0000000000764151
AUTHOR
Laurent Brachais
Efficient microwave-assisted synthesis of glycerol monodecanoate
International audience; Solvent-free microwave-assisted synthesis was carried out to prepare 2,3-dihydroxypropyl decanoate, by esterification of decanoic acid in the presence of two distinct glycerol derivatives, glycidol, and glycerol carbonate, respectively. The process described is based on microwaves heating source with electrical power in the range of 200–400 W, involving stoichiometric proportions of decanoic acid and glycerol derivatives, and using catalytic amounts of TBAI used as organocatalyst. Conversion and selectivity rates of esterification reactions were monitored by 1H and 13C{1H} NMR spectroscopy. The predominantly formed ester, 2,3-dihydroxypropyl decanoate was fully chara…
Synthesis and degradation of poly (2-hydroxyethyl methacrylate)-graft-poly (ε-caprolactone) copolymers
Abstract Poly (e-caprolactone) macromonomers carrying a methacryloyl end groups were synthesized using different lanthanide derivatives as catalysts, and characterized by SEC and 1 H NMR. Hydrophilic–hydrophobic copolymers from macromonomers and 2-hydroxyethyl methacrylate (HEMA) were obtained by solution free radical polymerization. Depending on the feed ratio of the two components, different copolymer structures were obtained. The expected graft structure of the copolymers was confirmed by 1 H NMR. Thermal properties of the copolymers were determined by DSC and TGA. Hydrolytic and enzymatic degradations of the materials were performed. Poly (2-hydroxyethyl methacrylate)- graft -poly (e-ca…
NMR T1-Relaxation Measurements on Paramagnetic Organolanthanides: An Alternative Tool for Structure Determination in Solution
1H NMR investigations were conducted on four paramagnetic organolanthanides, all bearing the tetraisopropylcyclopentadienyl ligand Cp4i (HC5iPr4) in order to verify whether or not interactions observed in the solid state are maintained in solution. In some cases variable-temperature experiments were necessary to enhance the resolution and determine the best conditions for the study. The 1D NMR spectrum could be interpreted in every case. Complementary 2D COSY experiments allowed the full attribution of the signals. T1 (1H) relaxation values were determined for all the paramagnetic complexes at the most suitable temperature, and compared with those of the diamagnetic KCp4i. The same tendency…
Chain-extending of Hydroxytelechelic Polybutadiene: Synthesis and Characterization
Extension of hydroxytelechelic polybutadiene oligomers ( 3200 g/mol) is performed in mild conditions, in order to avoid backbone modifications, using succinic anhydride or methylenedicyclohexyl diisocyanate. The two routes present significative extension of the initial oligomers. Extension through the anhydride route, in the presence of DCC and DMAP, leads to new hydroxytelechelic oligomers ( 8000 g/mol). Extension through the diisocyanate route, catalyzed by DBTL at 65°C leads to hydroxytelechelic oligomers of higher average molecular weight ( 20000 g/mol). New materials are characterized by FTIR/1H-NMR and changes in their Tg according to , are discussed. The influence of reaction time on…
Synthesis of polycaprolactone by microwave irradiation ? an interesting route to synthesize this polymer via green chemistry
Poly(e-caprolactone) has become an important biocompatible and biodegradable polymer. Indeed, due to its multiple biomedical applications, the synthesis of polycaprolactone has received increased attention in the past few decades. Moreover, microwave irradiation is a very clean modern technique widely used for green chemistry. Here, several polymers were synthesized by microwave irradiation, without any solvent, using nontoxic, biologically acceptable lanthanide halides as initiators. Reaction times varied between 2 and 90 min. The molecular weights of the obtained polymer products were between 3,000 and 16,000 g/mol. After polymerization, the polycaprolactone polymers were functionalized b…
Adsorption equilibria of water vapor on cork.
International audience; We report here for the first time a complete thermodynamic study of water vapor adsorption on crude cork powder and plate. Adsorption−desorption isotherms were accurately measured by thermogravimetry at 283, 298, and 313 K in a large range of relative pressure. Adsorption enthalpies were determined by calorimetry as a function of loading. Adsorption−desorption isotherms exhibit a hysteresis due to the swelling of the material. The influence of the presence of lenticels on the adsorption properties of cork is found to be negligible. A detailed analysis and interpretation of adsorption data allow proposal of an adsorption mechanism in two steps. (i) First, water adsorb…
Molécules aromatisantes et sapides
National audience
Characterizations of Thermoplastic Block Elastomers Based on Polybutadiene and ε -Caprolactone
A broad series of tri- and multiblock copolymers based on linear and branched oligomers of polybutadiene as central blocks and polycaprolactone (PCL) as block extremities are characterized by SEC, DSC, DMA, Dynamical Rheology and DRX. DSC analyses reveal phase separation between the two amorphous PB and PCL phases. By thermal analysis, the glass transition temperature of PCL is only detected for materials containing at least 80% w/w of PCL. This is attributed to the small length of the polyester blocks for copolymers containing less than 80% w/w of PCL. The increase of fusion heat with increasing PCL content in the copolymers is correlated to the greater ability of PCL chains to rearrange a…
Wine Oxidation and the Role of Cork
The present review aims to show the state of the art of oxidation mechanisms occurring especially in white wines by taking into account knowledge from different fields in relation to the subject. It is therefore divided into three main parts. First, the mechanisms of oxidation relevant to white wine are discussed in the light of recent scientific literature. Next, the phenomenon of oxygen solubility in wine during the winemaking process, and in particular during bottling is stated theoretically as well as practically. Finally, the aspect of wine conservation after bottling is examined with respect to mass transfers which may occur through the closure, with a special emphasis on cork. Curren…