Cellulose nanocrystals to stabilize. Pickering emulsions
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1 Cellulose nanocrystals to stabilize versatile O/W and W/W Pickering emulsions PRESENTED BY Isabelle Capron INRA Nantes France Co-Authors Karthick Peddireddy 1,2 Fanch Cherhal 1 Lazhar Benyahia 2 Taco Nicolaï 2 1 Biopolymeres, Interactions et Assemblages, INRA Nantes, France 2 Institut des Molécules et Matériaux du Mans, University of Le Mans, France
2 Emulsions An emulsion is a metastable system of two immiscible liquids that tend to macroscopic phase separation Phase 1 Phase 2 Phase 1 Phase 2 Biphasic system + Surface active agent Flocculation Coalescence Uncontroled emulsion Controled emulsion Stabilization
3 Three main types of interfacial stabilisation Surface active agents at an oil / water interface oil wat er oil wa ter oil wat er mono layer surfactant molecule multi layer associated polymers colloidal particles Pickering emulsions Renew since 15 years due to interest for innovative applications Pickering, S. U. Journal of Chemical society, (1907), 91, 2001.
4 Properties of Pickering emulsions: Size and wetting parameters for = 50 mn/m oil water Hydrophilic particle oil Hydrophobic particles oil Energy ² 1 cos ² water water Particles irreversibly adsorbed at the interfaces Surface chemistry influences emulsion properties B.P. Binks Current Opinion in Colloid & Interface Science 7 (2002) 2141
5 Cellulose nanocrystals as colloidal particles Colloidal suspension of cotton CNC Parallelepipedic shape by neutron scattering (2mM NaCl) dispersion at 1% MET Intensity (cm 1 ) Q (A 1 ) Crystalline planes for I allomorph Electrostatic interactions SO3 OH CH Hydrogen bonds, van der Waals, hydrophobic interactions thickness width length ± 0.2 nm ±3 nm ±30 nm Stiff nanorods (an alternative to spherical particles) with percolation limit and contrasted surfaces F. Cherhal, F. Cousin and I. Capron Langmuir (2015), 31,
6 CNC as surface active particles for oil / water Pickering Emulsion hexadecane emulsification aqueous phase suspension of CNC 50 mm NaCl 10 m highly stable emulsions : dispersion concentration creaming process time > 1 year temperature ph from 1 to 12 Patent n WO2012/017160, capron et al I. Kalashnikova, I. Capron et al., Langmuir (2011),, 27(12), µm MEB BIBS platform Nantes
7 Drop size and coverage modulation Diameter variation with the CNC concentration (NaCl 50mM) Monomodal distribution 60 D[3,2] (µm) Surface (%) 10 Drop diameter (µm) mg CNC / ml hexadecane) I. Kalashnikova, I. Capron et al. soft matter (2013), 9,
8 Drop size and surface coverage modulation Emulsions prepared varying concentration 0,9 0,8 Emulsions at various CNC contents % hexadecane emulsion ratio (%) 0,7 0,6 0,5 0,4 0,3 0,2 74% of hexadecane Close packing conditions 0, (g/l) concentration BCN (g/l) CN concentration (g/l) CNC concentration (g/l) After centrifugation 4000g 84% coverage Multilayers? (g/l) CNC concentration (g/l) Kalashnikova, I.; Bizot, H.; Cathala, B.; Capron, I. Langmuir, (2011), 27,
9 Drop size and surface coverage modulation Small angle neutrons scattering : thickness of 7 nm whatever the CNC concentration monolayer of CNCs. h =7 nm I. Kalashnikova, I. Capron et al. soft matter (2013), 9, F Cherhal, F Cousin, and I. Capron Biomacromolecules (2016), 7,
10 Structuration at the interface? Limited coalescence domain: drop size variation Fixed surface coverage 84% 40 D[3,2] (µm) Coverage variation, densification Accessibility of the (200) crystalline plane responsible for the stabilisation Mg CNC /ml hexadecane Due to their high anisotropy: percolation threshold + densification by orientation Less material is needed to stabilize emulsions High surface interaction = strong adsorption I. Kalashnikova, I. Capron et al. Biomacromolecules (2012), 13, F Cherhal, F Cousin, and I. Capron Biomacromolecules (2016), 7,
11 On the way to innovative emulsions compartmentalization for biotechnology and medicine Structural roles for innovative food emulsions Surfactant free cosmetics and coatings formulations Development of new types of surfactant free emulsions Oil emulsion: high internal phase emulsions Water emulsion: water in water emulsions
12 1 st example: High Internal Phase Emulsion (HIPE) oil as a gel HIPEs are emulsified systems with an internal phase volume fraction > 74% (maximum packing density of monodispersed hard spheres). + oil Adding oil upon shearing increases the drop size up to deformation without coalescence. 50% 74% Pickering MIPE 10µm 20% oil 60% oil HIPE 85% oil CLSM BIBS platform Nantes (F) Liquid emulsion Soft gel Hard gel I. Capron, H. Bizot & B. Cathala Brevet WO2013/ I. Capron and B. Cathala Biomacromolecules, (2013), 14, 291
13 1 st example: High Internal Phase Emulsion (HIPE) 90 % of oil 74 % Surface charge density variation < 0.01 e/nm² 0.2 e/nm² 0.6 e/nm² Up to 90% of oil stabilized without any surfactant irrespective of surface charge densities stabilized by less than 0.1% of CNC
14 2 nd exemple: Water in water (w/w) emulsion Polymer A + Polymer B Phase diagramm miscible Coacervation 12 < 0 Thermodynamic Incompatibility 12 > 0 C polymer B Tie line: same interfacial tension Volume fraction variation C polymer A Mixture of aqueous solutions of biopolymers is generally thermodynamically incompatible leading to phase separation. Very low interfacial tension values (0.5 mn/mfor W/W vs 50 mn/m for O/W emulsions) and large interfacial thickness Stabilization of w/w emulsions is a big challenge I. Capron, S. Costeux and M. Djabourov, Rheologica Acta, (2001), 40, M. Vis et al. ACS Macro Lett. 2015, 4 (9),
15 2 nd exemple: stable water in water (w/w) emulsion Phase diagramm PEO and FITC labelled dextran without CNC PEO phase C PEO (w%) Dextran phase + CNC + emulsification C dextran (w%) Stable PEO in dextran emulsion K Peddireddy, T. Nicolai, L. Benyahia and I. Capron ACS Macro lett. (2016), 5, 283.
16 Conclusions CNC for Pickering emulsions CNC at the interface form a rigid interfacial film CNCs stabilize emulsions forming a monolayer 7 nm thick CNCs offer a large range of surfactant free emulsions: O/W high internal phase emulsions (HIPE) may stabilise oil as a gel with very low amount of CNCs (<0.1 wt%) and water. W/W emulsions might be stabilized efficiently with CNC
17 Acknowledgement Emilie Perrin Joelle Davy Solène Grosbois Hervé Bizot Bernard Cathala
18 Thank you PRESENTED BY Isabelle Capron INRA - France Isabelle.capron@nantes.inra.fr
19 International Conference of Biobased Materials and Composites Processing of Bio-based composites Bioinspired and biomimetic Nanohybrids Degradation and Stabilization of Natural Polymer Materials for Energy Gels Interpenetrating polymer network BioNanocomposites Aerogels Materials for Biomedical Interface and Surface design Characterization and fractionation of biomass Stimuli responsive materials Pulp and Paper Rheology of Natural Polymers (ICBMC) Save the date: 29, 30, 31 March 2017 in NANTES (Fr) Honor guest: Prof. Hans R. Kricheldorf: Professor Emeritus at Hamburg University Invited speakers Pr. Giovanni Camino: Italy Dr. Patrick Navard: France Dr. Didier Letourneur: France Pr. Lars Wagberg: Sweden Website not indexed yet Symposium.inra.fr /icbmc2017 More information coming Scientific committee Bernard Cathala, Alain Dufresne, Etienne Fleury, Yves Grohens, Hamid Kaddami, Eric Leroy, Denis Lourdin, Bastien Séantier Contact: Sponsors
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