US4356108A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Encapsulation process
Assignee: Mead Corp
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Filing: 1979-12-20
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Granted: 1982-10-26
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Expires: 1999-12-20
Abstract
Abstract A process for the preparation of oil-containing microcapsules by interfacial condensation of a polyfunctional amine with a polyfunctional wall-forming material is disclosed. Microcapsules produced by this process have utility in the manufacture of carbonless copy paper. The process comprises emulsifying a mixture of a hydrophobic phase, which includes an oil, a chromogenic material and an oil soluble polyfunctional wall-forming material, and a hydrophilic phase, which includes water, a water soluble emulsifying agent and a water soluble salt of the desired polyfunctional amine. The amine salt may be formed in situ in the hydrophilic phase before the emulsification step. After emulsification, sufficient base is added to the emulsion to convert the polyfunctional amine salt to a polyfunctional amine and to neutralize acid formed during subsequent condensation reactions, thus initiating the reaction of the polyfunctional amine with the oil soluble polyfunctional wall-forming material and thus forming microcapsule walls around droplets of the hydrophobic phase.
Inventors
- 👤 Gerhart Schwab
- 👤 Gerald T. Davis
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 23:50
CPC Classifications
B; B41; B41M; B41M5/00; B41M5/124; B41M5/165; B01; B01J; B01J13/00; B01J13/02; B01J13/06; B01J13/14; B01J13/16; Y; Y10; Y10S; Y10S428/00; Y10S428/914
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
223 words
A process for the preparation of oil-containing microcapsules by interfacial condensation of wall-forming materials, said microcapsules having utility in the manufacture of carbonless copy paper, comprising steps of: (a) forming a hydrophilic phase comprising water, a water soluble emulsifying agent and a water soluble polyfunctional amine salt, said polyfunctional amine salt being the reaction product of a polyfunctional amine and an acid; (b) forming a hydrophobic phase comprising an oil and an oil soluble polyfunctional wall-forming material, said oil containing a chromogenic material; (c) mixing together said hydrophobic and said hydrophilic phases with agitation, thus forming an emulsion of droplets of said hydrophobic phase in said hydrophilic phase, said droplets being from 3 to 10 microns in diameter; (d) adding an inorganic base to said emulsion, said inorganic base being addd in an amount sufficient to convert said polyfunctional amine salt to a polyfunctional amine, and to neutralize acids formed during subsequent condensation reactions, said polyfunctional amine being coreactive with said oil soluble polyfunctional wall-forming material, the pH of said resulting emulsion being slightly alkaline; (e) stirring the resulting emulsion for a period of time sufficient to allow said polyfunctional amine and said oil soluble polyfunctional wall-forming material to react to form microcapsule walls around said droplets of hydrophobic phase, said microcapsule walls being substantially impermeable to said hydrophilic and said hydrophobic phases.
Claim 2
Dependent Claim
223 words
A process for the preparation of oil-containing microcapsules by interfacial condensation of wall-forming materials, said microcapsules having utility in the manufacture of carbonless copy paper, comprising steps of: (a) forming a hydrophilic phase comprising water, a water soluble emulsifying agent and a water soluble polyfunctional amine salt, said polyfunctional amine salt being the reaction product of a polyfunctional amine and an acid; (b) forming a hydrophobic phase comprising an oil and an oil soluble polyfunctional wall-forming material, said oil containing a chromogenic material; (c) mixing together said hydrophobic and said hydrophilic phases with agitation, thus forming an emulsion of droplets of said hydrophobic phase in said hydrophilic phase, said droplets being from 3 to 10 microns in diameter; (d) adding an inorganic base to said emulsion, said inorganic base being addd in an amount sufficient to convert said polyfunctional amine salt to a polyfunctional amine, and to neutralize acids formed during subsequent condensation reactions, said polyfunctional amine being coreactive with said oil soluble polyfunctional wall-forming material, the pH of said resulting emulsion being slightly alkaline; (e) stirring the resulting emulsion for a period of time sufficient to allow said polyfunctional amine and said oil soluble polyfunctional wall-forming material to react to form microcapsule walls around said droplets of hydrophobic phase, said microcapsule walls being substantially impermeable to said hydrophilic and said hydrophobic phases.
Claim 3
Dependent Claim
18 words
The process of claim 1 wherein said chromogenic material is a color precursor of the electron donating type.
Claim 4
Dependent Claim
31 words
The process of claim 1 wherein said polyfunctional amine salt is produced in situ in said hydrophilic phase by separately adding to said hydrophilic phase a polyfunctional amine and an acid.
Claim 5
Dependent Claim
23 words
The process of claim 3 wherein said polyfunctional amine is selected from the group consisting of diethylene triamine, triethylene tetramine and mixtures thereof.
Claim 6
Dependent Claim
22 words
The process of claim 3 wherein said acid is selected from the group consisting of acetic acid, hydrochloric acid and sulfuric acid.
Claim 7
Dependent Claim
16 words
The process of claim 1 wherein said oil soluble polyfunctional wall-forming material is a polyacyl chloride.
Claim 8
Dependent Claim
12 words
The process of claim 6 wherein said polyacyl chloride is terephthaloyl chloride.
Claim 9
Dependent Claim
20 words
The process of claim 1 wherein said emulsifying agent is selected from the group consisting of polyvinyl alcohol and carboxymethylcellulose.
Claim 10
Dependent Claim
257 words
A process for the preparation of oil-containing microcapsules by interfacial condensation of wall-forming materials, said microcapsules having utility in the manufacture of carbonless copy paper, comprising the steps of: (a) forming a hydrophilic phase comprising water, a water soluble emulsifying agent selected from the group consisting of polyvinyl alcohol and carboxymethylcellulose, a water soluble polyfunctional amine, and sufficient acid to convert said polyfunctional amine to a polyfunctional amine salt, said polyfunctional amine being selected from the group consisting of diethylene triamine, triethylene tetramine and mixtures thereof; (b) forming a hydrophobic phase comprising an oil and an oil soluble polyacyl chloride, said oil containing a chromogenic material, said chromogenic material being a color precursor of the electron donating type; (c) mixing together said hydrophobic and said hydrophilic phases with agitation, thus forming an emulsion of droplets of said hydrophobic phase in said hydrophilic phase, said droplets being from 3 to 10 microns in diameter; (d) adding an inorganic base to said emulsion, said inorganic base being added in an amount sufficient to convert said polyfunctional amine salt to a polyfunctional amine, and to neutralize acids formed during subsequent condensation reactions, said polyfunctional amine being coreactive with said oil soluble polyacyl chloride, the pH of the resulting emulsion being slightly alkaline; (e) stirring said resulting emulsion for a period of time sufficient to allow said polyfunctional amine and said oil soluble polyacyl chloride to react to form microcapsule walls around said droplets of said hydrophobic phase, said microcapsule walls being substantially impermeable to said hydrophilic and said hydrophobic phases.
Claim 11
Dependent Claim
257 words
A process for the preparation of oil-containing microcapsules by interfacial condensation of wall-forming materials, said microcapsules having utility in the manufacture of carbonless copy paper, comprising the steps of: (a) forming a hydrophilic phase comprising water, a water soluble emulsifying agent selected from the group consisting of polyvinyl alcohol and carboxymethylcellulose, a water soluble polyfunctional amine, and sufficient acid to convert said polyfunctional amine to a polyfunctional amine salt, said polyfunctional amine being selected from the group consisting of diethylene triamine, triethylene tetramine and mixtures thereof; (b) forming a hydrophobic phase comprising an oil and an oil soluble polyacyl chloride, said oil containing a chromogenic material, said chromogenic material being a color precursor of the electron donating type; (c) mixing together said hydrophobic and said hydrophilic phases with agitation, thus forming an emulsion of droplets of said hydrophobic phase in said hydrophilic phase, said droplets being from 3 to 10 microns in diameter; (d) adding an inorganic base to said emulsion, said inorganic base being added in an amount sufficient to convert said polyfunctional amine salt to a polyfunctional amine, and to neutralize acids formed during subsequent condensation reactions, said polyfunctional amine being coreactive with said oil soluble polyacyl chloride, the pH of the resulting emulsion being slightly alkaline; (e) stirring said resulting emulsion for a period of time sufficient to allow said polyfunctional amine and said oil soluble polyacyl chloride to react to form microcapsule walls around said droplets of said hydrophobic phase, said microcapsule walls being substantially impermeable to said hydrophilic and said hydrophobic phases.
Claim 12
Dependent Claim
12 words
The process of claim 9 wherein said polyfunctional amine includes diethylene triamine.
Claim 13
Dependent Claim
12 words
The process of claim 9 wherein said polyacyl chloride is terephthaloyl chloride.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-10-25 | 1986-04-26 | 1986-10-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-10-25 | 1990-04-26 | 1990-10-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-10-25 | 1994-04-26 | 1994-10-26 | $7700.00 | Window Closed / Lapsed |