USRE28779E
Expired / Lapsed
US
⏱️ 0.0 years remaining
Oil-containing microcapsules and method for their production
Assignee: Fujifilm Holdings Corp
•
Filing: 1973-08-30
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Granted: 1976-04-20
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Expires: 1993-08-30
Abstract
Abstract Method of producing microcapsules containing hydrophobic oily liquid, which comprises, in producing microcapsules by complex coacervation, using gelatin, as at least one hydrophilic colloid, adding an aqueous solution of shock preventing agent at a temperature lower than the gelling point of gelatin in order to prevent a rise in viscosity due to reaction of gelatin and aldehyde during hardening pretreatment and rapidly accomplishing hardening pretreatment.
Inventors
- 👤 Shizuo Katayama
- 👤 Hiroharu Matsukawa
- 👤 Junichi Matsuyama
- 👤 Masaya Yamamoto
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 11:54
CPC Classifications
B; B41; B41M; B41M5/00; B41M5/124; B41M5/165; B01; B01J; B01J13/00; B01J13/02; B01J13/06; B01J13/10; Y; Y10; Y10T; Y10T428/00; Y10T428/249921; Y10T428/249994; Y10T428/249995; Y10T428/249997; Y10T428/29; Y10T428/2982; Y10T428/2984; Y10T428/2985; Y10T428/2987
Claims Analysis
Total Claims: 30
Claim 1
Independent Claim
24 words
integer..]. 2. The method of claim .[.1.]. .Iadd.32 .Iaddend.wherein the amount of said polyelectrolyte is from 1/12 to 1/2 by weight based on the
Claim 2
Dependent Claim
28 words
total amount of hydrophilic colloids present. 3. The method of claim .[.1.]. .Iadd.32 .Iaddend.wherein said modified cellulose is selected from the group consisting of carboxymethyl cellulose, carboxyethyl cellulose,
Claim 3
Dependent Claim
40 words
cellulose sulfate, cellulose phosphate and a metal salt thereof. 4. The method of claim .[.1.]. .Iadd.32 .Iaddend.wherein in said anionic starch derivative is selected from the group consisting of carboxymethyl starch, carboxyethyl starch, starch sulfate, starch phosphate and starch xanthate.
Claim 4
Dependent Claim
9 words
. The method of claim .[.1.]. .Iadd.32 .Iaddend.wherein said
Claim 5
Dependent Claim
19 words
polyelectrolyte is an anionic acid polysaccharide. 6. The method of claim .[.1.]. .Iadd.32 .Iaddend.wherein said polyelectrolyte is a hydroxyethyl
Claim 6
Dependent Claim
16 words
cellulose derivative. 7. The method of claim .[.1.]. .Iadd.32 .Iaddend.wherein said polyelectrolyte is a vinylbenzene sulfonate
Claim 7
Dependent Claim
10 words
copolymer. 8. The method of claim .[.1.]. .Iadd.32 .Iaddend.wherein said
Claim 8
Dependent Claim
19 words
polyelectrolyte is an acrylic acid copolymer. 9. The method of claim .[.1.]. .Iadd.32 .Iaddend.wherein said microcapsules contain a colorless
Claim 9
Dependent Claim
22 words
leuco dye capable of forming a color dye when contacted with clay. 10. Oil-containing microcapsules produced according to the method of claim
Claim 10
Dependent Claim
7 words
.[.1.]. .Iadd.32. .Iaddend. 11. Oil-containing microcapsules produced
Claim 11
Dependent Claim
21 words
according to the method of claim 9. 12. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein said condensate of naphthalene sulfonic acid
Claim 12
Dependent Claim
32 words
and Formalin has a degree of polymerization ranging from 5 to 9. 13. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein said vinyl-benzene sulfonate in said vinyl-benzene sulfonate copolymer is present in an
Claim 13
Dependent Claim
34 words
amount of from 45 to 95 mol percent. 14. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein said vinyl-benzene sulfonate in said vinyl-benzene sulfonate copolymer is present in an amount of from 60 to 85
Claim 14
Dependent Claim
20 words
mol percent. 15. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein the molecular weight of said vinyl-benzene sulfonate copolymer ranges from
Claim 15
Dependent Claim
19 words
10,000 to 3,000,000. 16. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein the molecular weight of said vinyl-benzene sulfonate copolymer
Claim 16
Dependent Claim
20 words
ranges from 100,000 to 1,000,000. 17. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein said acrylic acid in said acrylic acid
Claim 17
Dependent Claim
40 words
copolymer is present in an amount of from 40 to 95 mol percent. 18. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein said acrylic acid in said acrylic acid copolymer is present in an amount of from 50 to 85 mol
Claim 18
Dependent Claim
22 words
percent. 19. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein said acrylic acid copolymer has a molecular weight of from 6,000 to 2,000,000.
Claim 19
Independent Claim
22 words
The method of claim .[.1.]. .Iadd.32.Iaddend., wherein said acrylic acid in said acrylic acid copolymer has a molecular weight of from 50,000
Claim 20
Dependent Claim
34 words
to 1,000,000. 21. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein said hydrophilic colloid is a member selected from the .[.roup.]. .Iadd.group .Iaddend.consisting of gelatin, casein, alginate, gum arabic, styrene-maleic anhydride copolymers, and polyethylene-maleic anhydride
Claim 21
Dependent Claim
21 words
copolymers. 22. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein the addition of said polyelectrolyte takes place at a temperature of below
Claim 22
Dependent Claim
22 words
20° C. 23. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein the addition of said polyelectrolyte takes place at a temperature of below
Claim 23
Dependent Claim
10 words
15° C. 24. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein
Claim 24
Dependent Claim
12 words
said pH is 7.0. 25. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein
Claim 25
Dependent Claim
12 words
said pH is 7.5. 26. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein
Claim 26
Dependent Claim
12 words
said pH is 8.0. 27. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein
Claim 27
Dependent Claim
26 words
said pH is 10.0. 28. The method of claim 4, wherein the cellulose of said anionic starch derivative has a degree of polymerization ranging from 50
Claim 28
Dependent Claim
25 words
to 500. 29. The method of claim 4, wherein the cellulose of said anionic starch derivative has a degree of esterification or etherification of from
Claim 29
Dependent Claim
12 words
5 to 1.2. 30. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein the
Claim 30
Dependent Claim
547 words
adjustment of pH occurs before addition of the hardening agent. 31. The method of claim .[.1.]. .Iadd.32.Iaddend., wherein the adjustment of pH occurs after the addition of the hardening agent. .Iadd. 32. In a method for producing oil-containing microcapsules by: (a) emulsifying a water-immiscible oil and an aqueous solution containing gelatin and another hydrophilic colloid, or (b) emulsifying a water-immiscible oil and an aqueous solution of a hydrophilic colloid to obtain a first sol, ionizable in water and admixing said first sol and an aqueous solution of a hydrophilic colloid to obtain a second sol, ionizable in water and having an electric charge opposite to that of said first sol, one of said colloids being gelatin, (c) adding water to either emulsion derived from (a) or (b) and/or adjusting the pH thereof to cause coacervation, thus to obtain coacervates, wherein the complex colloids are deposited around the individual oil drops, (d) cooling the coacervates to cause gelation thereof, and converting the pH to alkalinity, and (e) adding a hardening agent to the system and adjusting the pH thereof to a range of from 7 to 11, the improvement which comprises: adding an aqueous solution of a polyelectrolyte having anionic functional groups to the dispersion containing said coacervates at a temperature lower than the gelling point of the gelatin, in an amount sufficient to prevent a rise in viscosity thereof, said addition being made after gelation of the coacervates has occurred and before the adjustment of said pH to a range of from 7 to 11 and the adding of said hardening agent to the system has occurred, and said adjusting of said pH occurring before, after, or simultaneously with the addition of said hardening agent, said polyelectrolyte being a member selected from the group consisting of a modified cellulose comprising polysaccharides having beta-1,4-glucoside bonds of glucoses and having anionic functional groups, an anionic starch derivative composed of a linear polysaccharide amylose formed by only alpha-1,4 bonds of D-glucose, and a branched polysaccharide amylopectin formed by mainly alpha-1,4 bonds of D-glucose and a partially side chain branched by alpha-1,6 bonds, an anionic acid polysaccharide, obtained by polycondensing linearly D-galacturonic acid between the alpha-1,4 bonds thereof, said acid polysaccharide containing pectin, pectic acid, and pectinic acid, a condensate of naphthalene sulfonic acid and formalin, which condensate is represented by the formula: ##SPC5## wherein X is a hydrogen atom, an alkali metal, or an ammonium group, and n is a positive integer, a hydroxyethyl cellulose derivative selected from the group consisting of the carboxymethyl ether of hydroxyethyl cellulose, hydroxyethyl cellulose sulfate, and hydroxyethyl cellulose phosphate, a vinyl-benzene sulfonate copolymer selected from the group consisting of a vinylbenzene sulfonate-acryloylmorpholine copolymer, a vinylbenzene sulfonate-morpholino-methylacrylamide copolymer, a vinylbenzene sulfonate acrylamide copolymer, a vinylbenzene sulfonate-vinylpyrrolidone copolymer, and a vinylbenzene sulfonate-methyloxymethylacrylamide; said copolymer having the following group within its molecular structure: ##SPC6## wherein M is an alkali metal and n is a positive integer, and an acrylic acid copolymer selected from the group consisting of an acrylic acid acryloylmorpholine copolymer, an acrylic acid-morpholinomethylacrylamide copolymer, an acrylic acid-acrylamide copolymer, an acrylic acid-vinylpyrrolidone copolymer, and an acrylic acid-methoxymethylacrylamide copolymer, said copolymer having the following group within its molecular structure: ##EQU3## wherein X is a hydrogen atom or an alkali metal and n is a positive integer. .Iaddend.
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) | 1979-04-20 | 1979-10-20 | 1980-04-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-04-20 | 1983-10-20 | 1984-04-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-04-20 | 1987-10-20 | 1988-04-20 | $7700.00 | Window Closed / Lapsed |