Tunable process for silica capsules/spheres preparation and their use
Inventors
Aboshyan-Sorgho, Lilit • BELAND, François • Desplantier-Giscard, Delphine • Morin, Michel • Pandarus, Valerica
Assignees
Interested in licensing this patent?
MTEC can help explore whether this patent might be available for licensing for your application.
Publication Number
US-12201956-B2
Publication Date
2025-01-21
Expiration Date
Abstract
The disclosure relates to porous and non-porous silica capsules (capsules in capsule or core-shell capsules), porous microspheres, as well as their direct phase emulsification process without surfactant and their use, wherein the particles comprise a liposoluble active/payload.
Core Innovation
The invention relates to a process of preparation of spheroidal organosiloxane particle, including separately hydrolyzing two or more mono(silane) compounds in a hydrolytic media to provide two or more pre-hydrolyzed silica precursors, and combining all the pre-hydrolyzed silica precursors into one container. The mono(silane) compounds contain one silicon atom, and dipodal silane compounds contain two silicon atoms, where R and R are organic residues and L is halogen or an acetoxide or alkoxide group.
The process further includes pre-condensing the pre-hydrolyzed silica precursor mixture by removing a portion of or all volatile solvents from the hydrolytic media, then adding a liposoluble payload to provide a dispersed phase. The dispersed phase is emulsified in absence of a surfactant, in an aqueous continuous phase, to provide an oil-in-water emulsion, and a condensation catalyst is added to obtain the spheroidal organosiloxane particle.
In one described embodiment, the liposoluble payload is provided in various formulations for protecting and releasing liposoluble materials, including retinol (all-trans-retinol) and lipids present in simulated sebum media such as squalene and oleic acid. The disclosed particles are tunable as non-porous and porous spheroidal ORMOSil silica capsules/spheres, including capsules-in-capsules and core-shell-within-microcapsules, with particle morphology and porosity tailored by silica precursor selection and payload identity to achieve leakless non-porous particles and controlled-release porous particles.
Claims Coverage
The independent claim clm-00001 covers a five-step process for producing spheroidal organosiloxane particles using separately hydrolyzed mono- and/or dipodal silane precursors, surfactant-free oil-in-water emulsification of a liposoluble payload, and subsequent condensation with a catalyst. The inventive features are concentrated in precursor handling, surfactant-free emulsification, and the catalyst step to form spheroidal particles.
Separately hydrolyzing mono(silane) and/or dipodal silane precursors
Separately hydrolyzing two or more mono(silane) compounds in a hydrolytic media to provide two or more pre-hydrolyzed silica precursors and combining all the pre-hydrolyzed silica precursors into one container, wherein the mono(silane) compound contains one silicon atom of formula R4-xSi(L)x or a dipodal silane compound containing two silicon atoms of formula (L)3SiRSi(L)3, with R and R defined and L defined as halogen or acetoxide or alkoxide.
Pre-condensing the combined pre-hydrolyzed silica precursor mixture
Pre-condensing the combined one or more pre-hydrolyzed silica precursors by removing a portion of or all volatile solvents from the hydrolytic media to provide a pre-condensed silica precursor mixture.
Dispersing a liposoluble payload in the pre-condensed silica precursor mixture
Adding a liposoluble payload to the mixture of step 2 to provide a dispersed phase.
Surfactant-free oil-in-water emulsification
Emulsifying, in absence of a surfactant, the dispersed phase in an aqueous continuous phase to provide an oil-in-water emulsion.
Condensation-catalyst formation of spheroidal organosiloxane particles
Adding a condensation catalyst to the emulsion to obtain the spheroidal organosiloxane particle.
Across the independent claim, spheroidal organosiloxane particles are produced by separately hydrolyzing specified mono- and/or dipodal silane precursors, pre-condensing the combined pre-hydrolyzed precursors, dispersing a liposoluble payload, forming an oil-in-water emulsion without a surfactant, and then adding a condensation catalyst to yield the spheroidal particles.
Stated Advantages
“Leakless” non-porous particles.
Controlled-release porous particles.
Particle morphology and porosity are tailored by silica precursor selection and payload identity.
Documented Applications
Encapsulation of liposoluble payloads including retinol (all-trans-retinol).
Protection and release performance assessed using simulated sebum media containing squalene and oleic acid.
Encapsulation of lipids/oils and oil-phase constituents such as corn oil, triglyceride oils, and squalene (as described in the provided summary content).
Encapsulation of various cosmetic/cosmeceutical/dermatological/pharmaceutical/perfume/flavoring ingredients as liposoluble payloads (as supported by the dependent claim refinements in the provided claim set).
Interested in licensing this patent?