Patent ID: 11904288
Assignee: TRUCAPSOL LLC
Field: Chemical engineering (Chemistry)
Classification: CPC B  A  C  F | IPC A  B

Claim 19:
20. A method for preparing the composition of claim 1, said method comprising steps (A)(1)-(A)(9), steps (B)(1)-(B)(9) or steps (C)(1)-(C)(11) as follow:
(A)(1) preparing an oil phase comprising: (a) the at least one hydrophobic active ingredient, (b) at least one isocyanate, (c) at least one epoxy, (d) at least one polyol, (e) at least one plasticizer, (f) at least one inorganic solid particle, and optionally (g) a polysaccharide;
(A)(2) reacting the at least one isocyanate with the at least one polyol;
(A)(3) preparing an aqueous phase comprising an emulsifier;
(A)(4) combining the oil phase and the aqueous phase to emulsify the at least one hydrophobic active ingredient to provide an aqueous suspension of the at least one hydrophobic active ingredient;
(A)(5) adding an amine moiety containing material to the aqueous suspension to react with the at least one epoxy and optionally react with the at least one isocyanate for at least 30 minutes at a temperature of 50° C. to provide the wall;
(A)(6) increasing the temperature of the aqueous suspension to 60° C. and reacting for 2 to 5 hours;
(A)(7) adding a process aid to the aqueous suspension;
(A)(8) cooling the temperature of the aqueous suspension to 20-30° C.; and
(A)(9) optionally adding structuring agents to the suspension of the microcapsules to homogeneously suspend the microcapsules in an aqueous dispersion; or
(B)(1) preparing an oil phase comprising the at least one hydrophobic active ingredient, at least one isocyanate, at least one epoxy, at least one plasticizer, at least one organofunctional silane, and optionally an inorganic solid particle;
(B)(2) preparing an aqueous phase comprising a hydrolyzed protein by dissolving a protein in water, adding sodium hydroxide to achieve a pH of at least 10.5 and reacting for at least 16 hours at 40° C. to hydrolyze the protein, then adjusting the pH to 6.5 and adding an emulsifier;
(B)(3) combining the oil phase and the aqueous phase to emulsify the at least one hydrophobic active ingredient, at a solubilizing temperature to maintain a solubility of the hydrolyzed protein, and to provide an aqueous suspension of the at least one hydrophobic active ingredient;
(B)(4) adjusting the pH of the aqueous suspension to 8.5 over a period of 1 hour to allow the hydrolyzed protein to react with at least one of the at least one epoxy and the at least one organofunctional silane, and optionally react with the at least one isocyanate at 40° C. to provide the wall;
(B)(5) increasing the temperature of the aqueous suspension to 60° C., maintaining the pH above 8.5, and allowing contents of the aqueous suspension to react for at least 5 hours;
(B)(6) adding a process aid to the aqueous suspension;
(B)(7) cooling the temperature of the aqueous suspension to 20-30° C., and optionally adding a water dispersible protein;
(B)(8) optionally adding a water soluble dialdehyde and agitating for at least 2 hours; and
(B)(9) cooling the temperature of the aqueous suspension to 20-30° C. and optionally adding structuring agents to the aqueous suspension to homogeneously suspend the microcapsules in an aqueous dispersion; or
(C)(1) preparing an oil phase comprising the at least one hydrophobic active ingredient, at least one isocyanate, at least one epoxy, at least one oil soluble dialdehyde and at least one plasticizer;
(C)(2) preparing an aqueous phase comprising an emulsifier;
(C)(3) combining the oil phase and the aqueous phase to emulsify the at least one hydrophobic active ingredient to provide an aqueous suspension of the at least one hydrophobic active ingredient;
(C)(4) adding an amine moiety containing material to the aqueous suspension to react with at least one of the at least one epoxy and the at least one oil soluble dialdehyde, and optionally react with the at least one isocyanate for at least 30 minutes at a temperature of 20-30° C. to provide the wall;
(C)(5) adjusting a pH of the aqueous suspension to 8.5 over a period of 1 hour to allow the amine moiety containing material to further react with at least one of the at least one epoxy and the at least one oil soluble dialdehyde and optionally react with the at least one isocyanate at 40° C. to provide the wall;
(C)(6) raising the temperature of the aqueous suspension to 60° C., maintaining the pH above 8.5, and allowing contents of the aqueous suspension to react for at least 5 hours;
(C)(7) adding a process aid;
(C)(8) cooling the temperature of the aqueous suspension to 20-30° C., and optionally adding a water dispersible protein;
(C)(9) optionally adding a water soluble dialdehyde and agitating for at least 2 hours;
(C)(10) optionally adding colloidal silica to the aqueous suspension and spray drying the aqueous suspension using a co-current spray dryer at an inlet air temperature of 177-196° C. (350-385° F.), an outlet air temperature of 85-93° C. (185-200° F.), and an air pressure of 65 psig for a 2-fluid atomizer nozzle; and
(C)(11) cooling the temperature of the aqueous suspension to 20-30° C. and optionally adding structuring agents to the aqueous suspension to homogeneously suspend the microcapsules in an aqueous dispersion.