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US4444699A Expired / Lapsed US ⏱️ 0.0 years remaining

Capsule manufacture

Assignee: WTA Inc
•
Filing: 1982-04-20
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Granted: 1984-04-24
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Expires: 2002-04-20
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Abstract

Abstract A process is disclosed for performing encapsulation, en masse, by an in situ polymerization reaction to yield capsule wall material. The polymerization comprises a reaction between melamine and formaldehyde and/or polycondensation of monomeric methylol melamine or etherified methylol melamine, or a low molecular weight polymer thereof, in an aqueous vehicle and the reaction is conducted in the presence of negatively-charged, carboxyl-substituted polyelectrolyte material and certain salts, both dissolved in the vehicle. The disclosed encapsulation process permits the manufacture of microcapsules with more impermeable walls and/or lower capsule batch viscosities.

Inventors

  • 👤 Donald E. Hayford

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 13:14
CPC Classifications
B; B41; B41M; B41M5/00; B41M5/124; B41M5/165; B01; B01J; B01J13/00; B01J13/02; B01J13/06; B01J13/14; B01J13/18; C; C08; C08L; C08L61/00; C08L61/20; C08L61/26; C08L61/28; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2984; Y10T428/2985

Claims Analysis

Total Claims: 13
Claim 1
Independent Claim 260 words
A process for manufacturing minute capsules, en masse, in an aqueous manufacturing vehicle, comprising: establishing an agitating aqueous system comprising (A) melamine and formaldehyde; (B) monomeric methylol melamine or a low molecular weight polymer thereof; or (C) monomeric methylated methylol melamine or a low molecular weight polymer thereof as a starting material or mixtures of any of said starting materials, about 0.4 to about 15 percent by weight, based on the weight of aqueous manufacturing vehicle, of a system modifier material selected from the group consisting of poly(ethylene-co-maleic anhydride), poly(methyl vinyl ether-co-maleic anhydride), poly(acrylic acid), poly(propylene-co-maleic anhydride), poly(butadiene-co-maleic anhydride), poly(vinyl acetate-co-maleic anhydride) and poly(styrene-co-maleic anhydride), about 1 to about 10 percent by weight, based on the weight of aqueous manufacturing vehicle, of a salt selected from the group consisting of Periodic Group IA cations and tertiary and quaternary ammonium cations and chloride, sulfate, phosphate, nitrate, polyphosphate, citrate, maleate and fumarate anions, and particles of an intended capsule core material substantially insoluble in the system, in which agitating system the modifier is present prior to the addition of said particles, whereby said starting material polycondenses to form a condensation polymer resulting in (i) liquid-liquid phase separation of the resulting condensation polymer above a molecular weight to be soluble in the system; and (ii) continued polycondensation of the separated polymerization product to give solid capsule wall material individually surrounding particles of the dispersed intended capsule core wherein said salt is present in the aqueous manufacturing vehicle prior to the polycondensation, whereby increased capsule wall integrity and reduced capsule slurry viscosity are obtained.
Claim 2
Dependent Claim 260 words
A process for manufacturing minute capsules, en masse, in an aqueous manufacturing vehicle, comprising: establishing an agitating aqueous system comprising (A) melamine and formaldehyde; (B) monomeric methylol melamine or a low molecular weight polymer thereof; or (C) monomeric methylated methylol melamine or a low molecular weight polymer thereof as a starting material or mixtures of any of said starting materials, about 0.4 to about 15 percent by weight, based on the weight of aqueous manufacturing vehicle, of a system modifier material selected from the group consisting of poly(ethylene-co-maleic anhydride), poly(methyl vinyl ether-co-maleic anhydride), poly(acrylic acid), poly(propylene-co-maleic anhydride), poly(butadiene-co-maleic anhydride), poly(vinyl acetate-co-maleic anhydride) and poly(styrene-co-maleic anhydride), about 1 to about 10 percent by weight, based on the weight of aqueous manufacturing vehicle, of a salt selected from the group consisting of Periodic Group IA cations and tertiary and quaternary ammonium cations and chloride, sulfate, phosphate, nitrate, polyphosphate, citrate, maleate and fumarate anions, and particles of an intended capsule core material substantially insoluble in the system, in which agitating system the modifier is present prior to the addition of said particles, whereby said starting material polycondenses to form a condensation polymer resulting in (i) liquid-liquid phase separation of the resulting condensation polymer above a molecular weight to be soluble in the system; and (ii) continued polycondensation of the separated polymerization product to give solid capsule wall material individually surrounding particles of the dispersed intended capsule core wherein said salt is present in the aqueous manufacturing vehicle prior to the polycondensation, whereby increased capsule wall integrity and reduced capsule slurry viscosity are obtained.
Claim 3
Dependent Claim 22 words
The process of claim 1 wherein the system modifier material is selected from the group consisting of poly(acrylic acid) and poly(styrene-co-maleic anhydride).
Claim 4
Dependent Claim 13 words
The process of claim 2 wherein the system modifier material is poly(acrylic acid).
Claim 5
Dependent Claim 22 words
The process of claim 1 wherein the polycondensation reaction is effected at a temperature of about 40° C. to about 95° C.
Claim 6
Dependent Claim 22 words
The process of claim 4 wherein the polycondensation reaction is effected at a temperature of about 50° C. to about 60° C.
Claim 7
Dependent Claim 14 words
The process of claim 1, 3 or 5 wherein the salt is potassium phosphate.
Claim 8
Dependent Claim 254 words
A process for manufacturing minute capsules, en masse, in an aqueous manufacturing vehicle, comprising the steps of: (A) establishing an agitating single-phase aqueous solution system comprising about 0.4 to about 15 percent by weight, based on the weight of aqueous manufacturing vehicle, of a system modifier material selected from the group consisting of poly(ethylene-co-maleic anhydride), poly(methyl vinyl ether-co-maleic anhydride), poly(acrylic acid), poly(propylene-co-maleic anhydride), poly(butadiene-co-maleic anhydride), poly(vinyl acetate-co-maleic anhydride) and poly(styrene-co-maleic anhydride); (B) adding a starting material which comprises (a) melamine and formaldehyde, (b) monomeric methylol melamine or a low molecular weight polymer thereof or (c) monomeric methylated methylol melamine or a low molecular weight polymer thereof, or mixtures of any of said (a), (b) and (c) to the system; (C) dispersing into the solution system particles of an intended capsule core material substantially insoluble in the system; (D) adding about 1 to about 10 percent by weight, based on the weight of the aqueous manufacturing vehicle, of a salt selected from the group consisting of Periodic Group IA cations and tertiary and quaternary ammonium cations and chloride, sulfate, phosphate, nitrate, polyphosphate, citrate, maleate and fumarate anions; and (E) polycondensing said starting material to form a condensation polymer resulting in (i) liquid-liquid phase separation of the resulting condensation polymer above a molecular weight to be soluble in the system; and (ii) continued polycondensation of the separated polymerization product to give solid capsule wall material individually surrounding particles of the dispersed intended capsule core, whereby increased capsule wall integrity and reduced capsule slurry viscosity are obtained.
Claim 9
Dependent Claim 254 words
A process for manufacturing minute capsules, en masse, in an aqueous manufacturing vehicle, comprising the steps of: (A) establishing an agitating single-phase aqueous solution system comprising about 0.4 to about 15 percent by weight, based on the weight of aqueous manufacturing vehicle, of a system modifier material selected from the group consisting of poly(ethylene-co-maleic anhydride), poly(methyl vinyl ether-co-maleic anhydride), poly(acrylic acid), poly(propylene-co-maleic anhydride), poly(butadiene-co-maleic anhydride), poly(vinyl acetate-co-maleic anhydride) and poly(styrene-co-maleic anhydride); (B) adding a starting material which comprises (a) melamine and formaldehyde, (b) monomeric methylol melamine or a low molecular weight polymer thereof or (c) monomeric methylated methylol melamine or a low molecular weight polymer thereof, or mixtures of any of said (a), (b) and (c) to the system; (C) dispersing into the solution system particles of an intended capsule core material substantially insoluble in the system; (D) adding about 1 to about 10 percent by weight, based on the weight of the aqueous manufacturing vehicle, of a salt selected from the group consisting of Periodic Group IA cations and tertiary and quaternary ammonium cations and chloride, sulfate, phosphate, nitrate, polyphosphate, citrate, maleate and fumarate anions; and (E) polycondensing said starting material to form a condensation polymer resulting in (i) liquid-liquid phase separation of the resulting condensation polymer above a molecular weight to be soluble in the system; and (ii) continued polycondensation of the separated polymerization product to give solid capsule wall material individually surrounding particles of the dispersed intended capsule core, whereby increased capsule wall integrity and reduced capsule slurry viscosity are obtained.
Claim 10
Dependent Claim 26 words
The process of claim 7 wherein the salt is selected from the group consisting of Periodic Group IA cations and chloride, sulfate, phosphate and nitrate anions.
Claim 11
Dependent Claim 11 words
The process of claim 8 wherein the salt is potassium phosphate.
Claim 12
Dependent Claim 25 words
The process of claims 7, 8 or 9 wherein the polycondensation reaction is effected at a temperature of about 40° C. to about 95° C.
Claim 13
Dependent Claim 22 words
The process of claim 10 wherein the polycondensation reaction is effected at a temperature of about 50° C. to about 60° C.

References Cited (Backward Citations)

US2312693A Cited
US2653921A Cited
US3928272A Cited
US4100103A Cited
US4251386A Cited
US4233178A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1987-04-24 1987-10-24 1988-04-24 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1991-04-24 1991-10-24 1992-04-24 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1995-04-24 1995-10-24 1996-04-24 $7700.00 Window Closed / Lapsed

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