\> CrIOPF alpha-cellulose 47\%). This indicates that the acid hydrolysis allows the production of cellulose that is highly crystalline. BET surface area of OPF MCC was found to be higher than OPF alpha-cellulose (S-BETOPFMCC: 5.64 m(2) g(-1) \> SBETOPF alpha-cellulose :Q(a)(0) 2.04 m(2) g(-1)), which corroborates their potential as an adsorbent. In batch adsorption studies, it was observed that the experimental data fit well with Langmuir adsorption isotherm in comparison to Freundlich isotherm. The monolayer adsorption capacity (Q(a)(0)) of OPF MCC was found to be around 51.811 mg g(-1) and the experimental data fitted well to pseudo-second-order kinetic model.

}, author = {M.H. HUSSIN and N.A. POHAN and Z.N. GARBA and M.J. KASSIM and A.A. RAHIM and N. BROSSE and M. YEMLOUL and M.R.N. FAZITA and M.K.M. HAAFIZ} } @article {1249, title = {Antioxidant and anti corrosive properties of oil palm frond lignins extracted with different techniques. }, journal = {Ann. Forest Sc. }, volume = {72}, year = {2015}, month = {2015}, chapter = {17}, author = {M.H. HUSSIN and A. MOHD-SHAH and A.A. RAHIM and M.N. MOHAMAD-IBRAHIM and D. PERRIN and N. BROSSE} } @article {1568, title = { Characterization of Miscanthus pyrolysis by DRIFTs, UV Raman spectroscopy and mass spectrometry }, journal = { JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS }, volume = {113}, year = {2015}, pages = {402-411}, abstract = {

The aim of this work was to identify and quantify the chemical and structural modifications occurring during the pyrolysis of Miscanthus x giganteus. Miscanthus was pyrolyzed at slow heating rate (5 K/min) in the temperature range 200-400 degrees C. The biochars were then characterized by combining diffuse reflectance infrared Fourier transform spectrometry (DRIFTs) and Ultraviolet Raman spectrometry (UV Raman). In addition, the quantification of the functional groups remained on the biochars was conducted by temperature programmed desorption-mass spectrometer (TPD-MS) analysis.

DRIFT analysis showed that the decrease in the hydroxyl and C-H stretching bands and the evolution of the carboxyl vibration peak mainly occur between 300 and 350 degrees C. The evolution of the main markers (H2O, CO, CO2, CH4, and H-2) of the functional groups presents in the biochars as analyzed by TPD-MS is consistent with the spectroscopic analysis. It shows two peaks. The first one in the temperature range of 200-380 degrees C was explained by the loss of the main O- and H- containing groups and to the main primary volatile compounds. The second step (above 380 degrees C) can be interpreted by the rearrangement of the aromatic rings in the polycyclic structure.

}, url = {https://hal.archives-ouvertes.fr/hal-01230722}, author = {Y. ELMAY and Y. LE-BRECH and L. DELMOTTE and A. DUFOUR and N. BROSSE and R. GADIOU} } @article {1252, title = {Enhanced properties of oil palm fronds (OPF) lignin fractions produced via tangential ultrafiltration technique }, journal = {Ind. Crops \& Prod.}, volume = {66}, year = {2015}, month = {2015}, chapter = {1}, author = {M.H. HUSSIN and A.A. RAHIM and M.N. MOHAMAD-IBRAHIM and D. PERRIN and N. BROSSE} } @article {1250, title = {Enhancement of mechanical strength of environmentally friendly Pinus tannins adhesives for particleboards production using cellulose nanofibers.}, journal = {Ann. Forest Sc.}, volume = {72}, year = {2015}, pages = {27-32}, abstract = {

Condensed tannins have been successfully used as substitutes for phenol in the production of resins for wood products. However, the enhancement of the properties of tannin-based resins with nontoxic and cost effective additives is of great interest.

In the present work, the performance enhancement of tannin-based particleboards with cellulose nanofibers was investigated.

In presence of 2 \% of cellulose nanofibers, the viscosity of tannin-based adhesives and the internal bonding strength (IB) of the corresponding particleboards were increased from 350 to 5,462 mPa center dot s and from 0.85 to 0.98 MPa respectively. The modulus of elastic (MOE) and modulus of rupture (MOR) of the resins were also notably increased while thickness swelling (TS) of the panels was not affected.

The addition of cellulose nanofibers to tannin adhesives is an effective method for the production of high performance particleboards. Tannin-based adhesive containing 2 \% of cellulose nanofibers exhibits the best mechanical strength.

The addition of cellulose nanofibers into tannin-based adhesives notably enhanced the mechanical properties of the wood particleboards produced. The formulation containing 2 \% (w/w) of cellulose nanofibers exhibited the best mechanical strength.

}, author = {J. CUI and X. LU and X. ZHOU and L. CHRUSCIEL and Y. DENG and H. ZHOU and S. ZHU and N. BROSSE} } @article {1579, title = { High Resolution Solid State 2D NMR Analysis of Biomass and Biochar }, journal = { ANALYTICAL CHEMISTRY }, volume = {87}, year = {2015}, pages = {843-847}, abstract = {

Solid state NMR methods are required to analyze biomass as a function of its chemical or biological treatment for biofuels, chemicals, or biochar production. The native polymers network in lignocellulosic biomass and other solid materials, such as coal, coke, or biochar, can hardly be analyzed by liquid state NMR due to their poor swelling ability without chemical modification. A H-1-C-13 two-dimensional heteronuclear correlation (HETCOR) experiment with frequency-switched Lee-Goldburg (FSLG) irradiation is performed on a high field spectrometer (750 MHz). This method leads to previously unattained resolution for biomass and biochar and offers a unique ability to reveal their chemical composition. The formation of aromatic moieties from carbohydrates and lignin thermal conversion is clearly distinguished. This method can be applied to all other carbonaceous materials.

}, url = {https://hal.archives-ouvertes.fr/hal-01101584}, author = {Y. LE-BRECH and L. DELMOTTE and J. RAYA and N. BROSSE and R. GADIOU and A. DUFOUR} } @article {1557, title = {Improved corrosion inhibition of mild steel by chemically modified lignin polymers from Elaeis guineensis agricultural waste}, journal = {MATERIALS CHEMISTRY AND PHYSICS}, volume = {163}, year = {2015}, pages = {201-212}, abstract = {

This article describes that the modification of lignin by incorporation of aromatic scavengers (2-naphthol: AHN EOL and 1,8-dihydroxyanthraquinone: AHD EOL) during delignification process has improved the physical properties of the lignin fractions. Smaller fragments of lignin with high phenolic -OH content, increased solubility and antioxidant activity have led to improved inhibitive property of the modified lignin. The inhibition efficiency (84-93\%) of both modified lignin (500 ppm) were observed to be better than unmodified organosolv lignin (EOL). It was deduced that the inhibition process was spontaneous and the inhibitors were mainly physically adsorbed onto the mild steel surface.

}, author = {M.H. HUSSIN and A.A. RAHIM and M.N.M. IBRAHIM and N. BROSSE} } @article {1253, title = {Lophira Lanceolata seed oil extraction method (ancestral or modern) modifies the properties of the oil}, journal = {Ind. Crops \& Prod.}, year = {2015}, month = {2015}, author = {G. NONVIHO and C. PARIS and L. MUNIGLIA and D. SOHOUNHLOUE and N. BROSSE} } @article {1544, title = {Preparation and Characterization of Lignin Polyols from the Residues of Oil Palm Empty Fruit Bunch}, journal = {BIORESOURCES}, volume = {10}, year = {2015}, pages = {7339-7352}, abstract = {

In this work, lignin polyols were prepared from the liquefaction of kraft lignin and from the direct liquefaction of Elaeis guineensis lignocellulosic waste. The liquefaction reaction was performed with polyhydric alcohols using sulfuric acid as catalyst at 160 degrees C. The physical and chemical characterizations of lignin and lignin polyols were conducted by elemental analysis, Fourier transform-infrared spectroscopy, H-1 and C-13 nuclear magnetic resonance (NMR) spectroscopy, molecular weight distribution, and thermogravimetric analysis (TGA). Quantitative C-13 NMR showed that all aliphatic hydroxyl group values of polyols noticeably increased with the use of the two methods compared to kraft lignin. The average molecular weight analysis of the liquefied product showed that it exhibited high molecular weight compared to kraft lignin. Both structural and thermal characteristics suggest that lignin polyols would be a good substitute for kraft lignin in the synthesis of polymeric compounds such as environmentally friendly resins or wood adhesives, as it presents higher amounts of activated free ring positions, higher molecular weight, and high thermal stability.

}, url = {https://hal.archives-ouvertes.fr/LERMAB-UL/hal-01598213}, author = {A.H. FARIS and M.N.M. IBRAHIM and A.A. RAHIM and M.H. HUSSIN and N. BROSSE} } @article {1251, title = {Resolution solid state 2D NMR analysis of biomass and biochar }, journal = {Analytical Chemistry }, volume = {87}, year = {2015}, month = {2015}, chapter = {843}, author = {Y. LEBRECH and L. DELMOTTE and J. RAYA and N. BROSSE and R. GADIOU and A. DUFOUR} } @article {1246, title = {Composition of Lophira lanceolata and Carapa procera seed oils. }, journal = {Research Journal of Chemical Sciences}, volume = {4}, year = {2014}, month = {2014}, chapter = {57}, author = {G. NONVIHO and C. PARIS and L. MUNIGLIA and P. SESSOU and P. AGBANGNAN and N. BROSSE and D. SOHOUNLOUE} } @article {1244, title = {Impact of catalytic oil palm fronds (OPF)pulping on organosolv lignin properties. }, journal = {Polymer Degradation and Stability}, volume = {109}, year = {2014}, month = {2014}, chapter = {33}, author = {M.H. HUSSIN and A.A. RAHIM and M.N. MOHAMAD-IBRAHIM and D. PERRIN and M. YEMLOUL and N. BROSSE} } @article {702, title = {Investigation on the structure and antioxidant properties of modified lignin obtained by different combinative processes of oil palm fronds (OPF) biomass}, journal = {Industrial crops and products. }, volume = {52}, year = {2014}, month = {2014}, chapter = {544-551}, author = {MH. HUSSIN and A. RAHIM and MNM. IBRAHIM and M. YEMLOUL and D. PERRIN and N. BROSSE} } @article {1245, title = {UPLC method for the determination of vitamin E homologue and derivatives in vegetable oils, margarines and supplement capsules using pentafluorophenyl column}, journal = {Talanta}, volume = {130}, year = {2014}, month = {2014}, chapter = {299}, author = {Y. FOO-WONG and A. MAKAHLEH and B. SAAD and M.N. MOHAMAD-IBRAHIM and A.A. RAHIM and N. BROSSE} } @article {591, title = {Compositions and chemical variability of grape pomaces from french vineyard}, journal = {Ind crops prod}, volume = {43}, year = {2013}, month = {2013}, chapter = {251-254}, author = {P. RONDEAU and F. GAMBIER and F. JOLIBERT and N. BROSSE} } @article {592, title = {Investigation of the Effects of 1-Butyl-3-Methylimidazolium Acetate Pretreatment and Enzymatic Hydrolysis of Typha capensis}, journal = {Idi. Energy and Fuel }, volume = {27}, year = {2013}, month = {2013}, chapter = {189-196}, author = {G. AUDU and N. BROSSE and L. DESHARNAIS and K. SUDIT-RAKSHIT} } @article {594, title = {Revealing the chemistry of biomass thermal conversion by means of tunable synchrotron ionisation - mass spectrometry}, journal = {RCS Advances}, volume = {3}, year = {2013}, month = {2013}, chapter = {4786-4792}, author = {A. DUFOUR and J. WENG and L. JIA and X. TANG and R. FOURNET and N. BROSSE and B. SIRJEAN and G. MAUVIEL and F. QI} } @article {1239, title = {Combination enzymatic hydrolysis and ethanol organosolv pretreatments : effect on lignin structures, delignification yields and cellulose-to-glucose conversion }, journal = {Bioressources Technology}, volume = {112}, year = {2012}, month = {2012}, chapter = {156}, author = {P. OBAMA and G. RICOCHON and L. MUNIGLIA and N. BROSSE} } @article {583, title = {Effect of the pre-treatment severity on the antioxidant properties of ethanol organosolv Miscanthus x giganteus lignin}, journal = {Natural Resources}, volume = {3}, year = {2012}, month = {2012}, chapter = {29-34}, author = {R. ELHAGE and D. PERRIN and N. BROSSE} } @article {1241, title = {Ethanol organosolv pretreatment of Typha Capensis for bio-ethanol production and co-products }, journal = {BioRessources}, volume = {7}, year = {2012}, month = {2012}, chapter = {5917}, author = {I.G. AUDU and N. BROSSE and L. DESHARNAIS and S.K. RAKSHIT} } @article {1240, title = {Miscanthus: a fast growing crop for bio-fuels and chemicals production }, journal = {Biofuels Bioproducts and Biorefining}, volume = {6}, year = {2012}, month = {2012}, chapter = {580}, author = {N. BROSSE and A. DUFOUR and M. XIANZHI and Q. SUN and A. RAGAUSKAS} } @article {1238, title = {Origin of molecular mobility during biomass pyrolysis as revealed by in situ 1H 1NMR analysis}, journal = {ChemSusChem}, volume = {5}, year = {2012}, month = {2012}, chapter = {1}, author = {A. DUFOUR and M. CASTRO-DIAZ and N. BROSSE and M. BOUROUKB and C. SNAPE} }