Patent US4016098A successfully refreshed from Google Patents.
US4016098A
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Process for hardening microcapsules
Assignee: Fujifilm Holdings Corp
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Filing: 1974-12-13
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Granted: 1977-04-05
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Expires: 1994-12-13
Abstract
Abstract In a process for producing microcapsules which comprises microencapsulating hydrophobic oil droplets by complex coacervation using at least two hydrophilic colloids having opposite electric charges and being ionizable in water with at least one of the colloids being gellable, the improvement comprising hardening the coacervate wall by the presence of an oxidation product of a polysaccharide as a hardening agent and adjusting the pH.
Inventors
- 👤 Keiso Saeki
- 👤 Hiroharu Matsukawa
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 11:54
CPC Classifications
B; B01; B01J; B01J13/00; B01J13/02; B01J13/20; B01J13/206; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2984; Y10T428/2985; Y10T428/2987
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
104 words
In a process for producing microcapsules by complex coacervation to microencapsulate hydrophobic oil droplets within a gelled coacervate wall, said process utilizing as the coacervate wall material at least two hydrophilic colloids having opposite electric charges and being ionizable in water, at least one of said colloids being gellable, the improvement comprising a. subsequently to the formation of said gelled coacervate wall encapsulating said hydrophobic oil droplets, hardening said coacervate wall by contacting said coacervate wall with an oxidation product of a polysaccharide and b. during said hardening stage, adjusting the pH of the system to an alkaline value of about 7 or above.
Claim 2
Dependent Claim
104 words
In a process for producing microcapsules by complex coacervation to microencapsulate hydrophobic oil droplets within a gelled coacervate wall, said process utilizing as the coacervate wall material at least two hydrophilic colloids having opposite electric charges and being ionizable in water, at least one of said colloids being gellable, the improvement comprising a. subsequently to the formation of said gelled coacervate wall encapsulating said hydrophobic oil droplets, hardening said coacervate wall by contacting said coacervate wall with an oxidation product of a polysaccharide and b. during said hardening stage, adjusting the pH of the system to an alkaline value of about 7 or above.
Claim 3
Dependent Claim
34 words
The process of claim 1, wherein said oxidation product of said polysaccharide is the reaction product obtained on oxidizing at least about 20% of the secondary alcohol groups in said polysaccharide to aldehyde groups.
Claim 4
Dependent Claim
35 words
The process of claim 2, wherein said oxidation product of said polysaccharide is a glucan, a fructan, a mannan, a xylan, a galacturonan, a mannuronan, an N-acetylglucosamine derivative, a heteroglycan, a trihetroglycan, or a tetraheteroglycan.
Claim 5
Dependent Claim
19 words
The process of claim 3, wherein said polysaccharide is gum arabic, amylopectin, cellulose sulfate, starch, laminarin or alginic acid.
Claim 6
Dependent Claim
34 words
The process of claim 1, wherein said oxidation product of said polysaccharide is present in an amount of at least about 3% by weight based on the weight of said colloid which is gellable.
Claim 7
Dependent Claim
21 words
The process of claim 1, wherein said hydrophilic colloids having opposite electrical charges are gelatin, saccharides, gums or maleic anhydride copolymers.
Claim 8
Dependent Claim
156 words
a process for producing microcapsules which comprises emulsifying a hydrophobic oil in an aqueous solution of at least one first hydrophilic colloid ionizable in water to form an oil-in-water type emulsion and admixing an aqueous solution of at least one second hydrophilic colloid which is ionizable in water and which has an opposite electric charge to said first hydrophilic colloid or emulsifying said hydrophobic oily solution in an aqueous solution of at least two hydrophilic colloids having opposite electric charges to form an oil-in-water type emulsion; causing said hydrophilic colloids to coacervate around the emulsified oil droplets by adding water to the oil-in-water emulsion and/or adjusting the pH of said oil-in-water emulsion; cooling said oil-in-water emulsion to cause the gellation of the coacervate wall, and hardening said coacervate wall by adjusting the pH to an alkaline pH of about 7 or above in the presence of an oxidation product of a polysaccharide as a hardening agent.
Claim 9
Dependent Claim
156 words
a process for producing microcapsules which comprises emulsifying a hydrophobic oil in an aqueous solution of at least one first hydrophilic colloid ionizable in water to form an oil-in-water type emulsion and admixing an aqueous solution of at least one second hydrophilic colloid which is ionizable in water and which has an opposite electric charge to said first hydrophilic colloid or emulsifying said hydrophobic oily solution in an aqueous solution of at least two hydrophilic colloids having opposite electric charges to form an oil-in-water type emulsion; causing said hydrophilic colloids to coacervate around the emulsified oil droplets by adding water to the oil-in-water emulsion and/or adjusting the pH of said oil-in-water emulsion; cooling said oil-in-water emulsion to cause the gellation of the coacervate wall, and hardening said coacervate wall by adjusting the pH to an alkaline pH of about 7 or above in the presence of an oxidation product of a polysaccharide as a hardening agent.
Claim 10
Dependent Claim
34 words
The process of claim 7, wherein said oxidation product of said polysaccharide is the reaction product obtained on oxidizing at least about 20% of the seconary alcohol groups in said polysaccharide to aldehyde groups.
Claim 11
Dependent Claim
35 words
The process of claim 8, wherein said oxidation product of said polysaccharide is a glucan, a fructan, a mannan, a xylan, a galacturonan, a mannuronan, an N-acetylglucosamine derivative, a heteroglycan, a triheteroglycan, or a tetraheteroglycan.
Claim 12
Dependent Claim
19 words
The process of claim 9, wherein said polysaccharide is gum arabic, amylopectin, cellulose sulfate, starch, laminarin or alginic acid.
Claim 13
Dependent Claim
34 words
The process of claim 7, wherein said oxidation product of said polysaccharide is present in an amount of at least about 3% by weight based on the weight of said colloid which is gellable.
Claim 14
Dependent Claim
21 words
The process of claim 7, wherein said hydrophilic colloids having opposite electrical charges are gelatin, saccharides, gums or maleic anhydride copolymers.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-04-04 | 1980-10-04 | 1981-04-05 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-04-04 | 1984-10-04 | 1985-04-05 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-04-04 | 1988-10-04 | 1989-04-05 | $7700.00 | Window Closed / Lapsed |