Encapsulated solid hydrophilic particles
View Patent ↗A process of forming a population of microcapsules is described comprising a solid hydrophilic core material and a wall material at least partially surrounding the core material. The microcapsule population is formed by providing an anionic, or optionally a cationic, solid hydrophilic core material; providing an oil continuous phase which is low boiling and preferably nonflammable, the oil continuous phase comprising one or more esters with chain length up to about 18 carbons. A mixture is formed by dispersing the solid hydrophilic material in the oil continuous phase. Either an oil soluble or dispersible amine acrylate or methacrylate, along with acid, or alternatively acid acrylate or methacrylate along with base is added. A multifunctional acrylate or methacrylate monomer or oligomer is provided and an initiator. Optionally a surfactant is also added to form the mixture. Emulsification is achieved by subjecting the mixture to high shear agitation and heating the mixture for a time sufficient to enable the acid or amine acrylate or methacrylate and the multifunctional acrylate or methacrylate to form a prepolymer which migrates to the anionic or cationic solid hydrophilic material, thereby forming prepolymers adhered to the hydrophilic core materials. Temperature is held or heating continued for a time sufficient to enable the prepolymer to flow onto and coalesce into a continuous film surface coating on the hydrophilic core material. Heating is carried out or light exposure or both for a time and temperature sufficient to cross link the prepolymers.
1. A process for forming a population of microcapsules comprising a solid hydrophilic core material and a wall material at least partially surrounding the core material, the microcapsule population being formed by:
providing particles of a solid hydrophilic core material;
providing an oil continuous phase which is low boiling, the oil continuous phase comprising one or more hydrocarbons with chain length up to about 18 carbons;
dividing the oil continuous phase into oil 1 and oil 2 ;
dispersing into oil 1 an initiator;
dispersing into oil 2 a multifunctional acrylate or methacrylate monomer or oligomer, and an oil soluble or dispersible amine acrylate or methacrylate, and an acid;
subjecting oil 1 to one or more heating steps;
combining oil 1 and oil 2 ;
subjecting the combined oils to one or more heating steps, forming a cationic wall prepolymer;
forming a mixture by dispersing the solid hydrophilic material into the oil continuous phase and mixing for a sufficient time to allow the wall prepolymer to migrate to and deposit onto the solid hydrophilic core material particles;
optionally adding a surfactant;
holding the temperature for a time sufficient to enable the cationic prepolymer to flow and coalesce into a continuous film surface coating on the hydrophilic core material;
heating the mixture for a time sufficient to cross-link the deposited prepolymer continuous film surface coating on the surface of the particles.
2. The process of forming a population of microcapsules according to claim 1 wherein the acid and amine acrylate or methacrylate have a percent by weight as compared to weight of the wall material of from 0.1 to 25 percent.
3. The process of forming a population of microcapsules according to claim 1 wherein the weight ratio of amine to the multifunctional acrylate or methacrylate is from 0.1:99.9 to 10:90.
4. The process of forming a population of microcapsules according to claim 1 wherein the acid and amine acrylate or methacrylate have a molar proportion of from 1.5/1 to about 1/1.5.
5. The process of forming a population of microcapsules according to claims 1 wherein the solid hydrophilic core material is selected from the group consisting of anionic, cationic, or neutral but polar material.
6. The process of forming a population of microcapsules according to claim 1 wherein the amine acrylate or methacrylate is selected from a monofunctional amine acrylate or a monofunctional amine methacrylate with a nitrogen content of 5% by weight or greater.
7. The process of forming a population of microcapsules according to claim 1 wherein the amine acrylate is selected from the group consisting of alkyl amino acrylate and alkylaminomethacrylate having a nitrogen content of 5% by weight or greater.
8. The process of forming a population of microcapsules according to claim 1 wherein the acid is a carboxylic acid acrylate or carboxylic acid methacrylate having a —COOH content of 20% or greater by weight.
9. A process for forming a population of microcapsules comprising a solid hydrophilic core material and a wall material at least partially surrounding the core material, the microcapsule population being formed by:
providing particles of a solid hydrophilic core material;
providing an oil continuous phase which is low boiling, the oil continuous phase comprising one or more hydrocarbons with chain length up to about 18 carbons;
dividing the oil continuous phase into oil 1 and oil 2 ;
dispersing into oil 1 an initiator;
dispersing into oil 2 a multifunctional acrylate or methacrylate monomer or oligomer, and an oil soluble or dispersible acid acrylate or methacrylate, and a base;
subjecting oil 1 to one or more heating steps;
combining oil 1 and oil 2 ;
subjecting the combined oils to one or more heating steps, forming an anionic wall prepolymer;
forming a mixture by dispersing the solid hydrophilic material into the oil continuous phase and mixing for a time sufficient to allow the wall prepolymer to migrate to and deposit onto a surface of the solid hydrophilic core material particles;
optionally adding a surfactant,
holding the temperature for a time sufficient to enable the anionic prepolymer to flow onto and coalesce into a continuous film surface coating on the hydrophilic core material;
heating the mixture for a time sufficient to cross-link the deposited prepolymer continuous film surface coating on the particles.
10. The process according to claim 1 or 9 wherein the hydrocarbons of the oil continuous phase are esters.
11. The process according to claim 1 or 9 wherein the wall material is selected to be a water permeable, partially water permeable, water soluble, partially water soluble, water fracturable, water disintegratable, semi-porous or an osmotic material.
12. The process according to claims 1 or 9 wherein the oil continuous phase comprises in addition sucrose octyl stearate, a polysaccharide, polyethylene glycol, esters of polyethylene glycol, esterified polyol, saccharide ester, or wax.
13. The process according to claims 1 or 9 wherein a water soluble polymer is added in addition to the multifunctional acrylate.
14. The process of forming a population of microcapsules according to claims 1 or 9 wherein the oil continuous phase is selected from the group consisting of isoamyl benzoate, capric triglyceride, caprylic triglyceride and blends thereof.
15. The process of forming a population of microcapsules according to claim 1 or 9 wherein forming or crosslinking the prepolymers is accomplished by heating the mixture or exposing the mixture to actinic radiation or both.
16. The process of forming a population of microcapsules according to claim 9 wherein the base is selected from the group consisting of monofunctional amine acrylate or a monofunctional amine methacrylate with a nitrogen content of 5% by weight or greater.
17. The process of forming a population of microcapsules according to claim 9 wherein the base is selected from the group consisting of alkyl amino acrylate and alkylaminomethacrylate having a nitrogen content of 5% by weight or greater.
18. The process of forming a population of microcapsules according to claim 9 wherein the acid acrylate or methacrylate is a carboxylic acid acrylate or carboxylic acid methacrylate having a —COOH content of 20% or greater by weight.
19. The process of forming a population of microcapsules according to claim 9 wherein the solid hydrophilic core material is selected from the group consisting of anionic, cationic, or neutral but polar material.
20. The process of forming a population of microcapsules according to claim 9 wherein the base and acid acrylate or methacrylate have a percent by weight as compared to weight of the wall material of from 0.1 to 25 percent.