Methods of making capsules

Patent metadata

Field	Value
Publication number	US-11628413-B2
Application number	US-202016851194-A
Country	US
Kind code	B2
Filing date	Apr 17, 2020
Priority date	Apr 17, 2019
Publication date	Apr 18, 2023
Grant date	Apr 18, 2023

Abstract

A method of making a population of capsules, the capsules can include a core including a benefit agent and a shell surrounding the core, wherein the shell can include a first shell component.

First claim

What is claimed is:

1. A method of making capsules comprising a substantially inorganic shell surrounding an oil-based core, comprising:
admixing an oil phase comprising a benefit agent and a precursor, with an aqueous phase comprising water and inorganic nanoparticles, wherein the precursor comprises at least one compound of Formula (I):
(M v O z Y n ) w   (Formula I)

where M is at least one of silicon, titanium or aluminum,
v is the valence number of M and is 3 or 4,
z is from 0.5 to 1.6,
each Y is independently selected from —OH, —OR2, halo,

—NH2, —NHR2, —N(R2)2, and

wherein R2 is a C1 to C20 alkyl, C1 to C20 alkylene, C6 to C22 aryl, or a 5-12 membered heteroaryl comprising from 1 to 3 ring heteroatoms selected from O, N, and S,
R3 is a H, C1 to C20 alkyl, C1 to C20 alkylene, C6 to C22 aryl, or a 5-12 membered heteroaryl comprising from 1 to 3 ring heteroatoms selected from O, N, and S,
n is from 0.7 to (v-1), and
w is from 2 to 2000;

emulsifying the admixture of oil phase and aqueous phase under conditions sufficient to disperse droplets of oil phase in the aqueous phase, wherein the nanoparticles self-assemble around the oil droplets and are interposed at an interface of the aqueous phase and the oil phase, and the precursor from the oil phase hydrolyzes and condensates at the interface between the oil phase and aqueous phase;
curing the emulsion under conditions to solidify the hydrolyzed and condensed precursor, thereby forming a first shell component comprising the condensed precursor and nanoparticles around the oil droplets and forming the capsules having oil phase as the core;
Admixing the capsules with a second shell component solution comprising a second shell component precursor under conditions sufficient to obtain capsules with an inorganic second shell component, thereby forming capsules with both a first and second shell component.

2. The method according to claim 1 , wherein the benefit agent comprises at least one of chromogens and dyes, perfume compositions, perfume raw materials, lubricants, silicone oils, waxes, hydrocarbons, higher fatty acids, essential oils, lipids, skin coolants, vitamins, sunscreens, antioxidants, catalysts, malodor reducing agents, odor-controlling materials, softening agents, insect and moth repelling agents, colorants, pigments, pharmaceuticals, pharmaceutical oils, adhesives, bodying agents, drape and form control agents, smoothness agents, wrinkle control agents, sanitization agents, disinfecting agents, germ control agents, mold control agents, mildew control agents, antiviral agents, drying agents, stain resistance agents, soil release agents, fabric refreshing agents and freshness extending agents, chlorine bleach odor control agents, dye fixatives, color maintenance agents, color restoration/rejuvenation agents, anti-fading agents, anti-abrasion agents, wear resistance agents, fabric integrity agents, anti-wear agents, anti-pilling agents, defoamers, anti-foaming agents, UV protection agents, sun fade inhibitors, anti-allergenic agents, fabric comfort agents, shrinkage resistance agents, stretch resistance agents, stretch recovery agents, skin care agents and natural actives, dyes, phase change materials, fertilizers, nutrients, or herbicides.

3. The method according to claim 2 , wherein in the benefit agent is a perfume composition.

4. The method according to claim 2 , wherein the oil phase further comprises a core modifier.

5. The method according to claim 1 , wherein the aqueous phase pH is between about 1 to about 14.

6. The method according to claim 1 , wherein the aqueous phase pH is between about 1 to about 7.

7. The method according to claim 1 , wherein the inorganic nanoparticles comprise at least one of metal nanoparticles, mineral nanoparticles, metal-oxide nanoparticles or semi-metal oxide nanoparticles.

8. The method according to claim 1 , wherein the inorganic nanoparticles comprise at least one of SiO 2 , TiO 2 , Al 2 O 3 , Fe 2 O 3 , Fe 3 O 4 , CaCO 3 , clay, silver, gold, or copper.

9. The method of claim 1 , wherein the inorganic nanoparticles comprise at least one of SiO 2 , Al 2 O 3 , CaCO 3 or clay.

10. The method according to claim 1 , wherein the second shell component precursor comprises at least one of TEOS, TMOS, silicate salt solutions, silicon tetralkoxide solutions, iron sulfate salt, iron nitrate salt, titanium alkoxide solutions, aluminum trialkoxide solutions, zinc dialkoxide solutions, zirconium alkoxide solutions, calcium salt solutions, carbonate salt solutions, gold salt solutions, copper salt solutions, iron salt solutions ions, or nickel salt solutions.

11. The method according to claim 10 , wherein the second shell component precursor comprises at least one of TEOS, silicate salts, calcium salts or carbonate salts.

12. The method according to claim 1 , wherein the precursors of Formula (I) comprise: M is Silicon and Y is Ethoxy.

13. The method according to claim 1 , wherein the oil phase further comprises at least one of TMOS, TEOS or TBOS.

14. The method of claim 1 wherein the compound of formula (I) has a Polystyrene equivalent Weight Average Molecular Weight (Mw) of from about 700 Da to about 30,000 Da.

15. The method of claim 14 , wherein the compound of Formula (I) has a degree of branching of about 0.2 to about 0.6.

16. The method according to claim 15 , wherein for precursors of Formula (I): M is Silicon, Y is OR, and R is at least one of methyl, ethyl, propyl or butyl.

17. The method of claim 1 , wherein the compound of Formula (I) has a polydispersity index of about 1 to about 20.

18. The method of claim 1 , wherein the oil phase comprises between about 10% to about 60% by weight of precursor.

19. A method of making capsules comprising a substantially inorganic shell surrounding an aqueous core, comprising:
admixing an oil phase comprising a precursor with an aqueous phase comprising water and a benefit agent, wherein at least one of the oil phase or aqueous phase comprises inorganic nanoparticles, wherein the precursor comprises at least one compound of Formula (I):
(M v O z Y n ) w   (Formula I)

where M is at least one of silicon, titanium or aluminum,
v is the valence number of M and is 3 or 4,
z is from 0.5 to 1.6,
each Y is independently selected from —OH, —OR2, halo,

NH2, —NHR2, —N(R2)2, and

wherein R2 is a C1 to C20 alkyl, C1 to C20 alkylene, C6 to C22 aryl, or a 5-12 membered heteroaryl comprising from 1 to 3 ring heteroatoms selected from O, N, and S,
R3 is a H, C1 to C20 alkyl, C1 to C20 alkylene, C6 to C22 aryl, or a 5-12 membered heteroaryl comprising from 1 to 3 ring heteroatoms selected from O, N, and S,
n is from 0.7 to (v-1), and
w is from 2 to 2000;

emulsifying the admixture of the oil phase and aqueous phase under conditions sufficient to disperse droplets of aqueous phase in the oil phase, wherein the nanoparticles self-assemble around the aqueous droplets and are interposed at an interface of the aqueous phase and the oil phase, and the precursor hydrolyzes and condensates at the interface between the oil phase and a

Assignees

• Procter & Gamble

Inventors

• Cardoso Mariana B T
• Barros Andre Martim
• De Nies Peter
• Verstraete Pierre Daniel
• Wong Valerie
• Smith Steven Daryl
• Zhang Zhibing
• Preece Jon A

Classifications

• A61K8/11

  Encapsulated compositions · CPC title

• D06M13/507

  Organic silicon compounds without carbon-silicon bond · CPC title

• B01J13/10 Primary

  Complex coacervation, i.e. interaction of oppositely charged particles · CPC title

• C11D17/0039

  Coated compositions or coated components in the compositions, (micro)capsules · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title