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2017, Publications.

2017


  • Boisson S, Faucon M-P, Le Stradic S, et al. Specialized edaphic niches of threatened copper endemic plant species in the D.R. Congo: implications for ex situ conservation. Plant and soil 2017; 413: 261-273.
    Résumé : Background and aimsCopper (Cu) rich soils derived from rocks of the Katangan Copperbelt in the south-eastern Democratic Republic of Congo (DRC) support a rich diversity of metallophytes including 550 heavy metal tolerant; 24 broad Cu soil endemic; and 33 strict Cu soil endemic plant species. The majority of the plant species occur on prominent Cu hills scattered along the copperbelt. Heavy metal mining on the Katangan Copperbelt has resulted in extensive degradation and destruction of the Cu hill ecosystems. As a result, approximately 80 % of the strict Cu endemic plant species are classified as threatened according to IUCN criteria and represent a conservation priority. Little is known about the soil Cu tolerance optimum of the Cu endemic plant species. The purpose of this study was to quantify the soil Cu concentration (Cu edaphic niche) of four Cu endemic plant species to inform soil propagation conditions and microhabitat site selection for planting of the species in Cu hill ecosystem restoration.MethodsThe soil Cu concentration tolerance of Cu endemic plant species was studied including Crotalaria cobalticola (CRCO); Gladiolus ledoctei (GLLE); Diplolophium marthozianum (DIMA); and Triumfetta welwitschii var. rogersii (TRWE-RO). The in situ natural habitat distributions of the Cu endemic plant species with respect to soil Cu concentration (Cu edaphic niche) was calculated by means of a generalised additive model. Additionally, the seedling emergence and growth of the four Cu endemic plant species in three soil Cu concentrations was tested ex situ and the results were compared to that of the natural habitat soil Cu concentration optimum (Cu edaphic niche).ResultsCRCO exhibited greater performance on the highest soil Cu concentration, consistent with its calculated Cu edaphic niche occurring at the highest soil Cu concentrations. In contrast, both DIMA and TRWE-RO exhibited greatest performance at the lowest soil Cu concentration, despite the calculated Cu edaphic niche occurring at moderate soil Cu concentrations. GLLE exhibited equal performances in the entire range of soil Cu concentrations.ConclusionsThese results suggest that CRCO evolved via the edaphic specialization model where it is most competitive in Cu hill habitat with the highest soil Cu concentration. In comparison, DIMA and TRWE-RO appear to have evolved via the endemism refuge model, which indicates that the species were excluded into (i.e., took refuge in) the lower plant competition Cu hill habitat due to their inability to effectively compete with higher plant competition on normal soils. The soil Cu edaphic niche determined for the four species will be useful in conservation activities including informing soil propagation conditions and microhabitat site selection for planting of the species in Cu hill ecosystem restoration.


  • Brahim M, Checa Fernandez BL, Regnier O, et al. Impact of ultrasounds and high voltage electrical discharges on physico-chemical properties of rapeseed straw’s lignin and pulps. Bioresource Technology 2017; 237: 11-19.
    Résumé : In this study, ultrasound (US) and high voltage electrical discharges (HVED) were combined with chemical treatments (soda or organosolv) for rapeseed straw delignification. Delignification was improved by both physical pretreatments. US increased the extractability of hemicelluloses and HVED induced a partial degradation of cellulose. Best synergies were observed for HVED-soda and US-organosolv treatments. The obtained lignin fractions were characterized with 13C NMR and 2D 1H–13C HSQC. It was observed that the physical treatments affected the syringyl/guaiacyl (S/G) ratios. The values of S/G were ≈1.19, 1.31 and 1.75 for organosolv, HVED-organosolv and US-organosolv processes, suggesting recondensation reactions. The lignin fractions obtained from HVED-organosolv treatment contained less quantity of p-coumaric acid and ferulic acid as compared to those extracted by US-organosolv. Thermogravimetric analysis (TGA) revealed a better heat resistance of physically extracted lignins as compared to the control. The enzymatic digestibility increased by 24.92% when applying HVED to mild organosolv treatment.
    Mots-clés : Delignification, High voltage electrical discharges, Organosolv, Soda, Ultrasound.


  • Dupoiron S, Lameloise M-L, Pommet M, et al. A novel and integrative process: From enzymatic fractionation of wheat bran with a hemicellulasic cocktail to the recovery of ferulic acid by weak anion exchange resin. Industrial Crops and Products 2017; 105: 148-155.
    Résumé : An integrated and eco-friendly process including enzymatic hydrolysis with a hemicellulasic cocktail and a chromatographic purification step was developed to obtain ferulic acid from wheat bran. Thermobacillus xylanilyticus, a thermophilic and hemicellulolytic bacterium, was able to produce enzymatic cocktails containing xylanase, xylosidase, arabinosidase and esterase activities. The cocktails produced were used to deconstruct destarched wheat bran, allowing the release of 6%, 20% and 37% (w/w) of monomeric arabinose, xylose and ferulic acid, respectively. A weak anionic resin under free-base form was proved successful to separate the carbohydrate fraction from the ferulate one after acidification. Ferulate was recovered at high concentration (15g/L) during regeneration of the resin. This non-optimized purification step allowed recovering 67% of ferulic acid fixed on the resin. Global recovery of ferulic acid contained in wheat bran after both enzymatic fractionation and purification stages reached 21.8%.
    Mots-clés : Biorefinery, Ferulic acid, Weak anionic resin, Xylans.


  • Gallos A, Paës G, Allais F, Beaugrand J. Lignocellulosic fibers: a critical review of the extrusion process for enhancement of the properties of natural fiber composites. RSC Advances 2017; 7: 34638-34654.
    Résumé : Natural fiber composites have various applications, since they can bring interesting mechanical and sustainability properties. Extrusion with a single- or twin-screw is the main industrial process to incorporate lignocellulosic fibers into polymers. In this review, the origin and preparation of lignocellulosic fibers are first presented, before discussing the composite processing, with a particular emphasis on the impact of process conditions on the composites final properties that is highly related to the final application. A broad panel of composites reinforced with lignocellulosic fibers is reviewed along with their polymeric matrix, lignocellulosic fiber type and pretreatments, and extrusion process conditions. Finally, the most critical extrusion process parameters (screw profile, speed and temperature) are also examined in order to determine some guidelines to optimize lignocellulosic fiber composites preparation.


  • Gallos A, Paës G, Legland D, Allais F, Beaugrand J. Exploring the microstructure of natural fibre composites by confocal Raman imaging and image analysis. Composites Part A: Applied Science and Manufacturing 2017; 94: 32-40.
    Résumé : We describe a combination of Confocal Raman Imaging (CRI) and quantitative image analysis to characterise biocomposite material microstructures. Both techniques offer lateral resolutions close to 1.3μm and axial resolution of 13μm, while simplifying sample preparation to hand-cutting without any surface preparation. Extruded and injected polycaprolactone/hemp fibre composites were used as demonstration biocomposites. A green macrobisphenol additive (bis-O-dihydroferuloyl-1,4-butanediol) was also used as a chemical probe to characterise the dispersion efficiency of additives, with a detection threshold of 2.3wt% above which very local heterogeneity can be determined by this technique. CRI provided microstructure information for the entire binary structure formed by the fibre network. The fibre dispersion and orientation depend on their location in the matrix, and the specific surface of the fibres increases with the fibre content as aggregates start to develop. The technique also highlighted a possible core-skin effect in the injected composite.
    Mots-clés : A. Natural fibre, B. Microstructure, C. Numerical analysis, D. Surface analysis.


  • Gallos A, Paës G, Legland D, Beaugrand J, Allais F. A microstructural and chemical approach to highlight how a simple methyl group affects the mechanical properties of a natural fibers composite. ACS Sustainable Chemistry & Engineering 2017. doi:10.1021/acssuschemeng.7b02399.
    Résumé : Two ferulic acid derivatives (BDF and BDF-Me) were prepared using chemo-enzymatic synthesis and used as additives for the pretreatment of hemp fibers. Incorporation of these fibers into a polycaprolactone matrix by hot-melt extrusion process aimed to improve the dispersion of the fibers and the mechanical properties of the resulting materials. Young's modulus and tensile strength of the composites were investigated at the micrometer scale by chemical imaging. The very simple methylation of the phenolic functions led to significant mechanical properties differences due to the dispersion of the fibers caused by a plasticizing effect of the ferulic acid derivative. This significant plasticizing effect of BDF-Me is observed at a content as low as 0.8 w% and opens the way for synthesizing a new family of biobased plasticizers involving transition from crystal state to amorphous phase.


  • Guénin S, Hardouin J, Paynel F, et al. AtPME3, a ubiquitous cell wall pectin methylesterase of Arabidopsis thaliana, alters the metabolism of cruciferin seed storage proteins during post-germinative growth of seedlings. Journal of Experimental Botany 2017; 68: 1083-1095.
    Résumé : AtPME3 (At3g14310) is a ubiquitous cell wall pectin methylesterase. Atpme3-1 loss-of-function mutants exhibited distinct phenotypes from the wild type (WT), and were characterized by earlier germination and reduction of root hair production. These phenotypical traits were correlated with the accumulation of a 21.5-kDa protein in the different organs of 4-day-old Atpme3-1 seedlings grown in the dark, as well as in 6-week-old mutant plants. Microarray analysis showed significant down-regulation of the genes encoding several pectin-degrading enzymes and enzymes involved in lipid and protein metabolism in the hypocotyl of 4-day-old dark grown mutant seedlings. Accordingly, there was a decrease in proteolytic activity of the mutant as compared with the WT. Among the genes specifying seed storage proteins, two encoding CRUCIFERINS were up-regulated. Additional analysis by RT-qPCR showed an overexpression of four CRUCIFERIN genes in the mutant Atpme3-1, in which precursors of the α- and β-subunits of CRUCIFERIN accumulated. Together, these results provide evidence for a link between AtPME3, present in the cell wall, and CRUCIFERIN metabolism that occurs in vacuoles.
    Mots-clés : Arabidopsis, AtPME3, CRUCIFERIN, etiolated hypocotyl, seed germination, transcriptomic analyses..


  • Hano C, Corbin C, Drouet S, et al. The lignan (+)-secoisolariciresinol extracted from flax hulls is an effective protectant of linseed oil and its emulsion against oxidative damage. European Journal of Lipid Science and Technology 2017. doi:10.1002/ejlt.201600219.
    Résumé : Secoisolariciresinol (SECO) is a natural antioxidant lignan accumulated in large amounts in the seedcoat of flax and retained in the flaxseed cake residue during linseed oil pressing. Here SECO was extracted and purified from flaxseed cake and assayed for its ability to prevent oxidation of linseed oil and an o/w emulsion containing linseed oil. For this purpose, an accelerated storage (Schaal oven) test was performed and SECO effectiveness was compared to that of two antioxidants commonly used in food and cosmetic products: α-tocopherol (α-TOCO) and butylated hydroxyanisole (BHA). In our hands, SECO addition, ranging from 50 to 500 μmole per kg oil, significantly decreased the production of both primary (conjugated dienes, CD) and secondary (thiobarbituric acid-reactive substances, TBARS) oxidation products. This study evidenced that SECO is an effective stabilizer of linseed oil and its o/w emulsion and this protective effect outperformed both the natural α-TOCO and the synthetic BHA antioxidants. In particular, SECO was the most effective in the protection of the o/w emulsion against secondary oxidation products, which makes it a potential alternative preservative for oily products in foods and cosmetics. Practical applications: The present study could lead to applications in the food and cosmetic industries for the stabilization of o/w emulsions. Addition of SECO to linseed oil, already rich in ω-3, could also result in a new functional food with synergistic beneficial actions on human health.


  • Hardy B, Cornelis J-T, Houben D, Leifeld J, Lambert R, Dufey J. Evaluation of the long-term effect of biochar on properties of temperate agricultural soil at pre-industrial charcoal kiln sites in Wallonia, Belgium. European Journal of Soil Science 2017; 68. doi:10.1111/ejss.12395.
    Résumé : Research on biochar has increased, but its long-term effect on the fertility of temperate agricultural soil remains unclear. In Wallonia, Belgium, pre-industrial charcoal production affected former forested areas that were cleared for cultivation in the nineteenth century. The sites of traditional charcoal kilns, largely enriched in charcoal residues, are similar to soil amended with hardwood biochar more than 150 years ago. We sampled 17 charcoal kiln sites to characterize their effect on soil properties compared with adjacent reference soils. Charcoal-C content was estimated by differential scanning calorimetry. The kiln soil contains from 1.8 to 33.1 g kg−1 of charcoal-C, which markedly increases organic C:N and C:P ratios. It also contains slightly more uncharred soil organic carbon (SOC) than the reference soil, which accords with larger total N content. We measured a small increase in nitrates in the kiln soil that might relate to greater mineralization and nitrification of organic N. Frequent application of lime raised the pH to values close to neutral, which offset the residual effect of charcoal production on soil acidity. A cation exchange capacity (CEC) of 414 cmolc kg−1 was estimated for charcoal-C, whereas that of uncharred SOC was 213 cmolc kg−1. Despite the large CEC of the kiln soil, exchangeable K+ content was no different from the adjacent soil, whereas exchangeable Ca2+ and Mg2+ contents were considerably larger. Charcoal enrichment has little effect on available, inorganic and total P, but it can form strong complexes with Cu, which reduces the availability of the metal. Biochar is very persistent in soil; therefore, long-term implications should not be overlooked.


  • Hocq L, Sénéchal F, Lefebvre V, et al. Combined Experimental and Computational Approaches Reveal Distinct pH Dependence of Pectin Methylesterase Inhibitors. Plant Physiology 2017; 173: 1075-1093.
    Résumé : The fine-tuning of the degree of methylesterification of cell wall pectin is a key to regulating cell elongation and ultimately the shape of the plant body. Pectin methylesterification is spatiotemporally controlled by pectin methylesterases (PMEs; 66 members in Arabidopsis [Arabidopsis thaliana]). The comparably large number of proteinaceous pectin methylesterase inhibitors (PMEIs; 76 members in Arabidopsis) questions the specificity of the PME-PMEI interaction and the functional role of such abundance. To understand the difference, or redundancy, between PMEIs, we used molecular dynamics (MD) simulations to predict the behavior of two PMEIs that are coexpressed and have distinct effects on plant development: AtPMEI4 and AtPMEI9. Simulations revealed the structural determinants of the pH dependence for the interaction of these inhibitors with AtPME3, a major PME expressed in roots. Key residues that are likely to play a role in the pH dependence were identified. The predictions obtained from MD simulations were confirmed in vitro, showing that AtPMEI9 is a stronger, less pH-independent inhibitor compared with AtPMEI4. Using pollen tubes as a developmental model, we showed that these biochemical differences have a biological significance. Application of purified proteins at pH ranges in which PMEI inhibition differed between AtPMEI4 and AtPMEI9 had distinct consequences on pollen tube elongation. Therefore, MD simulations have proven to be a powerful tool to predict functional diversity between PMEIs, allowing the discovery of a strategy that may be used by PMEIs to inhibit PMEs in different microenvironmental conditions and paving the way to identify the specific role of PMEI diversity in muro.
    Mots-clés : Arabidopsis, Arabidopsis Proteins, Carboxylic Ester Hydrolases, Cell Wall, Computational Biology, Enzyme Inhibitors, Escherichia coli, Gene Expression Regulation, Plant, Germination, Hydrogen Bonding, Hydrogen-Ion Concentration, Hypocotyl, Molecular Dynamics Simulation, Plant Roots, Pollen Tube, Recombinant Proteins.


  • Hodroge A, Trécherel E, Cornu M, et al. Oligogalacturonic Acid Inhibits Vascular Calcification by Two Mechanisms: Inhibition of Vascular Smooth Muscle Cell Osteogenic Conversion and Interaction With Collagen. Arteriosclerosis, Thrombosis, and Vascular Biology 2017; 37: 1391-1401.
    Résumé : OBJECTIVE: Cardiovascular diseases constitute the leading cause of mortality worldwide. Calcification of the vessel wall is associated with cardiovascular morbidity and mortality in patients having many diseases, including diabetes mellitus, atherosclerosis, and chronic kidney disease. Vascular calcification is actively regulated by inductive and inhibitory mechanisms (including vascular smooth muscle cell adaptation) and results from an active osteogenic process. During the calcification process, extracellular vesicles (also known as matrix vesicles) released by vascular smooth muscle cells interact with type I collagen and then act as nucleating foci for calcium crystallization. Our primary objective was to identify new, natural molecules that inhibit the vascular calcification process. APPROACH AND RESULTS: We have found that oligogalacturonic acids (obtained by the acid hydrolysis of polygalacturonic acid) reduce in vitro inorganic phosphate-induced calcification of vascular smooth muscle cells by 80% and inorganic phosphate-induced calcification of isolated rat aortic rings by 50%. A specific oligogalacturonic acid with a degree of polymerization of 8 (DP8) was found to inhibit the expression of osteogenic markers and, thus, prevent the conversion of vascular smooth muscle cells into osteoblast-like cells. We also evidenced in biochemical and immunofluorescence assays a direct interaction between matrix vesicles and type I collagen via the GFOGER sequence (where single letter amino acid nomenclature is used, O=hydroxyproline) thought to be involved in interactions with several pairs of integrins. CONCLUSIONS: DP8 inhibits vascular calcification development mainly by inhibition of osteogenic marker expression but also partly by masking the GFOGER sequence-thereby, preventing matrix vesicles from binding to type I collagen.
    Mots-clés : Animals, Aorta, Thoracic, Aortic Diseases, Binding Sites, Biomarkers, Calcium, Cell Transdifferentiation, Cells, Cultured, Collagen Type I, Crystallization, Dose-Response Relationship, Drug, Extracellular Vesicles, Male, matrix vesicle, Mice, Muscle, Smooth, Vascular, Myocytes, Smooth Muscle, oligogalacturonic acid, Oligosaccharides, Osteogenesis, Protein Binding, Protein Interaction Domains and Motifs, Rats, Wistar, Signal Transduction, Tissue Culture Techniques, type I collagen, Vascular Calcification.

  • Houben D, Hardy B, Faucon M-P, Cornelis J-T. Effect of biochar on phosphorus bioavailability in an acidic silt loam soil - Effet du biochar sur la biodisponibilité du phosphore dans un sol limoneux acide. Biotechnology, Agronomy and Society and Environment 2017.http://popups.ulg.ac.be/1780-4507/index.php?id=13539 (consulté sans date).
    Résumé : Description du sujet. Cet article traite de l'impact du biochar sur la biodisponibilité en phosphore (P) dans les sols en vue d'améliorer la gestion et l'autonomie de la fertilisation en P des cultures. Objectifs. L'objectif général était d'explorer le potentiel du biochar à augmenter la biodisponibilité du P dans le sol. Les objectifs spécifiques étaient de préciser l'influence de la biomasse pyrolysée ainsi que la dose de biochar appliquée sur la solubilité du P. Méthode. Trois biochars produits à partir de biomasses différentes (résidus de Miscanthus, de bois et de café) ont été incorporés dans un Luvisol (pH acide) selon deux doses (1 et 3 % en masse). Après 76 jours d'incubation, la biodisponibilité du P a été estimée (extraction au CaCl 2 0,01 M). Les propriétés physico-chimiques du sol et la quantité de CO 2 émise durant la période d'incubation ont également été déterminées. Résultats. Seul le biochar produit à partir de résidus de bois et incorporé à une dose de 3 % a augmenté la concentration en P biodisponible dans le sol (+ 75 %). Cette augmentation résulterait non seulement d'une libération de P par le biochar lui-même (effet direct), mais également d'une remobilisation du P du sol (effet indirect) faisant suite à l'élévation drastique du pH (+ 3,6 unités) ainsi qu'à l'augmentation de l'activité biologique. Pour les autres traitements, l'absence d'effet significatif sur la biodisponibilité du P résulte vraisemblablement de leur faible impact sur le pH du sol, celui-ci restant dans une gamme (4,3 – 5,1) favorisant l'insolubilisation du P. Conclusions. Étant donné la variabilité des résultats et les incertitudes concernant les mécanismes responsables de la mobilisation du P en présence de biochar, il est essentiel de conduire des études complémentaires afin de mieux comprendre l'impact du biochar sur la mobilité du P dans les systèmes sol-plante. Effect of biochar on phosphorus bioavailability in an acidic silt loam soil Description of the subject. This paper deals with the impact of biochar on soil phosphorus (P) bioavailability with a view to improving the management of P fertilization. Objectives. The aim of this study was to explore the potential of biochar to increase P bioavailability in soil. The specific objectives were to elucidate the role of feedstock and the rate of application of biochar on P solubility. Method. Three biochars produced from different feedstocks (Miscanthus straws, coffee husks and woody material) were added to an acidic Luvisol at two rates of application (1% and 3%; w/w). At the end of a 76-day incubation period, P bioavailability was assessed (0.01 M CaCl 2 extraction). Soil physico-chemical properties and the amount of CO 2 emitted over the incubation period were also determined. Results. The wood-derived biochar applied at 3% was the only treatment that increased significantly P bioavailability (+ 75%). This increase might result from the release of P by biochar itself (direct effect) but also from an enhanced P solubility in soil (indirect effect) related to a large increase in pH (+3.6 units compared to the control) and a higher soil biological activity. The other treatments had no significant impact on soil P bioavailability, probably as a result of their minor effect on soil pH. Conclusions. Our study shows that biochar-induced changes in P bioavailability in soil varied greatly with type of feedstock and rate of application. However, the balance between the direct and indirect effects of biochar on P bioavailability was not elucidated. Further investigations are thus essential to clarify the potential of biochar to improve P bioavailability in the soil-plant system.


  • Husson E, Hadad C, Huet G, et al. The effect of room temperature ionic liquids on the selective biocatalytic hydrolysis of chitin via sequential or simultaneous strategies. Green Chemistry 2017; 19: 4122-4131.
    Résumé : An efficient conversion of chitin, the second most abundant renewable polymer on the Earth, into N-acetylglucosamine and N,N′-diacetylchitobiose, using room temperature ionic liquids (RTILs) and commercially available chitinases is described for the first time. The sequential strategy consists of the use of RTILs to pretreat chitin under mild conditions as a first step before enzymatic hydrolysis. [C2mim][OAc] (1-ethyl-3-methyl imidazolium) pretreatment provides an efficient production of N-acetylglucosamine (185.0 ± 4.0 mg per g chitin) or N,N′-diacetylchitobiose (667.60 ± 20.71 mg per g chitin) catalyzed by chitinase from Trichoderma viride or Streptomyces griseus, respectively. A thorough investigation of the structural changes of chitin induced by RTIL pretreatment suggested an increase in enzymes’ accessibility to the chitin substrate. Alternatively, a one-pot enzymatic hydrolysis of chitin in [C2mim][OAc]-aqueous medium constitutes a promising simultaneous route to selectively generate N-acetylglucosamine or N,N′-diacetylchitobiose by decreasing the required [C2mim][OAc] amount and the number of steps. Finally, the combination of the two chitinases from T. viride and S. griseus was shown to be very relevant to considerably increase the production of N-acetylglucosamine up to 760.0 ± 0.1 mg per g chitin.


  • Janvier M, Hollande L, Jaufurally AS, et al. Syringaresinol: A Renewable and Safer Alternative to Bisphenol A for Epoxy-Amine Resins. ChemSusChem 2017; 10: 738-746.
    Résumé : A renewable bisepoxide, SYR-EPO, was prepared from syringaresinol, a naturally occurring bisphenol deriving from sinapic acid, by using a chemo-enzymatic synthetic pathway. Estrogenic activity tests revealed no endocrine disruption for syringaresinol. Its glycidylation afforded SYR-EPO with excellent yield and purity. This biobased, safe epoxy precursor was then cured with conventional and renewable diamines for the preparation of epoxy-amine resins. The resulting thermosets were thermally and mechanically characterized. Thermal analyses of these new resins showed excellent thermal stabilities (Td5 % =279-309 °C) and Tg ranging from 73 to 126 °C, almost reaching the properties of those obtained with the diglycidylether of bisphenol A (DGEBA), extensively used in the polymer industry (Td5 % =319 °C and Tg =150 °C for DGEBA/isophorone diamine resins). Degradation studies in NaOH and HCl aqueous solutions also highlighted the robustness of the syringaresinol-based resins, similar to bisphenol A (BPA). All these results undoubtedly confirmed the potential of syringaresinol as a greener and safer substitute for BPA.
    Mots-clés : Amines, Benzhydryl Compounds, bisepoxide, bisphenol A, DGEBA, Epoxy Resins, Furans, Green Chemistry Technology, Lignans, Phenols, Polymers, resin, syringaresinol.


  • Kowalski D, Mallet J, Thomas S, et al. Electrochemical synthesis of 1D core-shell Si/TiO2 nanotubes for lithium ion batteries. Journal of Power Sources 2017; 361: 243-248.
    Résumé : Silicon negative electrode for lithium ion battery was designed in the form of self-organized 1D core-shell nanotubes to overcome shortcomings linked to silicon volume expansion upon lithiation/delithiation typically occurring with Si nanoparticles. The negative electrode was formed on TiO2 nanotubes in two step electrochemical synthesis by means of anodizing of titanium and electrodeposition of silicon using ionic liquid electrolytes. Remarkably, it was found that the silicon grows perpendicularly to the z-axis of nanotube and therefore its thickness can be precisely controlled by the charge passed in the electrochemical protocol. Deposited silicon creates a continuous Si network on TiO2 nanotubes without grain boundaries and particle-particle interfaces, defining its electrochemical characteristics under battery testing. In the core-shell system the titania nanotube play a role of volume expansion stabilizer framework holding the nanostructured silicon upon lithiation/delithiation. The nature of Si shell and presence of titania core determine stable performance as negative electrode tested in half cell of CR2032 coin cell battery.
    Mots-clés : Electrosynthesis, Nanotubes, Silicon, Silicon anode, Titania.


  • Labidi S, Firmin S, Verdin A, et al. Nature of fly ash amendments differently influences oxidative stress alleviation in four forest tree species and metal trace element phytostabilization in aged contaminated soil: A long-term field experiment. Ecotoxicology and Environmental Safety 2017; 138: 190-198.
    Résumé : Aided phytostabilization using coal fly ashes (CFAs) is an interesting technique to clean-up polluted soils and valorizing industrial wastes. In this context, our work aims to study the effect of two CFAs: silico-aluminous (CFA1) and sulfo-calcic (CFA2) ones, 10 years after their addition, on the phytostabilization of a highly Cd (cadmium), Pb (lead) and Zn (zinc) contaminated agricultural soil, with four forest tree species: Robinia pseudoacacia, Alnus glutinosa, Acer pseudoplatanus and Salix alba. To assess the effect of CFAs on trees, leaf fatty acid composition, malondialdehyde (MDA), oxidized and reduced glutathione contents ratio (GSSG: GSH), 8-hydroxy-2'-deoxyguanosine (8-OHdG), Peroxidase (PO) and Superoxide dismutase (SOD) activities were examined. Our results showed that CFA amendments decreased the CaCl2-extractable fraction of Cd and Zn from the soil. However, no significant effect was observed on metal trace element (MTE) concentrations in leaves. Fatty acid percentages were only affected by the addition of sulfo-calcic CFA. The most affected species were A. glutinosa and R. pseudoacacia in which C16:0, C18:0 and C18:2 percentages increased significantly whereas the C18:3 decreased. The addition of sulfo-calcic CFA induced the antioxidant systems response in tree leaves. An increase of SOD and POD activities in leaves of trees planted on the CFA2-amended plot was recorded. Conversely, silico-aluminous CFA generated a reduction of lipid and DNA oxidation associated with the absence or low induction of anti-oxidative processes. Our study evidenced oxidative stress alleviation in tree leaves due to CFA amendments. MTE mobility in contaminated soil and their accumulation in leaves differed with the nature of CFA amendments and the selected tree species.
    Mots-clés : Acer, Alnus, Biodegradation, Environmental, Cadmium, Coal Ash, Coal fly ashes, Deoxyguanosine, Fatty Acids, Forest trees, Glutathione, Lead, Malondialdehyde, MTE mobility, Oxidative Stress.


  • Lakraychi AE, Dolhem F, Djedaïni-Pilard F, Thiam A, Frayret C, Becuwe M. Decreasing redox voltage of terephthalate-based electrode material for Li-ion battery using substituent effect. Journal of Power Sources 2017; 359: 198-204.
    Résumé : The preparation and assessment versus lithium of a functionalized terephthalate-based as a potential new negative electrode material for Li-ion battery is presented. Inspired from molecular modelling, a decrease in redox potential is achieved through the symmetrical adjunction of electron-donating fragments (–CH3) on the aromatic ring. While the electrochemical activity of this organic material was maximized when used as nanocomposite and without any binder, the potential is furthermore lowered by 110 mV upon functionalization, consistently with predicted value gained from DFT calculations.
    Mots-clés : Binder-free electrode, DFT calculations, Organic anode material, Structure-property relationships, Substituent effect.


  • Lakraychi AE, Fahsi K, Aymard L, Poizot P, Dolhem F, Bonnet J-P. Carboxylic and sulfonic N-substituted naphthalene diimide salts as highly stable non-polymeric organic electrodes for lithium batteries. Electrochemistry Communications 2017; 76: 47-50.
    Résumé : Two N-substituted naphthalene tetracarboxylic diimide (NTCDI) ionic compounds, carboxylic and sulfonic sodium salts, were prepared and used as positive electrode active materials in lithium-half cells. The aim of this investigation was to assess the solubility-suppressing effect of two different negatively charged substituent groups on a redox-active organic backbone using a carbonate-based liquid electrolyte. NTCDI derivatives were obtained in high yields from reaction of naphthalene tetracarboxylic dianhydride with neutralized glycine or with neutralized taurine. They were mixed with carbon black and cycled in galvanostatic mode against lithium metal using 1M LiPF6 EC/DMC liquid electrolyte. These two NTCDI derivatives exhibit a quite stable electrochemical activity upon cycling at an average potential of 2.3V vs. Li+/Li0 giving rise to specific capacity values of 147mAh·g−1 and 113mAh·g−1 for the dicarboxylate and the disulfonate derivative, respectively. This study clearly supports the useful effect of such grafted permanent charges as a general rule on the electrochemical stability of crystallized organic materials based on the assembly of small redox-active units.
    Mots-clés : Lithium batteries, Naphthalene diimide, Organic batteries, Organic electrode.


  • Lange B, Van der Ent A, Baker AJM, et al. Copper and cobalt accumulation in plants: a critical assessment of the current state of knowledge. New Phytologist 2017; 213: 537-551.
    Résumé : This review synthesizes contemporary understanding of copper-cobalt (Cu-Co) tolerance and accumulation in plants. Accumulation of foliar Cu and Co to > 300 μg g-1 is exceptionally rare globally, and known principally from the Copperbelt of Central Africa. Cobalt accumulation is also observed in a limited number of nickel (Ni) hyperaccumulator plants occurring on ultramafic soils around the world. None of the putative Cu or Co hyperaccumulator plants appears to comply with the fundamental principle of hyperaccumulation, as foliar Cu-Co accumulation is strongly dose-dependent. Abnormally high plant tissue Cu concentrations occur only when plants are exposed to high soil Cu with a low root to shoot translocation factor. Most Cu-tolerant plants are Excluders sensu Baker and therefore setting nominal threshold values for Cu hyperaccumulation is not informative. Abnormal accumulation of Co occurs under similar circumstances in the Copperbelt of Central Africa as well as sporadically in Ni hyperaccumulator plants on ultramafic soils; however, Co-tolerant plants behave physiologically as Indicators sensu Baker. Practical application of Cu-Co accumulator plants in phytomining is limited due to their dose-dependent accumulation characteristics, although for Co field trials may be warranted on highly Co-contaminated mineral wastes because of its relatively high metal value.


  • Lenoir J, Hattab T, Pierre G. Climatic microrefugia under anthropogenic climate change: implications for species redistribution. Ecography 2017; 40: 253-266.
    Résumé : The role of modern climatic microrefugia is a neglected aspect in the study of biotic responses to anthropogenic climate change. Current projections of species redistribution at continental extent are based on climatic grids of coarse (≥ 1 km) resolutions that fail to capture spatiotemporal dynamics associated with climatic microrefugia. Here, we review recent methods to model the climatic component of potential microrefugia and highlight research gaps in accounting for the buffering capacity due to biophysical processes operating at very fine (< 1 m) resolutions (e.g. canopy cover) and the associated microclimatic stability over time (i.e. decoupling). To overcome this challenge, we propose a spatially hierarchical downscaling framework combining a free-air temperature grid at 1 km resolution, a digital elevation model at 25 m resolution and small-footprint light detection-and-ranging (LiDAR) data at 50 cm resolution with knowledge from the literature to mechanistically model sub-canopy temperatures and account for microclimatic decoupling. We applied this framework on a virtual sub-canopy species and simulated the impact of a warming scenario on its potential distribution. Modelling sub-canopy temperatures at 50 cm resolution and accounting for microclimatic stability over time enlarges the range of temperature conditions towards the cold end of the gradient, mitigates regional temperature changes and decreases extirpation risks. Incorporating these spatiotemporal dynamics into species redistribution models, being correlative, mechanistic or hybrid, will increase the probability of local persistence, which has important consequences in the understanding of the capacity of species to adapt. We finally provide a synthesis on additional ways that the field could move towards effectively considering potential climatic microrefugia for species redistribution.
    Mots-clés : Anthropogenic, Climate Change, Microrefugia.


  • Lu B, Miao Y, Vigneron P, et al. Measurement of cytotoxicity and irritancy potential of sugar-based surfactants on skin-related 3D models. Toxicology in Vitro 2017; 40: 305-312.
    Résumé : Sugar-based surfactants present surface-active properties and relatively low cytotoxicity. They are often considered as safe alternatives to currently used surfactants in cosmetic industries. In this study, four sugar-based surfactants, each with an eight carbon alkyl chain bound to a glucose or a maltose headgroup through an amide linkage, were synthesized and compared to two standard surfactants. The cytotoxic and irritant effects of surfactants were evaluated using two biologically relevant models: 3D dermal model (mouse fibroblasts embedded in collagen gel) and reconstituted human epidermis (RHE, multi-layered human keratinocytes). Results show that three synthesized surfactants possess lower cytotoxicity compared to standard surfactants as demonstrated in the 3D dermal model. Moreover, the IC50s of surfactants against the 3D dermal model are higher than IC50s obtained with the 2D dermal model (monolayer mouse fibroblasts). Both synthesized and standard surfactants show no irritant effects after 48h of topical application on RHE. Throughout the study, we demonstrate the difficulty to link the physico-chemical properties of surfactants and their cytotoxicity in complex models. More importantly, our data suggest that, prior to in vivo tests, a complete understanding of surfactant cytotoxicity or irritancy potential requires a combination of cellular and tissue models.
    Mots-clés : Cosmetic products testing, Cytotoxicity, Dermal equivalents, Irritancy screening, Reconstituted human epidermis, Sugar-based surfactants.


  • Muraille L, Aguié-Béghin V, Chabbert B, Molinari M. Bioinspired lignocellulosic films to understand the mechanical properties of lignified plant cell walls at nanoscale. Scientific Reports 2017; 7: 44065.
    Résumé : The physicochemical properties of plant fibres are determined by the fibre morphology and structural features of the cell wall, which is composed of three main layers that differ in chemical composition and architecture. This composition and hierarchical structure are responsible for many of the mechanical properties that are desirable for industrial applications. As interactions between the lignocellulosic polymers at the molecular level are the main factor governing the final cohesion and mechanical properties of plant fibres, atomic force microscopy (AFM) is well suited for the observation and measurement of their physical properties at nanoscale levels. Given the complexity of plant cell walls, we have developed a strategy based on lignocellulosic assemblies with increasing complexity to understand the influence of the different polymers on the nanomechanical properties. Measurements of the indentation moduli performed on one type of lignified cell wall compared with those performed on the corresponding lignocellulosic films clearly show the importance of the lignin in the mechanical properties of cell walls. Through this strategy, we envision a wide application of bioinspired systems in future studies of the physical properties of fibres.


  • Nasir MN, Lins L, Crowet J-M, et al. Differential Interaction of Synthetic Glycolipids with Biomimetic Plasma Membrane Lipids Correlates with the Plant Biological Response. Langmuir: the ACS journal of surfaces and colloids 2017; 33: 9979-9987.
    Résumé : Natural and synthetic amphiphilic molecules including lipopeptides, lipopolysaccharides, and glycolipids are able to induce defense mechanisms in plants. In the present work, the perception of two synthetic C14 rhamnolipids, namely, Alk-RL and Ac-RL, differing only at the level of the lipid tail terminal group have been investigated using biological and biophysical approaches. We showed that Alk-RL induces a stronger early signaling response in tobacco cell suspensions than does Ac-RL. The interactions of both synthetic RLs with simplified biomimetic membranes were further analyzed using experimental and in silico approaches. Our results indicate that the interactions of Alk-RL and Ac-RL with lipids were different in terms of insertion and molecular responses and were dependent on the lipid composition of model membranes. A more favorable insertion of Alk-RL than Ac-RL into lipid membranes is observed. Alk-RL forms more stable molecular assemblies than Ac-RL with phospholipids and sterols. At the molecular level, the presence of sterols tends to increase the RLs' interaction with lipid bilayers, with a fluidizing effect on the alkyl chains. Taken together, our findings suggest that the perception of these synthetic RLs at the membrane level could be related to a lipid-driven process depending on the organization of the membrane and the orientation of the RLs within the membrane and is correlated with the induction of early signaling responses in tobacco cells.


  • Nguyen T-K-O, Jamali A, Grand E, et al. Phenylpropanoid profiling reveals a class of hydroxycinnamoyl glucaric acid conjugates in Isatis tinctoria leaves. Phytochemistry 2017; 144: 127-140.
    Résumé : The brassicaceous herb, Isatis tinctoria, is an ancient medicinal plant whose rosette leaf extracts have anti-inflammatory and anti-allergic activity. Brassicaceae are known to accumulate a variety of phenylpropanoids in their rosette leaves acting as antioxidants and a UV-B shield, and these compounds often have pharmacological potential. Nevertheless, knowledge about the phenylpropanoid content of I. tinctoria leaves remains limited to the characterization of a number of flavonoids. In this research, we profiled the methanol extracts of I. tinctoria fresh leaf extracts by liquid chromatography - mass spectrometry (LC-MS) and focused on the phenylpropanoid derivatives. We report the structural characterization of 99 compounds including 18 flavonoids, 21 mono- or oligolignols, 2 benzenoids, and a wide spectrum of 58 hydroxycinnamic acid esters. Besides the sinapate esters of malate, glucose and gentiobiose, which are typical of brassicaceous plants, these conjugates comprised a large variety of glucaric acid esters that have not previously been reported in plants. Feeding with (13)C6-glucaric acid showed that glucaric acid is an acyl acceptor of an as yet unknown acyltransferase activity in I. tinctoria rosette leaves. The large amount of hydroxycinnamic acid derivatives changes radically our view of the woad metabolite profile and potentially contributes to the pharmacological activity of I. tinctoria leaf extracts.
    Mots-clés : Brassicaceae, Glucaric acid, Glucosinolates, Hydroxycinnamic acid derivatives, Isatis tinctoria, LC-MS, Metabolite profiling, Phenylpropanoids.


  • Oliveira C, Fournier C, Descamps V, et al. Apolipoprotein(a) inhibits hepatitis C virus entry through interaction with infectious particles. Hepatology (Baltimore, Md.) 2017; 65: 1851-1864.
    Résumé : The development of different cell culture models has greatly contributed to increased understanding of the hepatitis C virus (HCV) life cycle. However, it is still challenging to grow HCV clinical isolates in cell culture. If overcome, this would open new perspectives to study HCV biology, including drug-resistant variants emerging with new antiviral therapies. In this study we hypothesized that this hurdle could be due to the presence of inhibitory factors in patient serum. Combining polyethylene glycol precipitation, iodixanol gradient, and size-exclusion chromatography, we obtained from HCV-seronegative sera a purified fraction enriched in inhibitory factors. Mass spectrometric analysis identified apolipoprotein(a) (apo[a]) as a potential inhibitor of HCV entry. Apo(a) consists of 10 kringle IV domains (KIVs), one kringle V domain, and an inactive protease domain. The 10 KIVs are present in a single copy with the exception of KIV type 2 (KIV2 ), which is encoded in a variable number of tandemly repeated copies, giving rise to numerous apo(a) size isoforms. In addition, apo(a) covalently links to the apolipoprotein B component of a low-density lipoprotein through a disulfide bridge to form lipoprotein(a). Using a recombinant virus derived from the JFH1 strain, we confirmed that plasma-derived and recombinant lipoprotein(a) as well as purified recombinant apo(a) variants were able to specifically inhibit HCV by interacting with infectious particles. Our results also suggest that small isoforms are less inhibitory than the large ones. Finally, we observed that the lipoprotein moiety of HCV lipoviroparticles was essential for inhibition, whereas functional lysine-binding sites in KIV7 , KIV8 , and KIV10 were not required. CONCLUSIONS: Our results identify apo(a) as an additional component of the lipid metabolism modulating HCV infection. (Hepatology 2017;65:1851-1864).
    Mots-clés : Blotting, Western, Cell Survival, Cells, Cultured, Chromatography, Liquid, Hepacivirus, Hepatitis C, Hepatocytes, Humans, Immunoprecipitation, Lipoprotein(a), Lysine, Protein Binding, Sensitivity and Specificity, Structure-Activity Relationship.


  • Opfergelt S, Cornélis J-T, Houben D, Givron C, Burton KW, Mattielli N. The influence of weathering and soil organic matter on Zn isotopes in soils. Chemical geology. 2017; 466: 140-148.
    Résumé : Zinc is an essential micronutrient that is ultimately released during mineral weathering. In soils, organic matter plays a key role in influencing Zn partitioning and therefore on Zn biogeochemical cycling. Soil organic matter is partitioned between carbon that is more readily available for decomposition by microorganisms, and more stable carbon transiently preserved from decomposition. The role of the stable pool of soil organic matter on Zn biogeochemical cycling remains poorly understood. The pool of stable carbon is controlled by combination with mineral constituents or is material that is intrinsically resistant to decomposition. The Zn stable isotopes are fractionated by interactions between Zn and soil mineral and organic constituents. This study reports the Zn isotope composition of five Icelandic soil profiles derived from the same parent basalt and characterized by contrasting degrees of weathering and organic matter content (δ66Zn = + 0.10 ± 0.05 to + 0.35 ± 0.02‰), the distribution of reactive mineral constituents available to form associations with soil organic matter, and the amount of stable organic carbon. Throughout these soils, the δ66Zn isotope variations are little influenced by mineral constituents, but rather by soil organic matter content. These data suggest that a combination of organic matter accumulation and Zn loss by leaching is required to explain the observed decrease in Zn concentration in soils and lighter soil δ66Zn with increasing organic carbon content. These results suggest that the presence of stable organic carbon in soils provides a pool of light Zn, attributed to the Zn isotope signature of organic matter partially preserved from decomposition. Crucially, this stable organic carbon pool may also contribute to the formation of the light Zn isotope sink reported in organic-rich marine sediments, a key output required to explain the oceanic mass balance of Zn isotopes.

  • Ors M-eva, Randoux B, Selim S, et al. Cultivar-dependent partial resistance and associated defence mechanisms in wheat against Zymoseptoria tritici - Ors - 2017 - Plant Pathology - Wiley Online Library. 2017.http://onlinelibrary.wiley.com/doi/10.1111/ppa.12760/full.
    Résumé : Septoria tritici blotch caused by the fungus Zymoseptoria tritici is one of the most devastating foliar diseases of wheat. Knowledge regarding mechanisms involved in resistance against this disease is required to breed durable resistances. This study compared the expression of defence and pathogenicity determinants in three cultivars in semicontrolled culture conditions. The most susceptible cultivar, Alixan, presented higher necrosis and pycnidia density levels than Altigo, the most resistant one. In Premio, a moderately resistant cultivar, necrosis developed as in Alixan, while pycnidia developed as in Altigo. In noninfectious conditions, genes coding for PR1 (pr1), glucanase (gluc) and allene oxide synthase (aos) were constitutively expressed at a higher level in both Altigo and Premio than in Alixan, while chitinase2 (chit2), phenylalanine ammonia-lyase (pal), peroxidase (pox2) and oxalate oxidase (oxo) were expressed at a higher level in Premio only. Except for aos, all genes were induced in Alixan during the first steps of the symptomless infection phase. Only pox2, oxo, gluc and pal genes in Altigo and pal, chs and lox genes in Premio were up-regulated at some time points. Basal cultivar-dependent resistance against Z. tritici could therefore be explained by various gene expression patterns rather than high expression levels of given genes. During the necrotrophic phase, Z. tritici cell wall-degrading enzyme activity levels were lower in Altigo and Premio than in Alixan, and were associated more with pycnidia than with necrosis. Similar tissue colonization occurred in the three cultivars, suggesting an inhibition of the switch to the necrotrophic lifestyle in Altigo


  • Ramsay A, Fliniaux O, Quéro A, et al. Kinetics of the incorporation of the main phenolic compounds into the lignan macromolecule during flaxseed development. Food Chemistry 2017; 217: 1-8.
    Résumé : The main flax lignan, secoisolariciresinol diglucoside, is stored in a macromolecule containing other ester-bound phenolic compounds. In this study, NMR and HPLC-UV analyses were performed on flaxseeds harvested at different developmental stages to identify and quantify the main phenolic compounds produced during seed development. Extraction was carried out with or without alkaline hydrolysis to determine if these molecules accumulate in the lignan macromolecule and/or in a free form. Monolignol glucosides accumulate in a free form up to 9.85mg/g dry matter at the early developmental stages. Hydroxycinnamic acid glucosides and flavonoid accumulate (up to 3.18 and 4.07mg/g dry matter, respectively) in the later developmental stages and are ester-bound in the lignan macromolecule. Secosiolariciresinol diglucoside accumulates (up to 28.65mg/g dry matter) in the later developmental stages in both forms, mainly ester-bound in the lignan macromolecule and slightly in a free form.
    Mots-clés : Butylene Glycols, Flavonoids, Flax, Flaxseed, Glucosides, HPLC-UV, Hydrolysis, Kinetics, Lignan macromolecule, Lignans, Macromolecular Substances, Magnetic Resonance Spectroscopy, NMR, Phenolics, Phenols, Seed development, Seeds.


  • Schneider A, Gommeaux M, Duclercq J, et al. Response of bacterial communities to Pb smelter pollution in contrasting soils. The Science of the Total Environment 2017; 605-606: 436-444.
    Résumé : Anthropogenic inputs of trace elements (TE) into soils constitute a major public and environmental health problem. Bioavailability of TE is strongly related to the soil physicochemical parameters and thus to the ecosystem type. In order to test whether soil parameters influence the response of the bacterial community to TE pollution, we collected soil samples across contrasting ecosystems (hardwood, coniferous and hydromorphic soils), which have been contaminated in TE and especially lead (Pb) over several decades due to nearby industrial smelting activities. Bacterial community composition was analysed using high throughput amplicon sequencing and compared to the soil physicochemical parameters. Multivariate analyses of the pedological and biological data revealed that the bacterial community composition was affected by ecosystem type in the first place. An influence of the contamination level was also evidenced within each ecosystem. Despite the important variability in bacterial community structure, we found that specific bacterial groups such as γ-Proteobacteria, Verrucomicrobia and Chlamydiae showed a consistent response to Pb content across contrasting ecosystems. Verrucomicrobia were less abundant at high contamination level whereas Chlamydiae and γ-Proteobacteria were more abundant. We conclude that such groups and ratio's thereof can be considered as relevant bioindicators of Pb contamination.
    Mots-clés : Bacterial diversity, Bioindicator, Chlamydiae, Pb bioavailability, Pb contamination, Verrucomicrobia.


  • Teixeira ARS, Willig G, Couvreur J, et al. From bench scale to kilolab production of renewable ferulic acid-based bisphenols: optimisation and evaluation of different purification approaches towards technical feasibility and process environmental sustainability. React. Chem. Eng. 2017; 2: 406-419.
    Résumé : In earlier authors work, a new class of non-toxic and renewable bisphenols able to substitute bisphenol A and exhibiting potent antioxidant and antiradical activities has been prepared from ferulic acid through a chemoenzymatic pathways at bench scale. Scaling-up a process is not always trivial and straightforward. Technical feasibility of synthesis and overall process yield must be assessed. All decisions should be justified regarding technical constraints and environmental sustainability. This work is focused on the kilolab production of bis-O-dihydroferuloyl 1,4-butanediol (BDF), one of these very promising renewable bisphenols. Recrystallization and organic diananofiltration in a single stage (SSD) and two stages (TSD) were compared taking into account the previous considerations. As result, the synthesis and purification of BDF by recrystallization were successfully scaled-up at kilolab scale, being obtained a significant improvement in the overall yield (from 63% at labscale to 84% at kilolab scale) for a purity grade of 95%. To assess the organic diananofiltration as an alternative purification method, a set of 6 commercial organic solvent resistant membranes were evaluated. Starting from a solution (1 g/L) containing 80%(w/w) of BDF and 20% (w/w) of an excess reagent (ethyl dihydroferulate, EtDFe), GMT-oNF1 membrane showed to be able to discriminate them. A two-stage membrane diafiltration (TSD) in cascade was proposed, being observed a drastic increase in the product yield (from 77% in a single stage to 95%) without compromising its final purity (95%). Since solvent recycling has a significant impact on the process sustainability, a nanofiltration step for solvent recovery was assessed, . 90% of the solvent was recovered with a level of impurities lower than 1%. Recrystallization and all filtration-based processes were compared in terms of green metrics such as mass and solvent intensity and energy consumption. Results showed that only the integration of solvent recycling in filtration-based processes and the use of a concentrated starting solution (150 g/L instead of 1 g/L) may lead to similar magnitude values observed for recrystallization. Thus, even being a less energetic intensive process (4-fold), the TSD is still a solvent intensive process (3-fold), which is inevitably reflected in a higher environmental footprint (evaluated by LCA).
    Mots-clés : Acid, Bisphenols, Ferulic, Projet SFR.


  • Teixeira ARS, Willig G, Couvreur J, et al. From bench scale to kilolab production of renewable ferulic acid-based bisphenols: optimisation and evaluation of different purification approaches towards technical feasibility and process environmental sustainability. Reaction Chemistry & Engineering 2017; 2: 406-419.
    Résumé : In an earlier work by the authors, a new class of non-toxic and renewable bisphenols able to substitute bisphenol A and exhibiting potent antioxidant and antiradical activities has been prepared from ferulic acid through chemo-enzymatic pathways at bench scale. Scaling-up a process is not always trivial and straightforward. Technical feasibility of the synthesis and overall process yield must be assessed. All decisions should be justified regarding technical constraints and environmental sustainability. This work is focused on the kilolab production of bis-O-dihydroferuloyl 1,4-butanediol (BDF), one of the very promising renewable bisphenols. Recrystallization and organic diananofiltration in a single stage (SSD) and two stages (TSD) were compared taking into account the previous considerations. As a result, the synthesis and purification of BDF by recrystallization were successfully scaled-up at the kilolab scale, with a significant improvement in the overall yield obtained (from 63% at the labscale to 84% at the kilolab scale) for a purity grade of 95%. To assess organic diananofiltration as an alternative purification method, a set of 6 commercial organic solvent resistant membranes was evaluated. Starting from a solution (1 g L−1) containing 80% (w/w) of BDF and 20% (w/w) of an excess reagent (ethyl dihydroferulate, EtDFe), GMT-oNF1 membrane showed the ability to discriminate them. A two-stage membrane diafiltration (TSD) in cascade was proposed, with a drastic increase in the product yield observed (from 77% in a single stage to 95%) without compromising its final purity (95%). Since solvent recycling has a significant impact on the process sustainability, a nanofiltration step for solvent recovery was assessed. 90% of the solvent was recovered with a level of impurities lower than 1%. Recrystallization and all filtration-based processes were compared in terms of green metrics such as mass and solvent intensity and energy consumption. Results showed that only the integration of solvent recycling in filtration-based processes and the use of a concentrated starting solution (150 g L−1 instead of 1 g L−1) may lead to similar magnitude values observed for recrystallization. Thus, even being a less energetically intensive process (4-fold), the TSD is still a solvent intensive process (3-fold), which is inevitably reflected in a higher environmental footprint (evaluated by LCA).

  • Zinck P, Beaulieu R, Bonnet F, et al. Chimie de la biomasse - L'Actualité Chimique. 2017.https://www.lactualitechimique.org/Capteurs-et-suivi-sur-site-de-la-pollution-des-eaux.
    Résumé : Cet article présente un tour d’horizon de quelques-unes des thématiques de recherche développées en région Hauts-de-France dans les domaines de la chimie de la biomasse
    Mots-clés : biomasse, chimie.
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