IP Library Granted Patent US 10,597,298
Granted Patent B2
US 10,597,298 · App. 15/783,614 · Granted Mar 24, 2020

Ceramic encapsulation by use of one or more specialized silanes to template oil in an oil in water emulsion

Inventors: Daniel H. Traynor (Sarasota, FL); Hao Xu (Canton, MI); Henry G. Traynor (Sarasota, FL); John Carson (Union City, NJ); Martin S. Flacks (Danville, CA)
Assignee: CoLabs International Corporation
C01B33/18C09C1/30A61K9/501C01P2004/03C01P2004/34C01P2004/52
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Quick Facts
Patent No.
US 10,597,298
App. No.
15/783,614
Granted
Mar 24, 2020
Kind
B2
Abstract

This invention relates to a method for emulsion templating hollow silica-based particles. The particles are suitable for containing one or more active ingredients or for containing other smaller particles which may include one or more active ingredients. The emulsion templated particles can be formed from two or more silanes. The emulsion templated particles can also be formed from a silane and a compound that attaches a polymer on the shell of the hollow silica-based particles.

Claims (28)

1. A method for forming silica-based particles, the method comprising the steps:

(a) preparing an emulsion having a basic pH, the emulsion including a continuous phase that is polar and has one or more nonionic surfactants and/or one or more anionic surfactants, and a dispersed phase comprising droplets including a non-polar active ingredient and a non-polar diluent;

(b) adding a first modified silica precursor to the emulsion such that the first modified silica precursor is emulsion templated onto the surface of the droplets to form a silica-based first shell layer around the droplets, wherein the first shell layer formed has a mean thickness of about 1 nm to about 500 nm within 2 hours from addition of the first modified silica precursor to the emulsion, and wherein the first modified silica precursor has the general formula (I):

R 1 x -Si-(OR 2 ) y   (I)

wherein R 1 is selected from substituted and unsubstituted alkyl, aryl, alcohols, amines, amides, aldehydes, acids, esters, and functional groups having an unsaturated carbon-carbon bond, wherein R 2 is an alkyl group, wherein x+y=4, and wherein x=1 or 2;

(c) adding a second modified silica precursor to the emulsion such that a coating can be deposited on at least part of the silica-based first shell layer through the interaction of the second modified silica precursor with the first modified silica precursor present in the silica-based first shell layer to form a second shell layer, wherein the first silica precursor and the second silica precursor are different; and

(d) allowing the emulsion to sit for up to 2 days until the thickness of the first shell layer and the second shell layer together have a mean thickness in the range of about 1 μm to about 250 μm;

wherein the method produces silica-based particles having a silica-based shell surrounding a liquid core comprising the non-polar active ingredient and the non-polar diluent.

2. The method of claim 1 , wherein the second modified silica precursor has the general formula (II):

R 3 m -Si-(OR 4 ) n   (II)

wherein R 3 is selected from substituted and unsubstituted alkyl, aryl, alcohols, amines, amides, aldehydes, acids, esters, and functional groups having an unsaturated carbon-carbon bond, and amino functional groups, wherein R 4 is an alkyl group, wherein m+n=4, and wherein m=1 or 2.

3. The method of claim 2 , wherein at least one of R 1 of the first modified silica precursor and R 3 of the second modified silica precursor has a net charge to attract towards an opposite charge of a surfactant at interfaces between the droplets and the continuous phase.

4. The method of claim 2 , wherein at least one of R 1 of the first modified silica precursor and R 3 of the second modified silica precursor prevents or limits aggregation of the silica-based particles.

5. The method of claim 2 , wherein at least one of R 1 of the first modified silica precursor and R 3 of the second modified silica precursor allows for attachment of a polymer or other molecular complex to a surface of the particles by covalent linking.

6. The method of claim 2 , wherein step (c) comprises adjusting a ratio of the first modified silica precursor and the second modified silica precursor to modify the silica-based silica particle from a continuously formed shell to a partially formed shell.

7. The method of claim 1 , wherein the amount of the one or more nonionic surfactants and/or the one or more anionic surfactants is below a critical micelle concentration of the surfactant for precursor interface interaction.

8. The method of claim 1 , wherein the amount of the one or more nonionic surfactants and/or the one or more anionic surfactants is above a critical micelle concentration of the surfactant.

9. The method of claim 1 , wherein the one or more nonionic surfactants and/or the one or more anionic surfactants speed up the reaction at interfaces between the droplets and the continuous phase by targeting and directing precursor formation at interfaces between the droplets and the continuous phase.

10. The method of claim 1 , wherein the silica-based first shell layer has a first shell layer thickness of about 2 nm to about 200 nm.

11. The method of claim 10 , wherein the silica-based first shell layer has a first shell layer thickness of about 2 nm about 100 nm.

12. The method of claim 1 , wherein the second precursor is a water soluble polymeric compound or an unsaturated compound, and the coating includes a polymer.

13. The method of claim 12 , wherein the second precursor is a water soluble polymeric compound.

14. The method of claim 12 , wherein R 1 of the first modified silica precursor allows for attachment of the water soluble polymeric compound or the unsaturated compound to a surface of the particles by covalent linking.

15. The method of claim 1 , wherein the non-polar active ingredient is an oil, and the method further comprises washing the silica-based particles such that the oil remains in the shell of the silica-based particles after being washed.

16. The method of claim 1 , wherein the silica-based particles have a Zeta potential range from 0 mV to 150 mV.

17. The method of claim 1 , wherein the liquid core comprises the hydrophobic active ingredient in the form of a solution, dispersion, or emulsion.

18. The method of claim 1 , wherein the shell is a mono-pore shell.

19. The method of claim 1 , wherein the non-polar active ingredient includes a sunscreen, a steroidal anti-inflammatory active, an analgesic, active, an antifungal, an antibacterial, an antiparasitic, an antiviral, an anti-allergenic, an anti-cellulite additive, a medicinal active, a skin rash medication, a skin disease medication, a dermatitis medication, an insect repellant active, an antioxidant, a hair growth promoter, a hair growth inhibitor, a hair bleaching agent, a deodorant compound, a sunless tanning active, a skin lightening active, an antiacne active, an anti-skin wrinkling active, an anti-skin aging active, a vitamin, a nonsteroidal anti-inflammatory active, an anesthetic active, an anti-pruritic active, an anti-microbial active, a dental care agent, a personal care agent, a nutraceutical, a pharmaceutical, a fragrance, a flavoring, a antifouling agent, a pesticide, a lubricant, an etchant, mixtures thereof or combinations thereof.

Assignments (4)
CHANGE OF NAME Recorded Dec 11, 2017
From: AQUEA SCIENTIFIC CORPORATION
To: ASC DISSOLUTION CORPORATION
Reel/Frame 044349/0529 →
NUNC PRO TUNC ASSIGNMENT Recorded Nov 24, 2017
From: TRAYNOR, DANIEL H.; FLACKS, MARTIN S.
To: AQUEA SCIENTIFIC CORPORATION
Reel/Frame 044206/0609 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 24, 2017
From: XU, HAO; TRAYNOR, HENRY G.; CARSON, JOHN
To: AQUEA SCIENTIFIC CORPORATION
Reel/Frame 044206/0615 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 26, 2017
From: AQUEA SCIENTIFIC CORPORATION
To: COLABS INTL CORP
Reel/Frame 043960/0062 →
Continuity (3)
Continuation 13011564 · Jan 21, 2011
Provisional Application 61297122 · Jan 21, 2010
Related Publication 20180037464A1 · Feb 8, 2018