US4956129A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Microencapsulation process
Assignee: Syngenta Crop Protection LLC
•
Filing: 1988-02-01
•
Granted: 1990-09-11
•
Expires: 2008-02-01
Abstract
Abstract A process is disclosed for the microencapsulation of a substantially water-insoluble liquid material within a porous shell to effect a slow rate of release of said material through said shell which comprises (a) providing an organic solution comprising said material and an etherified urea-formaldehyde prepolymer dissolved therein which from about 50% to about 98% of the methylol groups of said prepolymer have been etherified with a C 4 -C 10 alcohol; (b) creating an emulsion of said organic solution in an continuous phase aqueous solution comprising water and a surfaceactive agent, wherein said emulsion comprises discrete droplets of said organic solution dispersed in said continuous phase aqueous solution, there being formed thereby an interface between the discrete droplets of organic solution and the surrounding continuous phase aqueous solution; and (c) causing in situ self-condensation and curing of said ureaformaldehyde prepolymers in the organic phase of said discrete droplets adjacent to said interface by simultaneously heating said emulsion to a temperature between about 20° C. to about 100° C., and adding to said emulsion an acidifying agent and maintaining said emulsion at a pH of between about 0 to about 4 for a sufficient period of time to allow substantial completion of in situ condensation of said resin prepolymers to convert the liquid droplets of said organic solution to capsules consisting of solid permeable polymer shells enclosing said liquid material. Also disclosed are the microcapsules formed by the above-described process. f
Inventors
- 👤 Herbert B. Scher
- 👤 Marius Rodson
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 17:25
CPC Classifications
B; B01; B01J; B01J13/00; B01J13/02; B01J13/06; B01J13/14; B01J13/18; A; A01; A01N; A01N25/00; A01N25/26; A01N25/28; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2984; Y10T428/2985
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
229 words
A process for the microencapsulation of a substantially water-insoluble liquid material within a porous shell to effect a slow rate of release of said material through said shell which comprises (a) providing an organic solution comprising said liquid material and an etherified urea-fonmaldehyde prepolymer dissolved therein in which from about 50% to about 98% of the methylol groups of said prepolymer have been etherified with a C 4 -C 10 alcohol; (b) creating an emulsion of said organic solution in an continuous phase aqueous solution comprising water and a surface-active agent, wherein said emulsion comprises discrete droplets of said organic solution dispersed in said continuous phase aqueous solution, there being formed thereby an interface between the discrete droplets of organic solution and the surrounding continuous phase aqueous solution; and (c) causing in situ self-condensation and curing of said ureaformaldehyde prepolymers in the organic phase of said discrete droplets adjacent to said interface by simultaneously heating said emulsion to a temperature between about 20° C. to about 100° C., and adding to said emulsion an acidifying agent and maintaining said emulsion at a pH of between about 0 to about 4 for a sufficient period of time to allow substantial completion of in situ condensation of said resin prepolymers to convert the liquid droplets of said organic solution to capsules consisting of solid permeable polymer shells enclosing said liquid material.
Claim 2
Dependent Claim
229 words
A process for the microencapsulation of a substantially water-insoluble liquid material within a porous shell to effect a slow rate of release of said material through said shell which comprises (a) providing an organic solution comprising said liquid material and an etherified urea-fonmaldehyde prepolymer dissolved therein in which from about 50% to about 98% of the methylol groups of said prepolymer have been etherified with a C 4 -C 10 alcohol; (b) creating an emulsion of said organic solution in an continuous phase aqueous solution comprising water and a surface-active agent, wherein said emulsion comprises discrete droplets of said organic solution dispersed in said continuous phase aqueous solution, there being formed thereby an interface between the discrete droplets of organic solution and the surrounding continuous phase aqueous solution; and (c) causing in situ self-condensation and curing of said ureaformaldehyde prepolymers in the organic phase of said discrete droplets adjacent to said interface by simultaneously heating said emulsion to a temperature between about 20° C. to about 100° C., and adding to said emulsion an acidifying agent and maintaining said emulsion at a pH of between about 0 to about 4 for a sufficient period of time to allow substantial completion of in situ condensation of said resin prepolymers to convert the liquid droplets of said organic solution to capsules consisting of solid permeable polymer shells enclosing said liquid material.
Claim 3
Dependent Claim
27 words
A process according to claim 1 in which from about 70% to about 90% of the methylol groups of the prepolymer of step (a) have been etherified.
Claim 4
Dependent Claim
31 words
A process according to claim 1 in which the alcohol with which the methylol groups of the prepolymer of step (a) have been etherified is a C 4 -C 6 alcohol.
Claim 5
Dependent Claim
28 words
A process according to claim 1 in which the alcohol with which the methylol groups of the prepolymer of step (a) have been etherified is n-butanol or iso-butanol.
Claim 6
Dependent Claim
40 words
A process according to claim 1 in which from about 70% to about 90% of the methylol groups of the prepolymer of step (a) have been etherified and the alcohol with which said methylol groups have been etherified is n-butanol.
Claim 7
Dependent Claim
41 words
A process according to claim 1 in which, prior to the formation of the organic solution of step (a), the prepolymer of step (a) is dissolved in an alcohol which is identical to that with which the prepolymer has been etherified.
Claim 8
Dependent Claim
28 words
A process according to claim 1 in which the surface active agent of step (b) is selected from the group consisting alkali salts of alkyl and alkylaryl sulfonates.
Claim 9
Dependent Claim
19 words
A process according to claim 1 in which the aqueous solution of step (b) further comprises a protective colloid.
Claim 10
Dependent Claim
30 words
A process according to claim 1 in which the aqueous solution of step (b) further comprises from about 0.1% to about 5.0% by weight of a polyvinyl alcohol protective colloid.
Claim 11
Dependent Claim
37 words
A process according to claim 1, 2, 3, 4, 5, 6, 7, 8, or 9 in which the prepolymer of step (a) comprises from about 1% to about 70% of the organic solution on a weight basis.
Claim 12
Dependent Claim
37 words
A process according to claim 1, 2, 3, 4, 5, 6, 7, 8, or 9 in which the prepolymer of step (a) comprises from about 5% to about 50% of the organic solution on a weight basis.
Claim 13
Dependent Claim
41 words
A process according to claim 1, 2, 3, 4, 5, 6, 7, 8, or 9 in which the protective colloid of step (b) is a polyvinyl alcohol and comprises from about 0.1% to about 5.0% by weight of the aqueous phase.
Claim 14
Dependent Claim
37 words
A process according to claim 1, 2, 3, 4, 5, 6, 7, 8, or 9 in which the droplets of the dispersion formed in step (b) are from about 0.5 microns to about 4000 microns in diameter.
Claim 15
Dependent Claim
37 words
A process according to claim 1, 2, 3, 4, 5, 6, 7, 8, or 9 in which the droplets of the dispersion formed in step (b) are from about 1 micron to about 100 microns in diameter.
Claim 16
Dependent Claim
36 words
A process according to claim 1, 2, 3, 4, 5, 6, 7, 8, or 9 in which the in situ self-condensation in step (c) is done at a pH of between about 1.0 and about 3.0.
Claim 17
Dependent Claim
48 words
A process according to claim 1, 2, 3, 4, 5, 6, 7, 8, or 9 in which the in situ self-condensation in step (c) is done at a pH of between about 1.0 and about 3.0 and at a temperature between about 40° C. and about 70° C.
Claim 18
Dependent Claim
31 words
A process according to claim 1 wherein said organic solution contains a wall-modifying agent which serves to modify the character of the wall by varying its permeability to the core material.
Claim 19
Dependent Claim
14 words
A process according to claim 17 wherein said wall-modifying agent is pentaerythritol tetrakis (mercaptopropionate).
References Cited (Backward Citations)
US3016308A
Cited
US3074845A
Cited
US3137631A
Cited
US3516941A
Cited
US3686015A
Cited
US4001140A
Cited
US4073968A
Cited
US4223060A
Cited
US4157983A
Cited
US4576891A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1993-09-10 | 1994-03-12 | 1994-09-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1997-09-10 | 1998-03-12 | 1998-09-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2001-09-10 | 2002-03-12 | 2002-09-11 | $7700.00 | Window Closed / Lapsed |