Storage-stable product systems for premix formulations

• US 9,199,211 B2
• Filed: 02/02/2009
• Issued: 12/01/2015
• Est. Priority Date: 02/13/2008
• Status: Active Grant

• Current Assignee: Evonik Operations GmbH (Rag-Stiftung)
• Original Assignee: Evonik Degussa GmbH
• Inventors: Tschernjaew, Juri, Stenner, Patrik, Pisula, Wojciech, Drexel, Claus-Peter, Gottheis, Martina, Seitz, Tanja, Hitzler, Martin G.
• Primary Examiner(s): ANTHONY, JOSEPH DAVID
• Application Number:
  US12/867,493
• Publication Number:
  US 20110037021A1
• Time in Patent Office: 2,493 Days
• Field of Search: 252/182.13, 106/15.05, 264/4, 523/122, 424/49, 424/50, 424/51, 424/403
• US Class Current: 1/1
• CPC Class Codes: B01J 2/006 Coating of the granules without description of the process or the device by which the granules are obtained to prevent the granules sticking together B01J2/30
• CPC Class Codes: B01J 2/06 in a liquid medium

Abstract

The present invention relates to storage-stable product systems having high latency and good mechanical stability, which are suitable, inter alia, for premix formulations. Furthermore, the present invention relates to a method for producing the formulations according to the invention and the use thereof.

Claims

1. A product system comprising

at least one porous carrier, wherein the porous carrier is inorganic, organic, or a combination thereof,

at least one active ingredient which is introduced into the porous carrier, and

at least one protective substance, wherein at least part of the total amount of the at least one protective substance present in the product system is introduced in the pores of the porous carrier, wherein the at least one protective substance can be deactivated in a targeted manner by one or more of an action of pressure waves on the product system, an action of UV radiation on the product system, increasing temperature of the product system, a pH change, and an action of at least one enzyme on the protective substance, wherein when the porous carrier is in an aqueous medium, the at least one protective substance does not allow any of the at least one active ingredient to be released prior to deactivation of the at least one protective substance,

wherein at least 80% by weight of the at least one active ingredient is released within 1 hour when the at least one protective substance is deactivated by an action of pressure waves on the product system,

wherein at least 80% by weight of the at least one active ingredient is released within 12 hours when the at least one protective substance is deactivated by an action of UV radiation on the product system,

wherein at least 60% by weight of the at least one active ingredient is released within 1 hour when the at least one protective substance is deactivated by increasing temperature of the product system,

wherein at least 70% by weight of the at least one active ingredient is released within 8 hours when the at least one protective substance is deactivated by a pH change,

wherein at least 80% by weight of the at least one active ingredient is released within 24 hours when the at least one protective substance is deactivated by an action of at least one enzyme on the protective substance,

and wherein, detected by investigating the outermost atomic layer of the product system by means of XPS, at least part of the outermost surface of the product system is formed by the porous carrier.

2. The product system as claimed in claim 1, wherein at least 10% of the surface of the product system, detected by investigating the outermost atomic layer of the product system by means of XPS, is not formed by the at least one active ingredient, the at least one protective substance, or a combination thereof.

3. The product system as claimed in claim 1, wherein the protective substance comprises at least one compound which is soluble in a solvent in which the at least one active ingredient is not soluble.

4. The product system as claimed in claim 1, wherein the at least one active ingredient is soluble in a polar solvent and the protective substance is insoluble in water, soluble in a nonpolar solvent, or a combination thereof, or wherein the at least one active ingredient is soluble in a nonpolar solvent and the protective substance is insoluble in a nonpolar solvent, soluble in a polar solvent, soluble in water, or a combination thereof.

5. The product system as claimed in claim 4, wherein the nonpolar solvent is an aromatic hydrocarbon, an alkane or a cycloalkane.

6. The product system as claimed in claim 1, wherein the weight ratio of the protective substance to the at least one active ingredient is in the range from 10:

1 to 1;

10.

7. The product system as claimed in claim 1, wherein the loading of the porous carrier with the at least one active ingredient is 0% by weight to 90% by weight, based on the DBP absorption of the porous carrier.

8. The product system as claimed in claim 1, wherein the loading of the porous carrier with the protective substance is at least 10% by weight, based on the DBP absorption of the porous carrier.

9. The product system as claimed in claim 7, wherein the unladen porous carrier has a DBP absorption of at least 180 g/100 g.

10. The product system as claimed in claim 1, wherein the product system is particulate.

11. The product system as claimed in claim 10, wherein the particles have an average particle size d50 in the range from 5 μ

m to 1000 μ

m.

12. A product system comprising

at least one porous carrier, wherein the porous carrier is inorganic, organic, or a combination thereof,

at least one active ingredient which is introduced into the porous carrier, and

at least one further substance, wherein at least part of the total amount of the at least one further substance present in the product system is incorporated in the pores of the porous carrier,

wherein the at least one further substance forms a protection system capable of being deactivated as a result of an input of energy, chemical conversion, breakup of the protection system, or a combination thereof, wherein when the porous carrier is in an aqueous medium, the protection system does not allow any of the at least one active ingredient to be released prior to deactivation of the protection system, and wherein at least 50% by weight of the at least one active ingredient is spontaneously released after deactivation of the protection system;

and wherein, detected by investigating the outermost atomic layer of the product system by means of XPS, at least part of the outermost surface of the product system is formed by the porous carrier.

13. The product system as claimed in claim 12, wherein the protection system is designed such that an input of energy through pressure waves, irradiation with UV light, increasing the temperature, or a combination thereof triggers the deactivation of the protection system.

14. The product system as claimed in claim 13, wherein an input of energy through pressure waves triggers the release of at least 80% by weight of the at least one active ingredient within 1 h.

15. The product system as claimed in claim 13, wherein irradiation with UV light triggers the release of at least 80% by weight of the at least one active ingredient within 12 h.

16. The product system as claimed in claim 13, wherein increasing the temperature triggers the release of at least 60% by weight of the at least one active ingredient within 60 min.

17. The product system as claimed in claim 12, wherein the protection system is designed such that a chemical conversion, pH shift, action of at least one enzyme, or a combination thereof triggers the deactivation of the protection system.

18. The product system as claimed in claim 17, wherein a pH shift triggers the release of at least 70% of the at least one active ingredient within 8 h.

19. The product system as claimed in claim 17, wherein the action of at least one enzyme triggers the release of at least 80% by weight of the at least one active ingredient within 24 h.

20. The product system as claimed in claim 12, wherein contacting the protection system with a suitable solvent triggers the release of at least 80% by weight of the at least one active ingredient over the course of 24 hours.

21. The product system as claimed in claim 12, wherein at least 80% by weight of the at least one active ingredient is released in a diffusion-controlled manner within 20 days after deactivation of the protection system.

22. A method for producing a product system as claimed in claim 12, wherein at least one active ingredient is introduced into a porous carrier and a protection system is produced.

23. The method as claimed in claim 22, comprising the following steps:

a) introduction as initial charge of at least one porous carrier in a solids mixing unit

b) optional evacuation of the solids mixing unit

c) optional preimpregnation of the porous carrier with at least one protective substance until at most 50% by weight of the DBP absorption value is achieved

d) addition of at least one active ingredient to the solids mixing unit

e) impregnation of the porous carrier with the at least one active ingredient

f) optional inhibition of the at least one active ingredient adhering to the outer particle surface of the porous carrier, washing, drying, or a combination thereof

g) addition of at least one protective substance

h) impregnation of the porous carrier with at least one protective substance

i) optional washing, drying, or a combination thereof

j) optional reactive inhibition of the at least one active ingredient adhering to the external particle surface of the porous carrier, washing, drying, or a combination thereof.

24. The method as claimed in claim 23, wherein steps b) to e), steps g) to h), or a combination thereof, are carried out several times, where, in the case of the repetition of steps d) and e), steps g) and h), or a combination thereof, in each case identical or different active ingredients, protective substances, or a combination thereof, are used.

25. The method as claimed in claim 23, wherein the porous carrier and the at least one active ingredient are mixed before being introduced into the solids mixing unit.

26. The method as claimed in claim 23, wherein a pretreatment of the porous carrier with surfactants or silanes takes place before the at least one active ingredient, the at least one protective substance, or a combination thereof are added.

27. The method as claimed in claim 26, wherein, in stage c), a mixture of the at least one active ingredient and the at least one protective substance is added.

28. The method as claimed in claim 22, wherein the added amount of the at least one protective substance in step g) is regulated such that the total amount of the at least one active ingredient and the at least one protective substance which are added during the production of the product system corresponds to 50% by weight to 100% by weight of the DBP absorption value of the porous carrier.

29. The method as claimed in claim 22, wherein the added amount of the at least one protective substance in step g) is regulated such that the total amount of the at least one active ingredient and the at least one protective substance which are added during the production of the product system is greater than the total pore volume of the porous carrier and that the excess of the at least one protective substance is absorbed by adding porous carrier, porous carrier laden with the at least one active ingredient, or a combination thereof.

30. The method as claimed in claim 22, wherein the method is performed at a mixing intensity and a metering which are matched to one another such that the pourability at the end of the method is ensured.

31. The method as claimed in claim 22, wherein the method further comprises stirring elements that are selected such that no abrasion takes place as a result of shear stress.

32. A method of producing an article selected from the group consisting of foods, feeds, medicaments, products for the land and forestry, cosmetics, components for coating formulations, and adhesive formulations or components for sports equipment and sports clothing, comprising incorporating a product system as claimed in claim 12 into the article.