US4626286A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Collagen gel and the process of making said gel
Assignee: London International Us Holdings Inc
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Filing: 1985-03-27
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Granted: 1986-12-02
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Expires: 2005-03-27
Abstract
Abstract The present invention relates to a collagen gel and to a process for obtaining it. More particularly, the present invention relates to an improved homogeneous collagen gel, which can be used in the manufacture of collagen film articles of improved thinness, smoothness, superior strength, and superior homogeneity, and to a process for obtaining the improved gel.
Inventors
- 👤 Eugene K. Lubbs
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 14:42
CPC Classifications
C; C08; C08L; C08L89/00; C08L89/04; C08L89/06; Y; Y10; Y10S; Y10S128/00; Y10S128/08
Claims Analysis
Total Claims: 33
Claim 1
Independent Claim
139 words
A method of making collagen gel for use in the manufacture of thin collagen film article shaving superior mechanical properties comprising: comminuting clean animal tendon containing at least 30% collagen essentially free of ligamentous tissue in the presence of about 65% water by weight to form a collagen slurry; treating said slurry with about 0.1-0.5% by weight of proteolytic enzyme derived from Aspergillus oryzae which effectively digests elastin and other non-collagenous matter contained in said tendon while leaving the collagen structure of said tendon substantially intact, said percentage being based on the collagen solids content of said slurry: swelling the slurry with an acid selected from the group consisting of lactic acid, maleic acid, succinic acid, malic acid, oxalic acid, and tartaric acid to form a swollen collagen suspension; homogenizing and deaerating said suspension to form a collagen gel.
Claim 2
Independent Claim
139 words
A method of making collagen gel for use in the manufacture of thin collagen film article shaving superior mechanical properties comprising: comminuting clean animal tendon containing at least 30% collagen essentially free of ligamentous tissue in the presence of about 65% water by weight to form a collagen slurry; treating said slurry with about 0.1-0.5% by weight of proteolytic enzyme derived from Aspergillus oryzae which effectively digests elastin and other non-collagenous matter contained in said tendon while leaving the collagen structure of said tendon substantially intact, said percentage being based on the collagen solids content of said slurry: swelling the slurry with an acid selected from the group consisting of lactic acid, maleic acid, succinic acid, malic acid, oxalic acid, and tartaric acid to form a swollen collagen suspension; homogenizing and deaerating said suspension to form a collagen gel.
Claim 3
Dependent Claim
10 words
The method of claim 1 wherein said enzyme is Rhozyme-31.
Claim 4
Dependent Claim
16 words
A method according to claim 2 wherein said microcomputer blade spacing is 0.5 to 1.5 mm.
Claim 5
Dependent Claim
21 words
A method according to claim 2 wherein the duration of said enzyme treatment ranges between about 3 and about 24 hours.
Claim 6
Dependent Claim
21 words
A method according to claim 2, wherein said acid is selected from the group consisting of lactic acid and maleic acid.
Claim 7
Dependent Claim
22 words
A method according to claim 2, wherein said slurry is also homogenized by processing through a microcutter upon addition of said Rhozyme.
Claim 8
Dependent Claim
21 words
A method according to claim 2, wherein said swollen collagen suspension is homogenized by processing through a microcutter prior to deaeration.
Claim 9
Dependent Claim
21 words
A method according to claim 2, wherein said deaeration takes place while mixing the suspension in a mechanical mixer under vacuum.
Claim 10
Dependent Claim
38 words
A method according to claim 2, wherein a small amount of formaldehyde is also added to the slurry, at substantially the same time as the addition of said acid therein, to effect partial cross-linking of the collagen molecules.
Claim 11
Dependent Claim
27 words
A method according to claim 9 wherein said formaldehyde is added in an amount ranging between 0.3 and 0.4% based on dry solid content of said slurry.
Claim 12
Dependent Claim
93 words
A method according to claim 2, wherein said tendon is bovine digital flexor tendon, said microcutter blade spacing in step (b) is 1 mm., said Rhozyme -41 treatment duration is 15 to 18 hours, said Rhozyme -41 amount is 0.5%, and said acid is lactic acid added in an amount of 50% based on the weight of collagen solids; said method further comprising addition of 0.36% formaldehyde substantially simultaneously with said acid addition, and homogenizing said slurry after said Rhozyme addition and said collagen suspension by processing through said microcutter, after acid swelling.
Claim 13
Dependent Claim
56 words
A method according to claim 1 wherein after said enzyme digestion an amount of powder selected from the group consisting of starch powder and talc powder is mixed into said slurry in an amount such that the resulting slurry contains between 20 and 100% by weight of said powder based on the slurry collagen solids content.
Claim 14
Dependent Claim
14 words
A method according to claim 12 wherein said tendon is bovine digital flexor tendon.
Claim 15
Dependent Claim
16 words
A method according to claim 12 wherein said microcutter blade spacing is 0.5 to 1.5 mm.
Claim 16
Dependent Claim
20 words
A method according to claim 12 wherein the duration of said enzyme treatment ranges between about 3 and 24 hours.
Claim 17
Dependent Claim
21 words
A method according to claim 12, wherein said acid is selected from the group consisting of lactic acid and maleic acid.
Claim 18
Dependent Claim
22 words
A method according to claim 12, wherein said slurry is also homogenized by processing through a microcutter upon addition of said Rhozyme.
Claim 19
Dependent Claim
22 words
A method according to claim 12, wherein said swollen collagen suspension is also homogenized by processing through a microcutter prior to deaeration.
Claim 20
Dependent Claim
21 words
A method according to claim 12, wherein said deaeration takes place while mixing the suspension in a mechanical mixer under vacuum.
Claim 21
Dependent Claim
38 words
A method according to claim 12, wherein a small amount of formaldehyde is also added to the slurry, at substantially the same time as the addition of said acid therein, to effect partial cross-linking of the collagen molecules.
Claim 22
Dependent Claim
27 words
A method according to claim 20 wherein said formaldehyde is added in an amount ranging between 0.3 and 0.40% based on dry solid content of said slurry.
Claim 23
Dependent Claim
90 words
A method according to claim 12, wherein said tendon is bovine digital flexor tendon, said microcutter blade spacing in step (b) is 1 mm., said Rhozyme -41 treatment duration is 15 to 18 hours, said Rhozyme -41 amount is 0.5%, and said acid is lactic acid added in an amount of 50% based on weight of collagen solids; said method further comprising addition of 0.36% formaldehyde substantially simultaneously with said acid addition, and homogenizing said slurry after said Rhozyme addition and said acid-swollen collagen suspension by processing through said microcutter.
Claim 24
Dependent Claim
41 words
A method according to claim 12 wherein said powder is mixed into said slurry in the form of an aqueous dispersion at the beginning of said acid-swelling step, said dispersion also containing dissolved therein said acid used during said acid-swelling step.
Claim 25
Dependent Claim
43 words
A method according to claim 20 wherein said powder is mixed into said slurry in the form of an aqueous dispersion at the beginning of said acid-swelling step said dispersion having dissolved therein said acid and said formaldehyde used during said acid-swelling step.
Claim 26
Dependent Claim
13 words
A method according to claim 12 wherein said powder is corn starch powder.
Claim 27
Dependent Claim
27 words
A method according to claim 12 wherein the amount of said powder mixed in said slurry is 60% by weight based on collagen solids in said slurry.
Claim 28
Dependent Claim
59 words
A method according to claim 22 wherein said powder is corn starch powder and is mixed into said slurry in the form of an aqueous dispersion containing dissolved therein said lactic acid and said formaldehyde and wherein the amount of said corn starch mixed in said slurry is 60% by weight based on the collagen solids in said slurry.
Claim 29
Dependent Claim
10 words
A collagen in accordance with the method of claim 2.
Claim 30
Dependent Claim
18 words
A collagen gel according to claim 28 having a viscosity ranging between about 1000 and about 3000 cps.
Claim 31
Dependent Claim
94 words
A film article made from the gel of claim 28 by a process comprising the steps of: forming a film by applying at least one coat of said gel onto a substrate surface; drying said film at a temperature in the range of about 65° to about 95° C.; neutralizing and coagulating said film in an alkaline solution containing from about 0.14 to about 1.3N of hydroxyl ion for a time in the range of about 30 seconds to about 5 minutes; washing said film with water; and removing said film from said substrate.
Claim 32
Dependent Claim
11 words
The film article of claim 30, said article being a condom.
Claim 33
Dependent Claim
14 words
A method according to claim 2 wherein said tendon is bovine digital flexor tendon.
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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) | 1989-12-01 | 1990-06-02 | 1990-12-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-12-01 | 1994-06-02 | 1994-12-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-12-01 | 1998-06-02 | 1998-12-02 | $7700.00 | Window Closed / Lapsed |