US4464317A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of encapsulating active agents with inorganic coatings
Assignee: Washington University in St. Louis
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Filing: 1982-03-24
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Granted: 1984-08-07
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Expires: 2002-03-24
Abstract
Abstract A method for forming discrete capsules that contain an active agent, such as a pesticide, involves first forming a suspension of the active agent suspended in a solution of an alkali metal silicate such as sodium silicate or a suspension of the active agent suspended in a liquid coacervate resulting from the addition of a coacervation agent such as acetone to the alkali metal silicate solution. The suspension, preferably in the form of droplets formed by ejecting the suspension through an orifice (e.g. a needle), is then contacted with an aqueous solution of a salt such as calcium chloride which reacts with the alkali metal silicate to form an insoluble silicate (e.g., calcium silicate) coating for the active agent while hardening the dispersed active agent in a silicate core matrix. Thus, capsules of the active agent are produced with an insoluble silicate coating. The capsules are maintained in the aqueous salt solution for a sufficient period of time to permit a high degree of conversion of soluble silicate to insoluble silicate. The capsules are then isolated and dried thereby providing structurally intact capsules which act as a free-flow powder. The capsules provide controlled release of the active agent over a prolonged period of time. Methods for preparing such capsules within a three hour period have been devices thereby improving substantially the economics of encapsulating active agents with inorganic coatings. Such brief preparation times are achieved through the use of soluble silicates rich in SiO2 and by increasing the temperature of the aqueous solution of the salt such as calcium chloride to effectively expedite the capsule curing process.
Inventors
- 👤 Curt Thies
- 👤 Francis W. Linek
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 14:26
CPC Classifications
A; A01; A01N; A01N25/00; A01N25/26; A61; A61K; A61K9/00; A61K9/48; A61K9/50; B; B01; B01J; B01J13/00; B01J13/02; B01J13/04
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
225 words
The method of encapsulating an active agent with an inorganic coating which comprises the steps of: forming (a) suspension containing the active agent suspended in a solution of an alkali metal silicate having an SiO 2 to alkali metal oxide (M 2 O) ratio between approximately 1.60 and 3.75 by weight or (b) a suspension containing the active agent suspended in a liquid coacervate resulting from the addition of a coacervation agent to a solution of an alkali metal silicate having an SiO 2 to alkali metal oxide (M 2 O) ratio between approximately 1.60 and 3.75 by weight; contacting the suspension with an aqueous solution of a salt which reacts with said alkali metal silicate to form an insoluble silicate coating for said active agent whereby capsules of the active agent with an insoluble silicate coating are formed, said insoluble silicate coating having a thickness of up to 100 μm and said aqueous solution of a salt which reacts with said alkali metal silicate being maintained at a temperature in the range of approximately 50° C.-85° C. to expedite the curing or hardening of said capsules; maintaining said capsules in said aqueous salt solution for a time sufficient to harden the silicate capsules; and isolating the capsules; thereafter drying the capsules, said capsules being characterized by having the active agent substantially uniformly dispersed throughout.
Claim 2
Independent Claim
225 words
The method of encapsulating an active agent with an inorganic coating which comprises the steps of: forming (a) suspension containing the active agent suspended in a solution of an alkali metal silicate having an SiO 2 to alkali metal oxide (M 2 O) ratio between approximately 1.60 and 3.75 by weight or (b) a suspension containing the active agent suspended in a liquid coacervate resulting from the addition of a coacervation agent to a solution of an alkali metal silicate having an SiO 2 to alkali metal oxide (M 2 O) ratio between approximately 1.60 and 3.75 by weight; contacting the suspension with an aqueous solution of a salt which reacts with said alkali metal silicate to form an insoluble silicate coating for said active agent whereby capsules of the active agent with an insoluble silicate coating are formed, said insoluble silicate coating having a thickness of up to 100 μm and said aqueous solution of a salt which reacts with said alkali metal silicate being maintained at a temperature in the range of approximately 50° C.-85° C. to expedite the curing or hardening of said capsules; maintaining said capsules in said aqueous salt solution for a time sufficient to harden the silicate capsules; and isolating the capsules; thereafter drying the capsules, said capsules being characterized by having the active agent substantially uniformly dispersed throughout.
Claim 3
Dependent Claim
28 words
The method as set forth in claim 1 wherein the aklali metal silicate is sodium silicate having an SiO 2 /Na 2 O ratio of 3.75 by weight.
Claim 4
Dependent Claim
40 words
The method as set forth in claim 1 wherein the aqueous solution of a salt which reacts with an alkali metal silicate to form an insoluble silicate coating is an aqueous solution of a salt of an alkaline earth metal.
Claim 5
Dependent Claim
35 words
The method as set forth in claim 3 wherein the aqueous solution of a salt which reacts with an alkali metal silicate to form an insoluble silicate coating is an aqueous solution of calcium chloride.
Claim 6
Dependent Claim
21 words
The method as set forth in claim 4 wherein the temperature of said aqueous solution is maintained at approximately 85° C.
Claim 7
Dependent Claim
22 words
The method as set forth in claim 4 wherein the molarity of the calcium chloride solution ranges from approximately 1 to 6.4.
Claim 8
Dependent Claim
36 words
The method as set forth in claim 1 wherein the active agent is selected from the group consisting of pesticides, insecticidal agents, fungicides, herbicides, algaecides, mildew preventative agents, drugs, mosquito control agents and plant growth agents.
Claim 9
Dependent Claim
18 words
The method as set forth in claim 1 wherein the coacervation agent is a water miscible nonpolymeric solvent.
Claim 10
Dependent Claim
24 words
The method as set forth in claim 1 wherein the capsules are dried at a temperature in the range of approximately 80° C.-120° C.
Claim 11
Dependent Claim
20 words
The method as set forth in claim 9 wherein the capsules are dried at a temperature of approximately 120° C.
Claim 12
Independent Claim
192 words
The method of encapsulating an active agent with an inorganic coating which comprises the steps of: forming a suspension containing the active agent suspended in a liquid coacervate resulting from the addition of a coacervation agent to a solution of an alkali metal silicate having an SiO 2 to alkali metal exide (M 2 O) ratio between approximately 1.60 and 3.75 by weight, said suspension having a viscosity of between approximately 20 and 620 centipoises as measured at 30° C. in a Ubbelohde viscometer; contacting the suspension with an aqueous solution of a salt which reacts with an alkali metal silicate to form an insoluble silicate coating for said active agent whereby capsules of the active agent with an insoluble silicate coating are formed said insoluble silicate coating having a thickness of up to 100 μm and said aqueous solution of a salt which reacts with said alkali metal silicate being maintained at a temperature in the range of approximately 50°-85° C. to expedite the curing of hardening of said capsules; isolating the capsules; and thereafter drying the capsules, said capsules being characterized by having the active agent substantially uniformly dispersed throughout.
Claim 13
Independent Claim
192 words
The method of encapsulating an active agent with an inorganic coating which comprises the steps of: forming a suspension containing the active agent suspended in a liquid coacervate resulting from the addition of a coacervation agent to a solution of an alkali metal silicate having an SiO 2 to alkali metal exide (M 2 O) ratio between approximately 1.60 and 3.75 by weight, said suspension having a viscosity of between approximately 20 and 620 centipoises as measured at 30° C. in a Ubbelohde viscometer; contacting the suspension with an aqueous solution of a salt which reacts with an alkali metal silicate to form an insoluble silicate coating for said active agent whereby capsules of the active agent with an insoluble silicate coating are formed said insoluble silicate coating having a thickness of up to 100 μm and said aqueous solution of a salt which reacts with said alkali metal silicate being maintained at a temperature in the range of approximately 50°-85° C. to expedite the curing of hardening of said capsules; isolating the capsules; and thereafter drying the capsules, said capsules being characterized by having the active agent substantially uniformly dispersed throughout.
Claim 14
Dependent Claim
16 words
The method as set forth in claim 11 wherein the alkali metal silicate is sodium silicate.
Claim 15
Dependent Claim
40 words
The method as set forth in claim 11 wherein the aqueous solution of a salt which reacts with an alkali metal silicate to form an insoluble silicate coating is an aqueous solution of a salt of an alkaline earth metal.
Claim 16
Dependent Claim
35 words
The method as set forth in claim 13 wherein the aqueous solution of a salt which reacts with an alkali metal silicate to form an insoluble silicate coating is an aqueous solution of calcium chloride.
Claim 17
Dependent Claim
22 words
The method as set forth in claim 14 wherein the molarity of the calcium chloride solution ranges from approximately 2.85 to 6.4.
Claim 18
Dependent Claim
23 words
The method as set forth in claim 11 wherein said suspension is converted into droplet form prior to contacting said aqueous salt solution.
Claim 19
Dependent Claim
18 words
The method as set forth in claim 11 wherein the coacervation agent is a water miscible nonpolymeric solvent.
Claim 20
Dependent Claim
36 words
The method as set forth in claim 11 wherein the active agent is selected from the group consisting of pesticides, insecticidal agents, fungicides, herbicides, algaecides, mildew preventative agents, drugs, mosquito control agents and plant growth agents.
References Cited (Backward Citations)
US2243296A
Cited
GB762700A
Cited
US3301701A
Cited
US3785798A
Cited
US3854981A
Cited
US3790497A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1987-08-07 | 1988-02-06 | 1988-08-07 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-08-07 | 1992-02-06 | 1992-08-07 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-08-07 | 1996-02-06 | 1996-08-07 | $7700.00 | Window Closed / Lapsed |