Process for Preparing a High Stability Microcapsule Product and Method for Using Same

Abstract

The present invention is directed to a process for preparing a capsule product through the increase in the polymerization cure temperature and cure time during the capsule-making process. The microcapsule products prepared according the process of the present invention exhibit enhanced retention of active materials in consumer products which promote instability.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

Figure I illustrates the heating rate used in Example 11 from ambient temperature to the cure temperature.

Figure II illustrates the first heating pattern used in Example 12 wherein the alternate cycling method mimics the use of a heat exchanger to raise the temperature of the reaction to a desired target cure temperature.

Figure III illustrated the second heating pattern used in Example 12 wherein it mimics cycling through a heat exchanger.

Claims

1. A process for preparing a microcapsule product which comprises curing at a temperature above 90° C. a crosslinked network of polymers containing an active material to provide a microcapsule product which is capable of retaining the active material in consumer products, the consumer products comprising surfactants, alcohols, volatile silicones and mixtures thereof.

2. The process of claim 1 wherein the consumer product comprises surfactants.

3. The process of claim 1 wherein the crosslinked network of polymers containing an active material is cured for greater than 1 hour.

4. The process of claim 1 wherein the crosslinked network of polymers containing an active material is cured for greater than 2 hours.

5. The process of claim 1 wherein the crosslinked network of polymers containing an active material is cured at a temperature above 110° C.

6. The process of claim 1 wherein the crosslinked network of polymers containing an active material is cured at a temperature above 120° C.

7. The process of claim 1 wherein the active material is selected from the group consisting of fragrances, flavoring agents, fungicide, brighteners, antistatic agents, wrinkle control agents, fabric softener actives, hard surface cleaning actives, skin and/or hair conditioning agents, malodour counteractants, antimicrobial actives, UV protection agents, insect repellents, animal/vermin repellents, flame retardants, and mixtures thereof.

8. The process of claim 7 wherein the active material is a liquid thereby providing a liquid core to the microcapsule product.

9. The process of claim 7 wherein said active material is a fragrance.

10. The process of claim 9 wherein the fragrance components has a clogP less than 4.0.

11. The process of claim 10 wherein the microcapsule product retains greater than 40% of the fragrance after a four week period in a surfactant containing consumer products.

12. The process of claim 9 wherein the fragrance has a clog P less than 3.0.

13. The process of claim 12 wherein the microcapsule product retains greater 40% of the fragrance after a four week period in a surfactant containing consumer products.

14. The process of claim 9 wherein the fragrance components has a clogP greater than 4.0.

15. The process of claim 14 wherein the microcapsule product retains greater 40% of the fragrance after a four week period in a surfactant containing consumer products.

16. The process of claim 1 wherein the encapsulating polymer is selected from a vinyl polymer, an acrylate polymer, melamine-formaldehyde, urea formaldehyde, amine-containing polymer, amine-generating polymer, aminoplasts, aldehydes, dialdehydes, active oxygen, poly-substituted carboxylic acids and derivatives, inorganic crosslinkers, organics capable of forming azo, azoxy and hydrazo bonds, lactones and lactams, thionyl chloride, phosgene, tannin/tannic acid, polyphenols, free radical crosslinkers, sodium persulfate, azoisobutylnitrile (AIBN) and mixtures thereof.

17. The process of claim 1 wherein the microcapsule product is further coated by a cationic polymer.

18. The process of claim 17 wherein the cationic polymer is selected from polysaccharides, cationically modified starch and cationically modified guar, polysiloxanes, poly diallyl dimethyl ammonium halides, copolymers of poly diallyl dimethyl ammonium chloride and vinyl pyrrolidone, acrylamides, imidazoles, imidazolinium halides, imidazolium halides and mixtures.

19. The method of claim 18 wherein the cationic polymer is selected from a cationically modified starch, cationically modified guar and mixtures thereof.

20. A method of imparting an olfactory effective amount of a fragrance into a consumer product comprising incorporating at least 0.25 weight % of the capsules of claim 1 into a consumer product.

21. The method of claim 20 wherein the consumer product is selected from the group consisting of laundry detergent, fabric softeners, bleach products, tumble dryer sheets, liquid dish detergents, automatic dish detergents, hair shampoos, hair conditioners, toothpastes, mouthwash, oral care products, liquid soaps, body wash, lotions, creams, hair gels, anti-perspirants, deodorants, shaving products, colognes, bodywash, automatic dishwashing compositions, foodstuffs, beverages and mixtures thereof.

22. A microcapsule product produced according to the process of claim 1.

23. A consumer product selected from the group consisting of laundry detergent, fabric softeners, bleach products, tumble dryer sheets, liquid dish detergents, automatic dish detergents, hair shampoos, hair conditioners, toothpastes, mouthwash, oral care products, liquid soaps, body wash, lotions, creams, hair gels, anti-perspirants, deodorants, shaving products, colognes, bodywash, and automatic dishwashing compositions, foodstuffs, beverages and mixtures thereof comprising the microcapsule product according to the process of claim 1.

24. A process for preparing a high stability capsule product which comprises: reacting polymers to form a crosslinked network of polymers;admixing an active material and an optional functional additive to the reactant mixture;encapsulating the active material with the crosslinked network of polymers to form a polymer encapsulated material;curing the polymer encapsulated material for greater than 1 hour at a curing temperature greater than 90° C. to provide a microcapsule product.

25. The process of claim 24 wherein the active material is selected from the group consisting of fragrances, flavoring agents, fungicide, brighteners, antistatic agents, wrinkle control agents, fabric softener actives, hard surface cleaning actives, skin and/or hair conditioning agents, malodour counteractants, antimicrobial actives, UV protection agents, insect repellents, animal/vermin repellents, flame retardants, and mixtures thereof.

26. The process of claim 25 wherein said active material is a fragrance.

27. The process of claim 24 wherein the microcapsule product is cured for greater than 2 hours.

28. The process of claim 24 wherein the curing temperature is greater than 110° C.

29. The process of claim 24 wherein the curing temperature is greater than 120° C.

30. The process of claim 24 wherein the crosslinked network of polymers is selected from a vinyl polymer, an acrylate polymer, melamine-formaldehyde, urea formaldehyde, amine-containing polymer, amine-generating polymer, aminoplasts, aldehydes, dialdehydes, active oxygen, poly-substituted carboxylic acids and derivatives, inorganic crosslinkers, organics capable of forming azo, azoxy and hydrazo bonds, lactones and lactams, thionyl chloride, phosgene, tannin/tannic acid, polyphenols, free radical crosslinkers, sodium persulfate, azoisobutylnitrile (AIBN) and mixtures thereof.

31. The process of claim 30 wherein the crosslinked network of polymers comprises a melamine-formaldehyde:acrylamide-acrylic acid copolymer wherein the mole ratio is in the range of from 9:1 to 1:9.

32. The process of claim 31 wherein the mole ratio of melamine-formaldehyde:acrylamide-acrylic acid copolymer is in the range of from 5:1 to 1:5.

33. The process of claim 31 wherein the mole ratio of melamine-formaldehyde:acrylamide-acrylic acid copolymer is in the range of from 2:1 to 1:2.

34. The process of claim 24 wherein the optional functional additive is a cationic polymer as the capsule deposition aid selected from polysaccharides, cationically modified starch and cationically modified guar, polysiloxanes, poly diallyl dimethyl ammonium halides, copolymers of poly diallyl dimethyl ammonium chloride and vinyl pyrrolidone, acrylamides, imidazoles, imidazolinium halides and imidazolium halides and poly vinyl amine and its copolymers with N-vinyl formamide, cationic amino resins, cationic urea resins, hydrophobic quaternary amines and mixtures thereof.

35. A process for preparing a high stability capsule product which comprises: reacting polymers to form a crosslinked network of polymers;admixing an active material to the reactant mixture;encapsulating the active material with the crosslinked network of polymers to form a polymer encapsulated material;raising the temperature of the reactant mixture to a target cure temperature of greater than about 90° C. over a period of time less than about sixty minutes; andmaintaining a temperature of greater than about 90° C. over a period of time at least up to about sixty minutes to provide a microcapsule product.

36. The process of claim 35 wherein the heating profile is at least up to about 2° C. a minute over a period of less than about sixty minutes.

37. The process of claim 35 wherein the heating profile is at least up to about 5° C. a minute over a period of less than about sixty minutes.

38. The process of claim 35 wherein the heating profile is at least up to about 8° C. a minute over a period of less than about sixty minutes.

39. The process of claim 38 wherein the heating profile is at least up to about 8° C. a minute over a period of less than about thirty minutes.

40. The process of claim 35 wherein the heating profile is up to about 10° C. a minute over a period of less than about sixty minutes.

41. The process of claim 40 wherein the heating profile is up to about 10° C. a minute over a period of less than about thirty minutes.

42. The process of claim 35 wherein the microcapsule product is cured for a period of time up to about 2 hours.

43. The process of claim 35 wherein the microcapsule product is cured for a period of time greater than about 2 hours.

44. The process of claim 35 wherein the curing temperature is greater than about 110° C.

45. The process of claim 35 wherein the curing temperature is greater than about 120° C.

46. The process of claim 35 wherein the microcapsule product contains greater than about 10 weight % of water.

47. The process of claim 35 wherein the microcapsule product contains greater than about 30 weight % of water.

48. The process of claim 35 wherein the microcapsule product contains greater than about 50 weight % of water.

49. The process of claim 35 wherein the microcapsule product is spray-dried.

50. The process of claim 35 wherein the active material is selected from the group consisting of fragrances, flavoring agents, fungicide, brighteners, antistatic agents, wrinkle control agents, fabric softener actives, hard surface cleaning actives, skin and/or hair conditioning agents, malodour counteractants, antimicrobial actives, UV protection agents, insect repellents, animal/vermin repellents, flame retardants, and mixtures thereof.

51. The process of claim 50 wherein the active material is a liquid thereby providing a liquid core to the microcapsule product.

52. The process of claim 50 wherein said active material is a fragrance.

53. The process of claim 52 wherein the fragrance components has a clog P less than about 4.0.

54. The process of claim 52 wherein the microcapsule product retains greater than about 40% of the fragrance after a four week period in a surfactant containing consumer product.

55. The process of claim 52 wherein the fragrance components has a clog P less than about 3.0.

56. The process of claim 55 wherein the microcapsule product retains greater than about 40% of the fragrance after a four week period in a surfactant containing consumer product.

57. The process of claim 52 wherein the fragrance components has a clog P greater than about 4.0.

58. The process of claim 57 wherein the microcapsule product retains greater than about 40% of the fragrance after a four week period in a surfactant containing consumer product.

59. The process of claim 35 wherein the crosslinked network of polymers is selected from a vinyl polymer, an acrylate polymer, melamine-formaldehyde, urea formaldehyde, amine-containing polymer, amine-generating polymer, aminoplasts, aldehydes, dialdehydes, active oxygen, poly-substituted carboxylic acids and derivatives, inorganic crosslinkers, organics capable of forming azo, azoxy and hydrazo bonds, lactones and lactams, thionyl chloride, phosgene, tannin/tannic acid, polyphenols, free radical crosslinkers, sodium persulfate, azoisobutylnitrile (AIBN) and mixtures thereof.

60. The process of claim 59 wherein the crosslinked network of polymers comprises a melamine-formaldehyde:acrylamide-acrylic acrylic acid copolymer wherein the mole ratio is in the range of from about 9:1 to about 1:9.

61. The process of claim 59 wherein the mole ratio of melamine-formaldehyde:acrylamide-acrylic acid copolymer is in the range of from about 5:1 to about 1:5.

62. The process of claim 59 wherein the mole ratio of melamine-formaldehyde:acrylamide-acrylic acid copolymer is in the range of from about 2:1 to about 1:2.

63. The process of claim 35 wherein the optional functional additive is a cationic polymer selected from polysaccharides, cationically modified starch and cationically modified guar, polysiloxanes, poly diallyl dimethyl ammonium halides, copolymers of poly diallyl dimethyl ammonium chloride and vinyl pyrrolidone, acrylamides, imidazoles, imidazolinium halides and imidazolium halides and poly vinyl amine and its copolymers with N-vinyl formamide, cationic amino resins, cationic urea resins, hydrophobic quaternary amines and mixtures thereof.

64. The process of claim 35 wherein the microcapsule product is further coated by a cationic polymer.

65. The process of claim 64 wherein the cationic polymer is selected from polysaccharides, cationically modified starch and cationically modified guar, polysiloxanes, poly diallyl dimethyl ammonium halides, copolymers of poly diallyl dimethyl ammonium chloride and vinyl pyrrolidone, acrylamides, imidazoles, imidazolinium halides, imidazolium halides and mixtures.

66. The process of claim 65 wherein the cationic polymer is selected from a cationically modified starch, cationically modified guar and mixtures thereof.

67. A method of imparting an olfactory effective amount of a fragrance into a consumer product comprising incorporating at least about 0.25 weight % of the capsules of claim 35 into a consumer product.

68. The method of claim 67 wherein the consumer product is selected from the group consisting of laundry detergent, fabric softeners, bleach products, tumble dryer sheets, liquid dish detergents, automatic dish detergents, hair shampoos, hair conditioners, toothpastes, mouthwash, oral care products, liquid soaps, body wash, lotions, creams, hair gels, anti-perspirants, deodorants, shaving products, colognes, bodywash, automatic dishwashing compositions, foodstuffs, beverages and mixtures thereof.

69. A microcapsule product produced according to the process of claim 35.

70. A consumer product selected from the group consisting of laundry detergent, fabric softeners, bleach products, tumble dryer sheets, liquid dish detergents, automatic dish detergents, hair shampoos, hair conditioners, toothpastes, mouthwash, oral care products, liquid soaps, body wash, lotions, creams, hair gels, anti-perspirants, deodorants, shaving products, colognes, bodywash, and automatic dishwashing compositions, foodstuffs, beverages and mixtures thereof comprising the microcapsule product according to the process of claim 35.