Responsable des stages Département Génie Chimique Génie des Procédés, IUT de Saint-Jérôme
Activités
Développement de procédés propres utilisant le CO2 supercritique et plus particulièrement l’extraction
Valorisation d’huiles microalgales extraites par CO2 supercritique
Fractionnement et mise en forme de nanoparticules (micronisation et encapsulation)
Publications scientifiques au M2P2
2024
Aymeric Fabien, Guillaume Lefebvre, Elisabeth Badens, Brice Calvignac, Damien Chaudanson, et al.. Contact angle of ethanol, water, and their mixtures on stainless steel surfaces in dense carbon dioxide. Journal of Colloid and Interface Science, 2024, 655, pp.535-545. ⟨10.1016/j.jcis.2023.10.163⟩. ⟨hal-04316090⟩ Plus de détails...
Hypothesis Contact angle can be a key parameter in chemical engineering. However, the development and the optimization of numerous processes using supercritical CO2, considered as environmentally friendly, requires new measurements under dense CO2 atmosphere. Besides, the influence of the roughness or the wetting regime on the contact angle is known at ambient conditions but remains to be discussed for systems under high pressure. Experimental Contact angle measurements of ethanol, water, and their mixtures, with ethanol mass fractions ranging from 0.25 to 0.75, on two stainless steels in saturated CO2 at pressures ranging from 0.1 MPa to 15.1 MPa, and at 313 K and 333 K were carried out in a set-up improving mass transfer between the studied liquid and the continuous fluid phase. Stainless steel surfaces have been characterized by atomic force and scanning electron microscopies allowing the application of the Wenzel equation. Findings Ethanol wetted totally both stainless steels while contact angles of all other liquids were increased by the rise of pressure, with contact angles up to 128 ° for water at 15.1 MPa. Trapped bubbles were observed at the solid/liquid interface and the bubble formation is discussed. Furthermore, the potential influence of bubble presence on the wetting regime is prospected through the question: could the pressure rise modify the wetting regime?
Aymeric Fabien, Guillaume Lefebvre, Elisabeth Badens, Brice Calvignac, Damien Chaudanson, et al.. Contact angle of ethanol, water, and their mixtures on stainless steel surfaces in dense carbon dioxide. Journal of Colloid and Interface Science, 2024, 655, pp.535-545. ⟨10.1016/j.jcis.2023.10.163⟩. ⟨hal-04316090⟩
Vénicia Numa, Christelle Crampon, Arnaud Bellon, Adil Mouahid, Elisabeth Badens. Valorization of food side streams by supercritical fluid extraction of compounds of interest from apple pomace. Journal of Supercritical Fluids, 2023, 202, pp.106056. ⟨10.1016/j.supflu.2023.106056⟩. ⟨hal-04294235⟩ Plus de détails...
Supercritical CO2 (scCO2) extraction, a green technology still little applied to side streams, has been used to explore the potential recovery of beneficial compounds from apple pomace, a food industry byproduct. The study examines the potential of scCO2 extraction on freeze-dried and airflow dried apple pomace, using laboratory-scale equipment with varying pressures (200–400 bar), temperatures (35–55 °C) with a fixed CO2 flow rate. Extracts were analyzed through LC-MS and GC-MS, while antioxidant capacity was assessed using the ABTS assay. The results were compared to those from Soxhlet n-hexane extraction. Optimal conditions of 300 bar and 55 °C with freeze-dried apple pomace yielded the highest mass loss. The main compounds identified included glyceryl dilinoleate, linoleic acid, and diacyl glycerol, with significant ursolic acid content. A preliminary higher scale feasibility test under optimal conditions demonstrated promising, duplicable outcomes, supporting prior claim that apple pomace contains valuable ingredients that can be reused in various industrial sectors.
Vénicia Numa, Christelle Crampon, Arnaud Bellon, Adil Mouahid, Elisabeth Badens. Valorization of food side streams by supercritical fluid extraction of compounds of interest from apple pomace. Journal of Supercritical Fluids, 2023, 202, pp.106056. ⟨10.1016/j.supflu.2023.106056⟩. ⟨hal-04294235⟩
Adil Mouahid, Magalie Claeys-Bruno, Isabelle Bombarda, Sandrine Amat, Andrea Ciavarella, et al.. Valorization of handmade argan press cake by supercritical CO2 extraction. Food and Bioproducts Processing, 2023, 137, pp.168-176. ⟨10.1016/j.fbp.2022.11.011⟩. ⟨hal-04063823⟩ Plus de détails...
The capability of supercritical CO2 to extract edible oil from handmade Argan press cake was investigated. The aim is to enable Moroccan cooperatives to improve their economic situation by valuing the handmade argan press cake, which is nowadays considered as a waste, applying a clean extraction process. Extraction experiments were conducted at 300 and 400 bar, 333 K and 0.14 kg/h on dried biomass. The fatty acids and tocopherols compositions of the extracted oil were found similar to previous studies and correspond to a commercial edible oil. The air flow dried biomass exhibits a higher extraction yield compared to the freeze-dried biomass. A pressure of 300 bar seems to be suffcient to allow the extraction of oil with a satisfactory extraction kinetic.
Adil Mouahid, Magalie Claeys-Bruno, Isabelle Bombarda, Sandrine Amat, Andrea Ciavarella, et al.. Valorization of handmade argan press cake by supercritical CO2 extraction. Food and Bioproducts Processing, 2023, 137, pp.168-176. ⟨10.1016/j.fbp.2022.11.011⟩. ⟨hal-04063823⟩
Adil Mouahid, Magalie Claeys-Bruno, Isabelle Bombarda, Sandrine Amat, Andrea Ciavarella, et al.. Valorization of handmade argan press cake by supercritical CO2 extraction. Food and Bioproducts Processing, 2023, 137, pp.168-176. ⟨10.1016/j.fbp.2022.11.011⟩. ⟨hal-03992094⟩ Plus de détails...
The capability of supercritical CO2 to extract edible oil from handmade Argan press cake was investigated. The aim is to enable Moroccan cooperatives to improve their economic situation by valuing the handmade argan press cake, which is nowadays considered as a waste, applying a clean extraction process. Extraction experiments were conducted at 300 and 400 bar, 333 K and 0.14 kg/h on dried biomass. The fatty acids and tocopherols compositions of the extracted oil were found similar to previous studies and correspond to a commercial edible oil. The air flow dried biomass exhibits a higher extraction yield compared to the freeze-dried biomass. A pressure of 300 bar seems to be suffcient to allow the extraction of oil with a satisfactory extraction kinetic.
Adil Mouahid, Magalie Claeys-Bruno, Isabelle Bombarda, Sandrine Amat, Andrea Ciavarella, et al.. Valorization of handmade argan press cake by supercritical CO2 extraction. Food and Bioproducts Processing, 2023, 137, pp.168-176. ⟨10.1016/j.fbp.2022.11.011⟩. ⟨hal-03992094⟩
Victorine Warambourg, Adil Mouahid, Christelle Crampon, Anne Galinier, Magalie Claeys-Bruno, et al.. Supercritical CO2 sterilization under low temperature and pressure conditions. Journal of Supercritical Fluids, 2023, 203, pp.106084. ⟨10.1016/j.supflu.2023.106084⟩. ⟨hal-04233306⟩ Plus de détails...
Sterilization using supercritical carbon dioxide has been proven to be efficient for decades now. The aim of this work was to implement a process of sterilization adapted to thermosensitive polymeric materials and highlight the lowest conditions of pressure and temperature which would enable a bacterial reduction higher than 6-log. Inactivation experiments were performed on spores of Bacillus subtilis over a pressure range lying from 60 to 200 bar, and a temperature varying from 35° to 60°C, with and without additive. Preliminary experiments allowed us to determine a restricted experimental domain used for the design of the experiments, investigating the influence of pressure, temperature, process duration, and additive content on bacterial reduction. It was shown that sterilization conducted at 110 bar, 40 °C, for 20 min with 200 ppm of H2O2, leading to a bacterial reduction of 8.73-log, may be considered as optimal for IMD sterilization.
Victorine Warambourg, Adil Mouahid, Christelle Crampon, Anne Galinier, Magalie Claeys-Bruno, et al.. Supercritical CO2 sterilization under low temperature and pressure conditions. Journal of Supercritical Fluids, 2023, 203, pp.106084. ⟨10.1016/j.supflu.2023.106084⟩. ⟨hal-04233306⟩
Aymeric Fabien, Guillaume Lefebvre, Brice CALVIGNAC, Pierre Legout, Elisabeth Badens, et al.. Interfacial tension of ethanol, water, and their mixtures in high pressure carbon dioxide: Measurements and modeling. Journal of Colloid and Interface Science, 2022, 613, pp.847-856. ⟨10.1016/j.jcis.2022.01.058⟩. ⟨hal-04124118⟩ Plus de détails...
Hypothesis. It is particularly noteworthy to study interfacial tension behavior under pressurized carbon dioxide for supercritical processes such as crystallization or fractionation. For the latter, a liquid phase and a supercritical phase are in contact, and interfacial properties influence mass transfer phenomena and hydrodynamics. Ethanol-water mixture is a good theoretical study case also involved in a wide range of applications. Experimental: Interfacial tensions of ethanol, water and three mixtures, with an ethanol mass fraction from 0.25 to 0.75, under pressurized CO2 were measured for pressures ranging from 0.1 MPa to 15.1 MPa at 313.15 K and 333.15 K. A specific experimental set-up was used for CO2 phase saturation. Findings: This work brings interfacial tension data of five different solutions including water and ethanol in contact with CO2. Effects of pressure, temperature, carbon dioxide density and ethanol mass fraction are discussed regarding the literature. Significant discrepancies are found with previous literature data for ethanol-water mixtures. The "two-step" decrease observed when pressure or density increase is also discussed regarding both the concept of Widom line, and the polar and dispersive contributions of the surface tension of a component. For the first time, fair accurate interfacial tension modeling involving these contributions is addressed. (C) 2022 Elsevier Inc. All rights reserved.
Aymeric Fabien, Guillaume Lefebvre, Brice CALVIGNAC, Pierre Legout, Elisabeth Badens, et al.. Interfacial tension of ethanol, water, and their mixtures in high pressure carbon dioxide: Measurements and modeling. Journal of Colloid and Interface Science, 2022, 613, pp.847-856. ⟨10.1016/j.jcis.2022.01.058⟩. ⟨hal-04124118⟩
Aymeric Fabien, Guillaume Lefebvre, Brice Calvignac, Pierre Legout, Elisabeth Badens, et al.. Interfacial tension of ethanol, water, and their mixtures in high pressure carbon dioxide: measurements and modeling. Journal of Colloid and Interface Science, 2022, 613, pp.847-56. ⟨10.1016/j.jcis.2022.01.058⟩. ⟨hal-03531186⟩ Plus de détails...
Hypothesis: It is particularly noteworthy to study interfacial tension behavior under pressurized carbon dioxide for supercritical processes such as crystallization or fractionation. For the latter, a liquid phase and a supercritical phase are in contact, and interfacial properties influence mass transfer phenomena and hydrodynamics. Ethanol-water mixture is a good theoretical study case also involved in a wide range of applications. Experimental: Interfacial tensions of ethanol, water and three mixtures, with an ethanol mass fraction from 0.25 to 0.75, under pressurized CO 2 were measured for pressures ranging from 0.1 MPa to 15.1 MPa at 313.15 K and 333.15 K. A specific experimental setup was used for CO 2 phase saturation. Findings: This work brings interfacial tension data of five different solutions including water and ethanol in contact with CO 2. Effects of pressure, temperature, carbon dioxide density and ethanol mass fraction are discussed regarding the literature. Significant discrepancies are found with previous literature data for ethanol-water mixtures. The "two-step" decrease observed when pressure or density increase is also discussed regarding both the concept of Widom line, and the polar and dispersive contributions of the surface tension of a component. For the first time, fair accurate interfacial tension modeling involving these contributions is addressed.
Aymeric Fabien, Guillaume Lefebvre, Brice Calvignac, Pierre Legout, Elisabeth Badens, et al.. Interfacial tension of ethanol, water, and their mixtures in high pressure carbon dioxide: measurements and modeling. Journal of Colloid and Interface Science, 2022, 613, pp.847-56. ⟨10.1016/j.jcis.2022.01.058⟩. ⟨hal-03531186⟩
Adil Mouahid, Isabelle Bombarda, Magalie Claeys-Bruno, Sandrine Amat, Emmanuelle Myotte, et al.. Supercritical CO2 extraction of Moroccan argan (Argania spinosa L.) oil: Extraction kinetics and solubility determination. Journal of CO2 Utilization, Elsevier, 2021, 46, pp.101458. ⟨10.1016/j.jcou.2021.101458⟩. ⟨hal-03142714⟩ Plus de détails...
Adil Mouahid, Isabelle Bombarda, Magalie Claeys-Bruno, Sandrine Amat, Emmanuelle Myotte, et al.. Supercritical CO2 extraction of Moroccan argan (Argania spinosa L.) oil: Extraction kinetics and solubility determination. Journal of CO2 Utilization, Elsevier, 2021, 46, pp.101458. ⟨10.1016/j.jcou.2021.101458⟩. ⟨hal-03142714⟩
Adil Mouahid, Isabelle Bombarda, Magalie Claeys-Bruno, Sandrine Amat, Emmanuelle Myotte, et al.. Supercritical CO2 extraction of Moroccan argan (Argania spinosa L.) oil: Extraction kinetics and solubility determination. Journal of CO2 Utilization, 2021, 46, pp.101458. ⟨10.1016/j.jcou.2021.101458⟩. ⟨hal-03142714⟩ Plus de détails...
Experimental and modelling investigations of supercritical CO 2 extraction of oil from Argania spinosa L. kernels were conducted at pressure range from 200 to 400 bar, temperature range of 313-333 K at a CO 2 flow rate of 0.14 kg/h. Regardless of the pressure and the temperature, the highest achievable yield was estimated at 0.63 kg oil / kg biomass. The extraction kinetics were modeled with Sovová's broken and intact cells model. The extraction of type B was found to be the most suited extraction type. Argan oil solubility in supercritical CO 2 was determined and modelled with the Chrastil equation. A retrograde solubility behaviour was observed at 200 bar and the faster extraction kinetics were found at 400 bar and 333 K. The total tocopherols concentration was found between 389.7 and 1688.6 mg/kg extract. Experiments were performed on unroasted and roasted kernels.
Adil Mouahid, Isabelle Bombarda, Magalie Claeys-Bruno, Sandrine Amat, Emmanuelle Myotte, et al.. Supercritical CO2 extraction of Moroccan argan (Argania spinosa L.) oil: Extraction kinetics and solubility determination. Journal of CO2 Utilization, 2021, 46, pp.101458. ⟨10.1016/j.jcou.2021.101458⟩. ⟨hal-03142714⟩
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-02960133⟩ Plus de détails...
Supercritical CO2 extraction experiments were conducted to investigate the effects of pretreatment and process parameters on neutral lipids, chlorophylls and carotenoids recovery on two species of Nannochloropsis. For Nannochloropsis maritima, a factorial experimental design was performed (P: [100-300] bar, T: [313-333] K). The highest extraction yields were obtained at the highest pressures and temperatures. Two drying modes, ring drying and air flow drying, were compared. Although total extraction yield and extraction kinetics were observed to be greater using air flow dried microalgae, extracts from this drying method resulted in partial degradation of glycerides in free fatty acids. Ring dried extracts maintained the same neutral lipid composition as the initial biomass. Based on these results, ring dried Nannochloropsis salina was extracted using supercritical CO2 at 333 K and both 300-400 bar. Extraction curves were modelled using the Sovova's mathematical model.
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-02960133⟩
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Sclareol purification using the supercritical fractionation process: A modeling case study. Journal of Supercritical Fluids, 2020, 159, pp.104754. ⟨10.1016/j.supflu.2020.104754⟩. ⟨hal-02892487⟩ Plus de détails...
The aim of this study was to model experimental results obtained for the supercritical CO2 fractionation of a liquid mixture containing 24% of sclareol in order to recover a raffinate with increased sclareol content. First, supercritical CO2 fractionation experiments were carried out at pressures (10-12) MPa, and temperatures (313-338) K. Secondly, the modeling of the raffinate and extract compositions for 12 selected compounds including sclareol was performed using the group method. The modeling was carried out at a temperature of 323 K and pressures of (10-11) MPa, and at a temperature of 338 K and a pressure of 12 MPa. The calculation of the raffinate and extract compositions required the adjustment of the number of theoretical stages and of the distribution coefficients for the selected compounds. Experimental raffinate and extract compositions were represented by the model with a relative error of about 15%.
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Sclareol purification using the supercritical fractionation process: A modeling case study. Journal of Supercritical Fluids, 2020, 159, pp.104754. ⟨10.1016/j.supflu.2020.104754⟩. ⟨hal-02892487⟩
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Sclareol purification using the supercritical fractionation process: A modeling case study. Journal of Supercritical Fluids, Elsevier, 2020, 159, pp.104754. ⟨10.1016/j.supflu.2020.104754⟩. ⟨hal-02892487⟩ Plus de détails...
The aim of this study was to model experimental results obtained for the supercritical CO2 fractionation of a liquid mixture containing 24% of sclareol in order to recover a raffinate with increased sclareol content. First, supercritical CO2 fractionation experiments were carried out at pressures (10-12) MPa, and temperatures (313-338) K. Secondly, the modeling of the raffinate and extract compositions for 12 selected compounds including sclareol was performed using the group method. The modeling was carried out at a temperature of 323 K and pressures of (10-11) MPa, and at a temperature of 338 K and a pressure of 12 MPa. The calculation of the raffinate and extract compositions required the adjustment of the number of theoretical stages and of the distribution coefficients for the selected compounds. Experimental raffinate and extract compositions were represented by the model with a relative error of about 15%.
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Sclareol purification using the supercritical fractionation process: A modeling case study. Journal of Supercritical Fluids, Elsevier, 2020, 159, pp.104754. ⟨10.1016/j.supflu.2020.104754⟩. ⟨hal-02892487⟩
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-02960133⟩ Plus de détails...
Supercritical CO2 extraction experiments were conducted to investigate the effects of pretreatment and process parameters on neutral lipids, chlorophylls and carotenoids recovery on two species of Nannochloropsis. For Nannochloropsis maritima, a factorial experimental design was performed (P: [100-300] bar, T: [313-333] K). The highest extraction yields were obtained at the highest pressures and temperatures. Two drying modes, ring drying and air flow drying, were compared. Although total extraction yield and extraction kinetics were observed to be greater using air flow dried microalgae, extracts from this drying method resulted in partial degradation of glycerides in free fatty acids. Ring dried extracts maintained the same neutral lipid composition as the initial biomass. Based on these results, ring dried Nannochloropsis salina was extracted using supercritical CO2 at 333 K and both 300-400 bar. Extraction curves were modelled using the Sovova's mathematical model.
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-02960133⟩
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-03232116⟩ Plus de détails...
Supercritical CO2 extraction experiments were conducted to investigate the effects of pretreatment and process parameters on neutral lipids, chlorophylls and carotenoids recovery on two species of Nannochloropsis. For Nannochloropsis maritima, a factorial experimental design was performed (P: [100-300] bar, T: [313-333] K). The highest extraction yields were obtained at the highest pressures and temperatures. Two drying modes, ring drying and air flow drying, were compared. Although total extraction yield and extraction kinetics were observed to be greater using air flow dried microalgae, extracts from this drying method resulted in partial degradation of glycerides in free fatty acids. Ring dried extracts maintained the same neutral lipid composition as the initial biomass. Based on these results, ring dried Nannochloropsis salina was extracted using supercritical CO2 at 333 K and both 300-400 bar. Extraction curves were modelled using the Sovova's mathematical model.
Adil Mouahid, Kanitta Seengeon, Mathieu Martino, Christelle Crampon, Avery Kramer, et al.. Selective extraction of neutral lipids and pigments from Nannochloropsis salina and Nannochloropsis maritima using supercritical CO2 extraction: Effects of process parameters and pre-treatment. Journal of Supercritical Fluids, 2020, 165, pp.104934. ⟨10.1016/j.supflu.2020.104934⟩. ⟨hal-03232116⟩
Alessia Di Capua, Renata Adami, Emanuela Cosenza, Vincent Jalaber, Christelle Crampon, et al.. β-Carotene/PVP microspheres produced by Supercritical Assisted Atomization. Powder Technology, 2019, 346, pp.228-236. ⟨10.1016/j.powtec.2019.01.069⟩. ⟨hal-02176986⟩ Plus de détails...
Beta-carotene (BC) is one of the best known and used bioactive compounds with antioxidant activity. In this work coprecipitation of BC with polyvinylpyrrolidone (PVP) by Supercritical Assisted Atomization (SAA) has been studied. to enhance BC bioavailability and to provide its protection against oxidation. Two solvents have been used: ethanol and a mixture acetone/ethanol 70/30 (v/v). In both cases SAA produced spherical and amorphous microspheres with d(50) ranging between 0.42 and 0.84 mu m using ethanol, and 0.28 and 0.48 mu m using the solvent mixture. UV-vis analyses revealed a BC content up to 94% and high scavenging activities confirm that PVP is able to protect it from degradation. BC dissolution rate in a phosphate buffered saline solution (PBS) was up to 22 times faster than that of physical mixture. The major difference between coprecipitates was in their dissolution rate: it depended also on the kind solvent used, indicating a possible different internal particles organization during droplet drying.
Alessia Di Capua, Renata Adami, Emanuela Cosenza, Vincent Jalaber, Christelle Crampon, et al.. β-Carotene/PVP microspheres produced by Supercritical Assisted Atomization. Powder Technology, 2019, 346, pp.228-236. ⟨10.1016/j.powtec.2019.01.069⟩. ⟨hal-02176986⟩
I. García-Casas, Christelle Crampon, A. Montes, C. Pereyra, E.J. Martínez de La Ossa, et al.. Supercritical CO2 impregnation of silica microparticles with quercetin. Journal of Supercritical Fluids, 2019, 143, pp.157-161. ⟨hal-01946903⟩ Plus de détails...
Supercritical carbon dioxide has been used to develop two methods for the impregnation of porous silica beads with a natural antioxidant, quercetin. These methods involved batch and semi-continuous supercritical impregnations. The first experiments performed in batch mode helped to understand the influence of pressure, temperature, duration, and the presence of a co-solvent on the impregnation efficiency. A co-solvent was added due to the low solubility of quercetin in supercritical CO2 under the operating conditions studied. In the range of temperatures and pressures studied, the best operating conditions, i.e., those that led to the highest quantity of quercetin impregnated (300 mu g of quercetin per g of silica), were 10 MPa and 323 K with ethanol as co-solvent for 2 h. These operating conditions, highlighted through the batch mode experiments, were subsequently applied to the semi-continuous process. This approach provided an impregnation ratio of 240 mu g of quercetin per g of silica.
I. García-Casas, Christelle Crampon, A. Montes, C. Pereyra, E.J. Martínez de La Ossa, et al.. Supercritical CO2 impregnation of silica microparticles with quercetin. Journal of Supercritical Fluids, 2019, 143, pp.157-161. ⟨hal-01946903⟩
Adil Mouahid, Halima Bouanga, Christelle Crampon, Elisabeth Badens. Supercritical CO2 extraction of oil from Jatropha curcas: An experimental and modelling study. Journal of Supercritical Fluids, 2018, 141, pp.2-11. ⟨10.1016/j.supflu.2017.11.014⟩. ⟨hal-02114700⟩ Plus de détails...
Experimental and modelling investigations of supercritical CO 2 extraction of oil from Jatropha curcas were conducted at a pressure range of 20-40 MPa and a temperature range of 313-333 K at a CO 2 flow rate of 0.4 kg/ h. The extraction yield was estimated to be about 0.6 kg oil /kg biomass for all experiments. The model of broken and intact cells published by Sovová was applied. It was found that the extraction of type B was the most suited extraction type to apply as the experimental extraction curves exhibit three parts. Whatever the pressure and the temperature applied, the asymptotic yield at infinite time was found to be the same. At 20 MPa, increasing the temperature from 313 to 323 K enhances the extraction kinetics. A retrograde solubility zone was found at 30 and 40 MPa. The Jatropha curcas oil solubility in SC-CO 2 was determined and the data were modelled with the Chrastil equation.
Adil Mouahid, Halima Bouanga, Christelle Crampon, Elisabeth Badens. Supercritical CO2 extraction of oil from Jatropha curcas: An experimental and modelling study. Journal of Supercritical Fluids, 2018, 141, pp.2-11. ⟨10.1016/j.supflu.2017.11.014⟩. ⟨hal-02114700⟩
Myriam Slama, Cédric Leblond, Pierre Sagaut. A Kriging-based elliptic extended anisotropic model for the turbulent boundary layer wall pressure spectrum. Journal of Fluid Mechanics, 2018, 840, pp.25 - 55. ⟨10.1017/jfm.2017.810⟩. ⟨hal-02115966⟩ Plus de détails...
The present study addresses the computation of the wall pressure spectrum for a turbulent boundary layer flow without pressure gradient, at high Reynolds numbers, using a new model, the Kriging-based elliptic extended anisotropic model (KEEAM). A space–time solution to the Poisson equation for the wall pressure fluctuations is used. Both the turbulence–turbulence and turbulence–mean shear interactions are taken into account. It involves the mean velocity field and space–time velocity correlations which are modelled using Reynolds stresses and velocity correlation coefficients. We propose a new model, referred to as the extended anisotropic model, to evaluate the latter in all regions of the boundary layer. This model is an extension of the simplified anisotropic model of Gavin (PhD thesis, 2002, The Pennsylvania State University, University Park, PA) which was developed for the outer part of the boundary layer. It relies on a new expression for the spatial velocity correlation function and new parameters calibrated using the direct numerical simulation results of Sillero et al. (Phys. Fluids, vol. 26, 2014, 105109). Spatial correlation coefficients are related to space–time coefficients with the elliptic model of He & Zhang (Phys. Rev. E, vol. 73, 2006, 055303). The turbulent quantities necessary for the pressure computation are obtained by Reynolds-averaged Navier–Stokes solutions with a Reynolds stress turbulence model. Then, the pressure correlations are evaluated with a self-adaptive sampling strategy based on Kriging in order to reduce the computation time. The frequency and wavenumber–frequency wall pressure spectra obtained with the KEEAM agree well with empirical models developed for turbulent boundary layer flows without pressure gradient.
Myriam Slama, Cédric Leblond, Pierre Sagaut. A Kriging-based elliptic extended anisotropic model for the turbulent boundary layer wall pressure spectrum. Journal of Fluid Mechanics, 2018, 840, pp.25 - 55. ⟨10.1017/jfm.2017.810⟩. ⟨hal-02115966⟩
Elisabeth Badens, Yasmine Masmoudi, Adil Mouahid, Christelle Crampon. Current situation and perspectives in drug formulation by using supercritical fluid technology. Journal of Supercritical Fluids, 2018, 134, pp.274-283. ⟨10.1016/j.supflu.2017.12.038⟩. ⟨hal-02111546⟩ Plus de détails...
Supercritical fluid (SCF) technology has been applied to drug product development over the last thirty years and drug particle generation using SCFs appears to be an efficient way to carry out drug formulation which will form end-products meeting targeted specifications. This article presents an overview of drug particle design using SCFs from a rather different perspective than usual, more focused on chemical and process engineering aspects. The main types of existing processes are described in a concise way and a focus is put on how to choose the right operating conditions considering both thermodynamic and hydrodynamic aspects. It is shown that the operating conditions and parameters can be easily optimized so as to facilitate the further process scale-up. Furthermore, the new trends in particle generation using SCFs are introduced, related either to new types of drug medicines that are treated or new ways of process implementation methods.
Elisabeth Badens, Yasmine Masmoudi, Adil Mouahid, Christelle Crampon. Current situation and perspectives in drug formulation by using supercritical fluid technology. Journal of Supercritical Fluids, 2018, 134, pp.274-283. ⟨10.1016/j.supflu.2017.12.038⟩. ⟨hal-02111546⟩
Frederique Bertaud, Christelle Crampon, Elisabeth Badens. Volatile terpene extraction of spruce, fir and maritime pine wood: supercritical CO2 extraction compared to classical solvent extractions and steam distillation
. Holzforschung, 2017, 71 (7-8), pp.667-763. ⟨10.1515/hf-2016-0197⟩. ⟨hal-01596420⟩ Plus de détails...
Frederique Bertaud, Christelle Crampon, Elisabeth Badens. Volatile terpene extraction of spruce, fir and maritime pine wood: supercritical CO2 extraction compared to classical solvent extractions and steam distillation
. Holzforschung, 2017, 71 (7-8), pp.667-763. ⟨10.1515/hf-2016-0197⟩. ⟨hal-01596420⟩
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Purification of sclareol by supercritical CO2 fractionation process. Journal of Supercritical Fluids, 2017, 122, pp.35 - 42. ⟨10.1016/j.supflu.2016.12.001⟩. ⟨hal-01596425⟩ Plus de détails...
The implementation and optimization of continuous supercritical CO2 fractionation of a clary sage extract containing 25 wt% of sclareol were performed in order to increase its sclareol content. After preliminary experiments confirming the feasibility of the process, different operating conditions were studied: CO(2-)over-feed mass ratio from 25 up to 115, and pressure between 11 and 13 MPa, with an internal reflux due to a thermal gradient 323-338 K along the column, through an experimental design. Four responses were highlighted: sclareol mass fraction in the raffinate, sclareol mass fraction in the extract, sclareol yield in the raffinate, and the amount of an undesirable compound exhibiting a similar behaviour to sclareol and thus, hard to separate from sclareol by conventional techniques. This work allowed us to highlight the best operating conditions: a pressure of 12.6 MPa and a CO2-over-feed mass ratio of 114.5 leading to a sclareol mass fraction in raffinate and extract of 75.3% and 4.6% respectively, to a sclareol yield of 82.4% in the raffinate, and to an amount of 0.08% of the undesirable compound in the raffinate.
C. Dufour, Christelle Crampon, C. Delbecque, P-P. Garry, Elisabeth Badens. Purification of sclareol by supercritical CO2 fractionation process. Journal of Supercritical Fluids, 2017, 122, pp.35 - 42. ⟨10.1016/j.supflu.2016.12.001⟩. ⟨hal-01596425⟩
Carlos Ariel Pieck, Christelle Crampon, Elisabeth Charton. A new model for the fractionation of fish oil FAEEs. Journal of Supercritical Fluids, 2017, 120 (2, SI), pp.258-265. ⟨10.1016/j.supflu.2016.05.024⟩. ⟨hal-01464693⟩ Plus de détails...
In this work, the supercritical fractionation of fatty acid ethyl estersă derived from fish oil was carried out with carbon dioxide at 333 K andă 14.5 MPa. The feed mixture is very complex, with over 80 differentă compounds detected by GC. Among them, the EicosaPentaenoic Acid (EPA)ă and DodecaHexaenoic Acid (DHA) ethyl esters are of major industrială interest since the consumption of these omega-3 acids has been linked toă a reduced risk of cardiovascular diseases. The influence of the processă parameters on the separation efficiency is an important point for ană economic analysis of the overall purification process. First, theă partition of the feed mixture was determined for differentă solvent-to-feed ratios varying between 21.8 and 143; the extract yieldă (i.e. the mass fraction of feed recovered as extract) has beenă calculated for each condition. Then, a new simplified equilibrium-stageă model was developed and applied to the mixture. Supposing a constantă distribution ratio, this model is able to correlate the influence of theă solvent-to-feed ratio (through a calculated extract yield) on theă concentration of the major 24 compounds present either in the feed or ină the extract and raffinate, including components with low, medium andă high distribution ratios. (C) 2016 Elsevier B.V. All rights reserved.
Carlos Ariel Pieck, Christelle Crampon, Elisabeth Charton. A new model for the fractionation of fish oil FAEEs. Journal of Supercritical Fluids, 2017, 120 (2, SI), pp.258-265. ⟨10.1016/j.supflu.2016.05.024⟩. ⟨hal-01464693⟩
This article deals with the extraction of neutral lipids andă antioxidants from enriched Spirulina platensis microalgae usingă supercritical carbon dioxide (CO2), and more particularly with theă influence of experimental conditions on extraction yields and kineticsă at laboratory and pilot scales. Preliminary studies were carried out ată laboratory scale before the establishment of an experimental design:ă extraction curves were plotted for different autoclave fill rates, andă under different conditions of pressure and temperature. Using a Responseă Surface Methodology, the significant influence of pressure on extractionă efficiency was highlighted. Surface responses showed that, in theă studied experimental field, mass loss increased when pressure,ă temperature, and CO2/microalgae mass ratio increased. Extract analysesă showed that oil extracts contained chlorophylls a and b, as well asă beta-carotene. Finally, larger-scale experiments were carried out withă batches of 1 and 50 kg (scale-factors of 100 and 5000, respectively) andă the results were consistent with those obtained at laboratory scale. (C)ă 2016 Elsevier B.V. All rights reserved.
Rania Djerafi, Andri Swanepoel, Christelle Crampon, Lonji Kalombo, Philip Labuschagne, et al.. Supercritical antisolvent co-precipitation of rifampicin and ethyl cellulose. European Journal of Pharmaceutical Sciences, 2017, 102, pp.161 - 171. ⟨10.1016/j.ejps.2017.03.016⟩. ⟨hal-01524709⟩ Plus de détails...
Adil Mouahid, Christelle Crampon, Sid-Ali Amine Toudji, Elisabeth Badens. Effects of high water content and drying pre-treatment on supercritical CO2 extraction from Dunaliella salina microalgae: Experiments and modelling. Journal of Supercritical Fluids, 2016, 116, pp.271-280. ⟨10.1016/j.supflu.2016.06.007⟩. ⟨hal-01461796⟩ Plus de détails...
This study investigates the effects due to the water content and to the drying pre-treatment on the extraction kinetics of solutes extracted from Dunaliella sauna microalgae by supercritical CO2. The extraction experiments were conducted at pressure range from 20 up to 40 MPa at a temperature of 333 K on crushed samples with water content varying from 5.5 up to 23 wt%. Three drying pre-treatments were applied: air flow drying at 318 K, air flow drying followed by additional microwave treatment and freeze-drying. A water content up to 23 wt% helps to extract a higher content of carotenoids (mainly beta-carotene) and does not restrict the extraction process. Sovova's mathematical model was applied and the parameters were adapted for the description of the extraction curves from samples containing high water content with a deviation between experimental and calculated values comprised between 1.1% and 4.3%. (C) 2016 Elsevier B.V. All rights reserved.
Adil Mouahid, Christelle Crampon, Sid-Ali Amine Toudji, Elisabeth Badens. Effects of high water content and drying pre-treatment on supercritical CO2 extraction from Dunaliella salina microalgae: Experiments and modelling. Journal of Supercritical Fluids, 2016, 116, pp.271-280. ⟨10.1016/j.supflu.2016.06.007⟩. ⟨hal-01461796⟩
Ahmed Zermane, Ouassila Larkeche, Abdeslam-Hassen Meniai, Christelle Crampon, Elisabeth Badens. Optimization of Algerian rosemary essential oil extraction yield by supercritical CO2 using response surface methodology. Comptes Rendus. Chimie, 2016, 19 (4), pp.538-543. ⟨10.1016/j.crci.2015.08.011⟩. ⟨hal-01461780⟩ Plus de détails...
The present study deals with the determination of optimal values of operating parameters such as temperature and pressure leading to the best yield of a supercritical CO2 extraction of essential oil from local rosemary plants, using the response surface methodology (RSM). The maximum of essential oil recovery percentage relative to the initial mass of leaf powder was 3.52 wt%, and was obtained at 313 K and 22 MPa. A second-order polynomial was used to express the oil recovery and the calculated mass of recovered oil using the RSM was very close to the experimental value, confirming the reliability of this technique. The chemical composition of the Algerian rosemary oil under the obtained optimal conditions (313 K and 22 MPa), determined by GC-MS analysis, revealed the presence of camphor (major compound) (52.12%), 1,8-cineole (9.65%), camphene (7.55%), alpha-pinene (6.05%), borneol (3.52%), aroma dendrene (2.11%), verbenone (1.97%), alpha-caryophyllene (1.71%), and others. (C) 2016 Academie des sciences. Published by Elsevier Masson SAS. All rights reserved.
Ahmed Zermane, Ouassila Larkeche, Abdeslam-Hassen Meniai, Christelle Crampon, Elisabeth Badens. Optimization of Algerian rosemary essential oil extraction yield by supercritical CO2 using response surface methodology. Comptes Rendus. Chimie, 2016, 19 (4), pp.538-543. ⟨10.1016/j.crci.2015.08.011⟩. ⟨hal-01461780⟩
Carlos Ariel Pieck, Christelle Crampon, Frédéric Charton, Elisabeth Badens. Multi-scale experimental study and modeling of the supercritical fractionation process. Journal of Supercritical Fluids, 2015, 105, pp.158-169. ⟨10.1016/j.supflu.2015.01.021⟩. ⟨hal-01297564⟩ Plus de détails...
In this work, the fractionation of water–ethanol mixtures by supercritical carbon dioxide at 333 K and 10.1 MPa was used as a model system to compare experimental extract and raffinate compositions and overhead loadings at laboratory, pilot and industrial scales to contribute toward a sizing methodology for counter-current supercritical fractionation columns. A series of three columns with an internal diameter of 19, 58 and 126 mm and with a height of 2, 4 and 8 m respectively were used for the different scales, meaning scaling factors from 9 to 44 between columns. The massic solvent-to-feed ratio was varied between 5.2 and 78.8. Experimental results at the different scales are analyzed and compared from the thermodynamic, mass transfer and column hydrodynamics points of view; and also using process simulation by equilibrium-stage models. In total, 42 successful experimental runs are taken into account, including 6 at a pilot scale unit and 2 at an industrial scale.
Carlos Ariel Pieck, Christelle Crampon, Frédéric Charton, Elisabeth Badens. Multi-scale experimental study and modeling of the supercritical fractionation process. Journal of Supercritical Fluids, 2015, 105, pp.158-169. ⟨10.1016/j.supflu.2015.01.021⟩. ⟨hal-01297564⟩
Béatrice Perrier, Christelle Crampon, Olivier Guézet, Coralie Simon, François Maire, et al.. Production of a methyl ester from the microalgae Nannochloropsis grown in raceways on the French west coast. Fuel, 2015, 153, pp.640-649. ⟨10.1016/j.fuel.2015.03.011⟩. ⟨hal-01247077⟩ Plus de détails...
The present article describes the production of oil from autotrophic microalgae grown in raceways in France, and presents the bench test results of a Diesel monocylinder engine with the derived biodiesel (methyl ester).The cultivation of Nannochloropsis has been performed under nitrogen limitation in order to increase the lipid content of the microalgae. After harvesting, a drying operation has been carried out so as to obtain a dry microalgae powder with controlled water content. Neutral lipids were then recovered using supercritical carbon dioxide extraction technology applied to the dry powder. One hundred kilograms of dry microalgae has been treated leading to about five kilograms of algal oil, free of polar lipids, that has been transesterified with methanol. The fuel obtained has been blended with a standard biofuel-free Diesel fuel (10% algal fuel/90% standard Diesel fuel B0) and engine tests have been carried out with the resulting blend (B10). In order to compare with well-known fuels similar engine tests were performed with B0 and with a B10 fuel made of ten percent vegetable oil methyl ester complying with the European 14214 fuel standard (B10 EU-type). The B10 quality was rather close to Diesel fuel except for oxidation stability, which was well below the minimum limit for Diesel fuel. The behavior of the B10 fuel appears to be very similar in terms of combustion efficiency and pollutant emissions to the one of the standard Diesel fuel B0.
Béatrice Perrier, Christelle Crampon, Olivier Guézet, Coralie Simon, François Maire, et al.. Production of a methyl ester from the microalgae Nannochloropsis grown in raceways on the French west coast. Fuel, 2015, 153, pp.640-649. ⟨10.1016/j.fuel.2015.03.011⟩. ⟨hal-01247077⟩
O. Larkeche, A. Zermane, A.-H. Meniai, C. Crampon, E. Badens. Supercritical extraction of essential oil from Juniperus communis L. needles: Application of response surface methodology. Journal of Supercritical Fluids, 2015, 99, pp.8-14. ⟨10.1016/j.supflu.2015.01.026⟩. ⟨hal-01297558⟩ Plus de détails...
The extraction of oil from Juniperus communis needles was investigated using supercritical CO2. The extraction was carried out varying the pressure in the range of 10–30 MPa, the temperature within 308–328 K, with a solvent flow rate fixed at 0.42 kg h−1, and a mean particle diameter equal to 0.5 mm or less than 0.315 mm. The operating parameters have been optimized using the response surface methodology where a second order polynomial expression was used to express the oil recovery, and the results were satisfactory. The maximum oil recovery relative to the initial mass was 6.55 wt%. It was obtained for an extraction under 328 K, 30 MPa and a particle diameter less than 0.315 mm. Selected samples of extracts were analyzed using gas chromatography–mass spectrometry (GC/MS) and the results show that the most concentrated compounds were germacrene D and 1-octadecene.
O. Larkeche, A. Zermane, A.-H. Meniai, C. Crampon, E. Badens. Supercritical extraction of essential oil from Juniperus communis L. needles: Application of response surface methodology. Journal of Supercritical Fluids, 2015, 99, pp.8-14. ⟨10.1016/j.supflu.2015.01.026⟩. ⟨hal-01297558⟩
Jean-Claude Bertrand, Pierre Doumenq, Remy Guyoneaud, Benoît Marrot, Fabrice Martin-Laurent, et al.. Applied microbial ecology and bioremediation. Environmental Microbiology : Fundamentals and Applications, Springer, Netherlands, 2015, Print ISBN : 978-94-017-9117-5 Online ISBN : 978-94-017-9118-2. ⟨10.1007/978-94-017-9118-2_16⟩. ⟨hal-02793466⟩ Plus de détails...
The large diversity of metabolic capacities and the high genetic plasticity of microorganisms allow them to degrade virtually all organic compounds of natural or anthropogenic (xenobiotics) origin including those that are sources of environmental pollution. Thus microorganisms are major actors to eliminate or alleviate pollutions in the environment. The natural attenuation processes due to microbial activities (biodegradation and/or biotransformation) as well as the possibilities of using microorganisms in preventive treatments and bioremediation – biostimulation, bioaugmentation, rhizostimulation, bioleaching, and bioimmobilization – are presented. The main methods for microbial treatment of pollution, the chemical structure and the origin of the major pollutants, as well as the mechanisms of degradation by microorganisms – on the basis of physiological, biochemical, and genetic approaches – are described. Examples of treatments are presented for urban wastewater (activated sludge, lagoons, and planted beds), solid wastes (aerobic treatment or composting, anaerobic treatment and methanization, discharges), gaseous effluents, pesticides, polychlorobiphenyls, and finally hydrocarbons and petroleum products in the marine environment.
Jean-Claude Bertrand, Pierre Doumenq, Remy Guyoneaud, Benoît Marrot, Fabrice Martin-Laurent, et al.. Applied microbial ecology and bioremediation. Environmental Microbiology : Fundamentals and Applications, Springer, Netherlands, 2015, Print ISBN : 978-94-017-9117-5 Online ISBN : 978-94-017-9118-2. ⟨10.1007/978-94-017-9118-2_16⟩. ⟨hal-02793466⟩
N. Wu, Yvan Wyart, Jérôme Rose, B Angeletti, Philippe Moulin. Application of membrane processes in fractionation of elements in river water. Water Science and Technology, 2015, 72 (12), pp.2277-90. ⟨10.2166/wst.2015.444⟩. ⟨hal-01294900⟩ Plus de détails...
The influence of wastewater treatment plant (WWTP) effluents from one microelectronic industrial zone on element concentrations and partitioning in river water was investigated. The stepwise membrane filtration is used to distinguish different size fractions including large particulate (>18 μm), particulate (0.2-18 μm), colloidal/nanoparticle (10 kDa-0.2 μm) and truly dissolved fractions (<10 kDa) in river water samples and WWTP effluents. Results demonstrated that anthropogenic inputs (WWTP effluents and industrial area) had an important influence on concentrations and partitioning of some elements in river water. Mass balance results showed that membrane filtration processes could realize a good fractionation for many elements (good recoveries) in water samples. Flux decline during 0.2 μm and 10 kDa filtrations were analyzed, and corresponding fouling mechanisms are discussed.
N. Wu, Yvan Wyart, Jérôme Rose, B Angeletti, Philippe Moulin. Application of membrane processes in fractionation of elements in river water. Water Science and Technology, 2015, 72 (12), pp.2277-90. ⟨10.2166/wst.2015.444⟩. ⟨hal-01294900⟩
Supercritical anti-solvent (SAS) process is considered to be a clean technology suitable for particle design. It is generally used in order to micronize compounds of interest under mild operating conditions of temperature and with very low residual solvent traces in the end-product. By varying the process parameters, the properties of the produced powders can be adjusted with defined size (generally micron or nanometer sized particles), morphology and a narrow particle size distribution. There is currently a growing interest for the elaboration of controlled delivery systems. For this purpose, the SAS process can also be applied in order to co-precipitate molecules of interest with biocompatible and/or biodegradable polymers. An experimental study dealing with supercritical anti-solvent (SAS) precipitation has been carried out in order to micronize a biocompatible polymer, ethyl cellulose, widely used as a drug carrier in controlled delivery systems for oral administration. Supercritical carbon dioxide was used as anti-solvent for the polymer and ethyl acetate (EtAc), generally recognized as safe (GRAS) by the FDA (Food and Drug Administration) as solvent. The influence of the variation of the main operating parameters upon the characteristics of the micronized polymer was evaluated. In particular, the temperature (308, 318 and 333 K), the polymer concentration (1, 3 and 4 wt%), the EtAc/CO2 molar ratio (5 and 8 mol%) and the capillary tube diameter (127 and 254 μm) while pressure was kept constant and equal to 10 MPa. Using a low organic solution concentration of 1 wt% and at a temperature of 308 K, ethyl cellulose was successfully micronized in submicron particles with a mean size of 300 nm. However, increasing the temperature or the polymer concentration in the organic solution favored the particle coalescence and even led to fiber formation.
Rania Djerafi, Yasmine Masmoudi, Christelle Crampon, Abdeslam-Hassen Meniai, Elisabeth Badens. Supercritical anti-solvent precipitation of ethyl cellulose. Journal of Supercritical Fluids, 2015, 105, pp.92-98. ⟨hal-01266175⟩
A. Zermane, O. Larkeche, Abdeslam-Hassen Meniai, Christelle Crampon, Elisabeth Badens. Optimization of essential oil supercritical extraction from Algerian Myrtus communis L. leaves using response surface methodology. Journal of Supercritical Fluids, 2014, 85, pp.89-94. ⟨10.1016/j.supflu.2013.11.002⟩. ⟨hal-01053268⟩ Plus de détails...
The present work deals with the application of the supercritical fluid extraction process to extract essential oils from the leaves of an Algerian myrtle plant (Myrtus communis L.). Using the surface response methodology, an optimization of the extraction recovery was carried out, varying the pressure in the range of [10-30 MPa], the temperature within [308-323 K], a solvent flow rate fixed at 0.42 kg h(-1) and a mean particle diameter equal to 0.5 mm or less than 0.315 mm. The maximum value of essential oil recovery relative to the initial mass of leaf powder was 4.89 wt%, and was obtained when the SC-CO2 extraction was carried out under 313 K, 30 MPa and with a particle diameter less than 0.315 mm. A second-order polynomial expression was used to express the oil recovery. The calculated mass of recovered oil using the response surface methodology was very close to the experimental value, confirming the reliability of this technique.
A. Zermane, O. Larkeche, Abdeslam-Hassen Meniai, Christelle Crampon, Elisabeth Badens. Optimization of essential oil supercritical extraction from Algerian Myrtus communis L. leaves using response surface methodology. Journal of Supercritical Fluids, 2014, 85, pp.89-94. ⟨10.1016/j.supflu.2013.11.002⟩. ⟨hal-01053268⟩
Adil Mouahid, Christelle Crampon, Sid-Ali Amine Toudji, Elisabeth Badens. Supercritical CO2 extraction of neutral lipids from microalgae: experiments and modelling. Journal of Supercritical Fluids, 2013, 77, pp.7-16. ⟨10.1016/j.supflu.2013.01.024⟩. ⟨hal-00993077⟩ Plus de détails...
The aim of this work is to show that the equations developed by Sovová, based on the concept of broken and intact cells for describing the supercritical extraction curves from plants and vegetables, can be applied for the modelling of the supercritical CO2 extraction curves obtained with microalgae. Experimental and modelling results of supercritical carbon dioxide extraction of lipids from four different microalgae: Nannochloropsis oculata, Cylindrotheca closterium, Chlorella vulgaris and Spirulina platensis, are presented. The experimental setup is a laboratory scale apparatus which allows an accurate monitoring of the mass loss of the microalgae sample during the extraction. The experimental data were obtained at a pressure of 40 MPa, a temperature of 333 K and CO2 flow rates from 0.3 to 0.5 kg/h. The extraction experiments were performed on samples having undergone different pretreatments: (i) after harvesting and centrifugation, microalgae were dried either by freeze-drying or air flow drying) and (ii) they were ground and sieved at different particle sizes (particle diameters ranging from 160 to 1000 μm). The complete extraction of neutral lipids was performed leading to mass losses up to 30% depending on the samples and on the operating conditions. Extracts were mainly composed of triglycerides (more than 90 wt% of extracts). The mathematical model published in 2005 and the simplified equations of extraction curves (using the characteristic times characterizing each extraction step) published in 2012 by Sovová were chosen to fit the experimental data. Among the hypotheses proposed by Sovovà, we considered that the flow pattern of supercritical CO2 in the extraction autoclave was plug flow and the extraction process was supposed to occur with negligible solute-matrix interactions. The adjustable parameters were calculated by minimizing the sum of least squares between experimental and calculated values of the extraction yield. Good agreement between the two models and our experimental measurements was obtained. The average absolute relative deviation ranges between 0.5 and 10.2%.
Adil Mouahid, Christelle Crampon, Sid-Ali Amine Toudji, Elisabeth Badens. Supercritical CO2 extraction of neutral lipids from microalgae: experiments and modelling. Journal of Supercritical Fluids, 2013, 77, pp.7-16. ⟨10.1016/j.supflu.2013.01.024⟩. ⟨hal-00993077⟩
Christelle Crampon, Adil Mouahid, Sid-Ali Amine Toudji, Olivier Lépine, Elisabeth Badens. Influence of pretreatment on supercritical CO2 extraction from Nannochloropsis oculata. Journal of Supercritical Fluids, 2013, 79, pp.337-344. ⟨10.1016/j.supflu.2012.12.022⟩. ⟨hal-00993082⟩ Plus de détails...
This work demonstrates that supercritical carbon dioxide extraction is efficient for the complete recovery of neutral lipids from microalgae with a water content up to 20 wt%, allowing thus a further full characterization of this oil. This is a first useful step in the framework of lipid production from microalgae either for nutraceutical, food or for energy applications. This study is particularly focused on the influence of the pretreatments upon extraction kinetics and yields. This study proposes a complete study at laboratory scale (10 g per batch of dry biomass) of the influence of pretreatments (type of drying and grinding) and of water content on the extraction kinetics and yields as well as on the oil composition in terms of lipidic classes and profiles. Two drying pretreatments (drying under air flow and freeze-drying) applied on Nannochloropsis oculata were studied. Extraction experiments were carried out at 40 MPa, 333 K, with a carbon dioxide flow rate of 0.5 kg h−1 and for different granulometries. Results showed that drying under air flow at 308 K is the most adequate pretreatment leading to the most rapid kinetics. Whatever the pretreatment used, the extracted oil contains more than 90 wt% of triglycerides and does not contain phospholipids. As expected, the smaller the particle size, the faster the extraction kinetics. Finally, an increase in the biomass water content up to 20 wt% increases the global extraction kinetics (extraction of both water and oil) but appears to have no influence on oil extraction yields. Moreover, the extraction of neutral lipids happens to be complete for a CO2/charge mass ratio ranging from 30 to 130 depending on the operating conditions and on the characteristics of the treated biomass. Finally, pilot scale experiments were performed with batches up to 15 kg in order to evaluate the influence of pressure and particle size on the extraction kinetics and yields. Extracts obtained at 333 K with operating pressures of 50 MPa and 85 MPa have similar compositions and do not contain phospholipids.
Christelle Crampon, Adil Mouahid, Sid-Ali Amine Toudji, Olivier Lépine, Elisabeth Badens. Influence of pretreatment on supercritical CO2 extraction from Nannochloropsis oculata. Journal of Supercritical Fluids, 2013, 79, pp.337-344. ⟨10.1016/j.supflu.2012.12.022⟩. ⟨hal-00993082⟩
Nan Wu, Yvan Wyart, Jérôme Rose, B Angeletti, Philippe Moulin. Influence of wastewater treatment from microelectronics industry on concentrations and partitioning of elements in a river. Advances in Biomedical Engineering, 2012, 7, pp.121-129. ⟨hal-00997222⟩ Plus de détails...
The influence of wastewater treatment plant (WWTP) effluents from a microelectronic industrial zone (IZ) on natural waters (Arc river) was investigated. Surface water samples from upstream, downstream, and WWTP effluents were analyzed by distinguishing 'background' geogenic sources from anthropological sources. Amongst the five elements (Si, V, Se, Sr, U) analyzed, Si increased in concentration (in raw water) in the downstream compared to upstream, which indicated a discharge of Si from anthropological sources (IZ site) into receiving waters, even if no contaminated levels were reached. Meanwhile, the anthropogenic inputs have an important influence on the distribution of elemental partitioning among large particulates (>18 μm), particulates (0.22-18 μm), colloidal/nanoparticle (10 kDa-0.22 μm) and truly dissolved fractions (<10 kDa), which were distinguished by filter cartridges and membranes with decreasing cut-offs.
Nan Wu, Yvan Wyart, Jérôme Rose, B Angeletti, Philippe Moulin. Influence of wastewater treatment from microelectronics industry on concentrations and partitioning of elements in a river. Advances in Biomedical Engineering, 2012, 7, pp.121-129. ⟨hal-00997222⟩
Laurène Lesoin, Christelle Crampon, Olivier Boutin, Elisabeth Badens. Preparation of liposomes using the supercritical anti-solvent (SAS) process and comparison with a conventional method. Journal of Supercritical Fluids, 2011, 57 (2), pp.162-174. ⟨10.1016/j.supflu.2011.01.006⟩. ⟨hal-01044553⟩ Plus de détails...
Two methods to produce liposomes encapsulating a fluorescent marker were compared: the supercritical anti-solvent (SAS) method and a conventional one (Bangham). Liposome size and encapsulation efficiency were measured to assess the methods. Micronized lecithin produced by the SAS process was characterized in terms of particle size, morphology and residual solvent content in order to investigate the influence of experimental parameters (pressure, CO2/solvent molar ratio and solute concentration). It appears that when the lecithin concentration increases from 15 to 25 wt.%, at 9 MPa and 308 K, larger (20-60 μm) and less aggregated lecithin particles are formed. As concerns liposomes formed from SAS processed lecithin, size distribution curves are mainly bimodal, spreading in the range of 0.1-100 μm. Liposome encapsulation efficiencies are including between 10 and 20%. As concerns the Bangham method, more dispersed liposomes were formed; encapsulation efficiencies were about 20%, and problems of reproducibility have been raised.
Laurène Lesoin, Christelle Crampon, Olivier Boutin, Elisabeth Badens. Preparation of liposomes using the supercritical anti-solvent (SAS) process and comparison with a conventional method. Journal of Supercritical Fluids, 2011, 57 (2), pp.162-174. ⟨10.1016/j.supflu.2011.01.006⟩. ⟨hal-01044553⟩
Laurène Lesoin, Olivier Boutin, Christelle Crampon, Elisabeth Badens. CO2/water/surfactant ternary systems and liposome formation using supercritical CO2: a review. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2011, 377 (1-3), pp.1-14. ⟨10.1016/j.colsurfa.2011.01.027⟩. ⟨hal-01044546⟩ Plus de détails...
The aim of this review is to explain the various phenomena involved in liposome formation using dense gas processes and especially supercritical CO2. Before liposome formation, the review focuses on the phase behavior of CO2/water/surfactant ternary systems. First of all, the two main cases of CO2/water/surfactant fluid phase behavior are studied: reverse micelle systems and Winsor systems. Then, the various mechanisms of emulsion destabilization as a function of formulation variables (pressure, temperature and water content) are tackled. Influence of formulation variables is also addressed in the case of liposome formation during depressurization and CO2 release for dense gas techniques. Techniques using supercritical or subcritical conditions are classified according to the hydration way: in the first case, hydration is carried out under pressure and in the second one, hydration is achieved after depressurization. Hydration under pressure involves the formation of a CO2/water/surfactant system which is not the case when hydration is carried out during depressurization. An emergent tendency in liposome formation may be noted: (i) large unilamellar vesicles would appear when hydration is achieved under pressure, i.e. when liposomes are the result of two phase inversions (inversion phase from water-in-CO2 emulsion to CO2-in-water emulsion and inversion phase from CO2-in-water emulsion to liposomes); (ii) multilamellar vesicles would be formed when hydration is realized during depressurization, i.e. when liposomes are the result of one phase inversion (inversion phase from CO2-in-water to liposomes). Lastly, a model of liposome formation is developed.
Laurène Lesoin, Olivier Boutin, Christelle Crampon, Elisabeth Badens. CO2/water/surfactant ternary systems and liposome formation using supercritical CO2: a review. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2011, 377 (1-3), pp.1-14. ⟨10.1016/j.colsurfa.2011.01.027⟩. ⟨hal-01044546⟩
Journal: Colloids and Surfaces A: Physicochemical and Engineering Aspects
Christelle Crampon, Olivier Boutin, Elisabeth Badens. Supercritical carbon dioxide extraction of molecules of interest from microalgae and seaweeds. Industrial and engineering chemistry research, 2011, 50 (15), pp.8941-8953. ⟨10.1021/ie102297d⟩. ⟨hal-01044580⟩ Plus de détails...
The purpose of this paper is to guide lectors in the extraction of algal (microalgae and seaweeds) compounds using supercritical carbon dioxide (SC-CO2) from dry biomass. It proposes a review of 30 articles dealing with the SC-CO2 extraction of molecules of interest from microalgae and seaweeds. Among these papers, 20 are devoted to microalgae. The most extracted compounds are neutral lipids and antioxidants. Several operating conditions have been tested: pressures from 7.8 to 70 MPa, temperatures from 313.15 to 349.15 K, and CO2/algae mass ratio from 6 to 500. All extraction studies were performed at laboratory scale, with the masses of dry algae powder never exceeding 180 g. Extraction yields vary significantly with operating conditions: pressure seems to be the most influential parameter. The higher the pressure, the higher the yields and/or the faster the extraction kinetics. Temperature also has an influence, but its effect is dependent on pressure (retrograde behavior). Moreover, as expected, it is advised to work with a high CO2/algae mass ratio. From these works, it appears that, to perform an efficient extraction with SC-CO2, the influence of the algae pretreatment is highly significant. The first step is a centrifugation. The resulting concentrated algal suspension must then undergo a drying operation, which is generally freeze-drying or low-temperature drying. Finally, the algae are crushed. Concerning the influence of crushing, the reported results show that, as expected, the smaller the particles, the more rapid the extraction kinetics and/or the higher the yields.
Christelle Crampon, Olivier Boutin, Elisabeth Badens. Supercritical carbon dioxide extraction of molecules of interest from microalgae and seaweeds. Industrial and engineering chemistry research, 2011, 50 (15), pp.8941-8953. ⟨10.1021/ie102297d⟩. ⟨hal-01044580⟩
Journal: Industrial and engineering chemistry research
Laurène Lesoin, Christelle Crampon, Olivier Boutin, Elisabeth Badens. Development of a continuous dense gas process for the production of liposomes. Journal of Supercritical Fluids, 2011, 60, pp.51-62. ⟨10.1016/j.supflu.2011.04.018⟩. ⟨hal-01044574⟩ Plus de détails...
A new process called Continuous Anti-Solvent (CAS) process was developed for the production of liposomes using supercritical CO2. Unlike the current dense gas technologies, CAS method is a single step and continuous process. Preliminary experiments were conducted in semi-batch mode to determine the most suitable operating conditions (stirring speed = 225 rpm; water/lecithin mass ratio = 21) to ensure an efficient phase mixing in the autoclave. Then, two procedures were developed for the CAS process in the continuous mode. According to the results, the single exit procedure enhances the phase mixing in the autoclave with the formation of a CO2-in-water emulsion which is a good precursor to liposome formation. Liposomes prepared with the CAS method (P = 9 MPa; T = 308 K; CO2 flow rate = 0.3 kg h−1; organic solution flow rate = 240 mL h−1; water flow rate = 180 mL h−1) are spherical and multilamellar with a medium diameter included between 10 and 100 μm.
Laurène Lesoin, Christelle Crampon, Olivier Boutin, Elisabeth Badens. Development of a continuous dense gas process for the production of liposomes. Journal of Supercritical Fluids, 2011, 60, pp.51-62. ⟨10.1016/j.supflu.2011.04.018⟩. ⟨hal-01044574⟩
