High concentration encapsulation of water soluble-materials

• US 4,534,783 A
• Filed: 01/03/1984
• Issued: 08/13/1985
• Est. Priority Date: 01/03/1984
• Status: Expired due to Term

• Current Assignee: Monsanto Company (Bayer AG)
• Original Assignee: Monsanto Company (Bayer AG)
• Inventors: Beestman, George B.
• Primary Examiner(s): Dixon, Jr., William R.
• Assistant Examiner(s): Johnson, C.
• Application Number:
  US06/567,585
• Time in Patent Office: 588 Days
• Field of Search: 71/64.11, 71/27, 264/4, 264/4.1, 264/4.7
• US Class Current: 71/27
• CPC Class Codes: A01N 25/28 Microcapsules or nanocapsules
• CPC Class Codes: B01J 13/16 Interfacial polymerisation

Abstract

This invention relates to a process for encapsulation, and particularly to the production of small or minute capsules constituted by a skin or thin wall of polymeric material e.g., polyurea, polyamide, polysulfonamide, polyester, polycarbonate, or polyurethane, which involves first providing an organic liquid (continuous phase liquid) containing an oil soluble alkylated polyvinylpyrrolidone emulsifier A discontinuous (aqueous) phase liquid containing a water-soluble material, which is the material to be encapsulated, plus a first shell wall component; is dispersed in the continuous phase liquid to form a water-in-oil emulsion. The second shell wall component is added to the water-in-oil emulsion whereupon the first shell wall component reacts with the second shell wall component to form a solid polymeric shell wall about the material to be encapsulated. The capsules formed may be directly used as in the form of an organic suspension, i.e., a suspension of microcapsules in the organic liquid.

Claims

1. A process of encapsulating a water-soluble material within a shell wall of polymeric materials which comprises:

(a) providing an organic continuous phase liquid containing an oil soluble alkylated polyvinylpyrrolidone emulsifier;

(b) dispersing in said continuous phase liquid an aqueous discontinuous phase liquid containing a first shell wall component and a water-soluble material dissolved therein to form a dispersion of discontinuous phase droplets throughout the continuous phase;

(c) adding with agitation to said dispersion a second shell wall component, whereby said second shell wall component reacts with said first shell wall component to form a polymeric shell wall about said discontinuous phase droplet;

wherein the concentration of said water-soluble material is from about 480 grams to about 700 grams per liter of composition;

wherein the concentration of said emulsifier is from 0.5% to about 15.0% by weight of said water-soluble material;

wherein the concentration of said first shell wall component is from about 1.5% to about 10.0% by weight of said water soluble material and wherein the concentration of said second shell wall component is from about 3.5% to about 20.0% by weight of said water-soluble material.

2. A process according to claim 1 wherein said polymeric shell wall is selected from the group consisting of polyamide, polyurethane, polysulfonamide, polyurea, polyester and polycarbonate or mixtures thereof.

3. A process according to claim 1 wherein said polymeric shell wall is polyurea.

4. A process according to claim 1 wherein said first shell wall component is a difunctional or polyfunctional reactant which is soluble in said water-soluble material and which is capable of reacting with said second shell wall component to form a polymeric shell wall about said water-soluble material.

5. A process according to claim 1 wherein said second shell wall component is a water-insoluble material which is capable of reacting with said first shell wall component to form a polymeric shell wall about said water-soluble material.

6. A process according to claim 3 wherein said second shell wall component is a polyisocyanate and wherein said first shell wall component is a difunctional or polyfunctional amine.

7. A process according to claim 3 wherein said second shell wall component is a diisocyanate and said first shell wall component is a polyfunctional amine or a mixture of polyfunctional and difunctional amines.

8. A process according to claim 1 wherein the concentration of said water-soluble materal is from about 480 grams to about 600 grams per liter of composition and wherein the concentration of emulsifier is from about 2.0% to about 4.0% by weight of said water-soluble material.

9. A process according to claim 8 wherein said water-soluble material is isopropylamine salt of N-phosphonomethylglycine and said continuous phase liquid is 2-chloro-2'"'"',6'"'"'-diethyl-N-methoxymethyl acetanilide or 2'"'"'-methyl-6'"'"'-ethyl-N-(1-methoxy-prop-2-yl)-2-chloroacetanilide or 2-chloro-N-(ethoxymethyl)-6'"'"'-ethyl-o-acetatoluidide.

10. A process according to claim 1 wherein the average particle size of the microcapsules produced by said process is in the range of from about 1 micron to about 50 microns in diameter.

11. A composition consisting essentially of microcapsules suspended in an organic liquid comprising a water-soluble material contained within an encapsulating wall of polymeric material wherein:

(a) the concentration of said water-soluble material is from about 480 grams to about 700 grams per liter of composition;

(b) wherein said encapsulating wall of polymeric material is the reaction product of a first shell wall component which is a difunctional or polyfunctional reactant that is soluble in said water-soluble material and a second shell wall component which is water insoluble and which is a difunctional or polyfunctional reactant and wherein concentration of first shell wall component is from about 1.5% to about 10.0% relative to the weight of said water-soluble material and wherein the concentration of said second shell wall component is from about 3.5% to about 20.0% relative to the weight of said water-soluble material; and

(c) wherein said organic liquid contains from about 0.5% to about 15% by weight of said water-soluble material of an oil soluble alkylated polyvinylpyrrolidone emulsifier.

12. A composition as described in claim 11 wherein said polymeric shell wall is polyurea.

13. A composition as described in claim 11 wherein the concentration of said water-soluble material is from about 480 grams to about 600 grams per liter of composition, wherein the concentration of said first shell wall component is from about 2.0% to about 5.0% relative to the weight of said water-soluble material, wherein the concentration of said second shell wall component is from about 5.0% to about 10.0% relative to the weight of said water-soluble material, and wherein the concentration of said emulsifier is from about 2.0% to about 6.0% relative to the weight of said water-soluble material.

14. A composition as described in claim 13 wherein the concentration of said first shell wall component is about 4.0% relative to the weight of said water-soluble material, wherein the concentration of said second shell wall component is about 6.5% relative to the weight of said water-soluble material and wherein the concentration of said emulsifier is about 2% relative to the weight of said water-soluble material.

15. A composition as described in claim 11 wherein said water-soluble material is an herbicide, insecticide, plant growth regulant or an herbicidal antidote.

16. A composition as described in claim 15 wherein said organic liquid is alachlor, butachlor, metolachlor, triallate or diallate herbicides.

17. A composition according to claim 11 wherein the organic liquid additionally contains from 1% to 10% of formulation ingredients based on the weight of the total composition.

18. A composition consisting essentially of a mixture of organic liquid and microcapsules containing a water-soluble material, said mixture being produced by a process which comprises the steps of:

(a) providing an organic (continuous) phase liquid containing an oil soluble alkylated polyvinylpyrrolidone emulsifier;

(b) dispersing in said continuous phase, an aqueous (discontinuous) phase consisting essentially of a first shell wall component dissolved in said water-soluble material, to form a dispersion of discontinuous droplets throughout the continuous phase;

(c) adding, with agitation, to said dispersion a second shell wall component whereby said second shell wall component reacts with said first shell wall component to form a polymeric shell wall about said water-soluble material;

(d) wherein the concentration of said water-soluble material is from about 480 grams to about 700 grams per liter of said composition, wherein the concentration of first shell wall component is from about 1.5% to about 10.0% by weight of said water-soluble material, wherein the concentration of said second shell wall component is from about 3.5% to about 20.0% by weight of said water-soluble material, and wherein the concentration of said emulsifier is from about 0.5% to about 15% by weight of said water-soluble material.

19. A composition as described in claim 18 wherein said water-soluble material is the isopropylamine salt of N-phosphonomethylglycine, wherein said continuous phase liquid is 2-chloro-2'"'"',6'"'"'-diethyl-N-methoxymethyl acetanilide and wherein said polymeric shell wall is polyurea.