US 12,186,723 B2
Method for preparing capsules comprising at least one volatile compound and capsules obtained therefrom
Damien Demoulin, Paris (FR); Ludivine Mousnier, Villebon sur Yvette (FR); Karima Ouhenia, Neuilly Plaisance (FR); and Jamie Walters, Paris (FR)
Assigned to CALYXIA, Bonneuil-sur-Marne (FR)
Appl. No. 16/496,057
Filed by CALYXIA, Bonneuil-sur-Marne (FR)
PCT Filed Mar. 21, 2018, PCT No. PCT/EP2018/057216
§ 371(c)(1), (2) Date Sep. 20, 2019,
PCT Pub. No. WO2018/172433, PCT Pub. Date Sep. 27, 2018.
Claims priority of application No. 1752332 (FR), filed on Mar. 21, 2017.
Prior Publication US 2021/0113984 A1, Apr. 22, 2021
This patent is subject to a terminal disclaimer.
Int. Cl. B01J 13/18 (2006.01); C08F 2/22 (2006.01); C08F 2/50 (2006.01)
CPC B01J 13/18 (2013.01) [C08F 2/22 (2013.01); C08F 2/50 (2013.01)] 14 Claims
 
1. A method for preparing solid microcapsules comprising the following steps:
a) preparing a composition C1, which is either a composition C1a, comprising a single hydrophobic solid particle, or a composition C1b comprising a plurality of hydrophobic solid particles dispersed in a hydrophilic phase,
the hydrophobic solid particle(s) containing one or more lipophilic volatile compounds and one or more hydrophobic materials, said material(s) being solid at room temperature and liquid at a temperature above Tm,
b) adding, under stirring, of the composition C1 in a polymeric composition C2 at a temperature Tb, the compositions C1 and C2 being immiscible with one another, the temperature Tb being greater than Tm when the composition C1 is a composition C1a and the temperature Tb being less than Tm when the composition C1 is a composition C1b,
the composition C2 comprising at least one monomer or polymer and at least one crosslinking agent, and at least one (photo) initiator or crosslinking catalyst,
the viscosity of the composition C2 being between 500 mPa·s and 100 000 mPa·s at 25° C., and being greater than the viscosity of the composition C1,
whereby an emulsion (E1) comprising drops of composition C1a or C1b dispersed in composition C2 is obtained;
c) adding, under stirring, of the emulsion (E1) in a composition C3 at a temperature Tc, the compositions C2 and C3 not being miscible with each other, the temperature Tc being greater than Tm when the emulsion (E1) comprises drops of composition C1a dispersed in composition C2 and the temperature Tc being less than Tm when the emulsion (E1) comprises drops of composition C1b dispersed in the composition C2, the viscosity of the composition C3 being between 500 mPa·s and 100 000 mPa·s at 25° C., and being greater than the viscosity of the emulsion (E1),
whereby a double emulsion (E2) comprising drops dispersed in the composition C3 is obtained;
d) applying shear to the emulsion (E2) at a temperature Td, the temperature Td being greater than Tm when the composition C1 of step a) is a composition C1a and the temperature Td being less than Tm when the composition C1 of step a) is a composition C1b,
whereby a double emulsion (E3) is obtained comprising controlled size drops dispersed in the composition C3; and
e) polymerizing the composition C2, whereby solid microcapsules dispersed in the composition C3 are obtained.