Alpha-keratin solutions comprising alpha-keratin intermediate filaments in liquid crystal phase, methods of preparation, and uses thereof

Patent metadata

Field	Value
Publication number	US-12139818-B2
Application number	US-201917262318-A
Country	US
Kind code	B2
Filing date	Jul 26, 2019
Priority date	Jul 26, 2018
Publication date	Nov 12, 2024
Grant date	Nov 12, 2024

Abstract

The present invention provides methods for preparing an alpha-keratin solution comprising alpha-keratin protofibrils and intermediate filaments in liquid crystal phase and uses thereof for fabricating, e.g., shape-memory polymeric fibers, yarns, threads, fabrics, structures and objects.

First claim

We claim:

1. A method for preparing an alpha-keratin solution comprising alpha-keratin protofibrils and intermediate filaments in liquid crystal phase from hair for preparation of shape-memory polymeric fibers, comprising providing a hair powder;
contacting the hair powder with an aqueous solution comprising about 6 M to about 12 M of a denaturing agent and about 50 mM to about 300 mM of a reducing agent, thereby preparing a hair residue suspension comprising insoluble hair residue and a solution comprising alpha-keratin protofibrils and intermediate filaments in liquid crystal phase;
separating the insoluble hair residue from the solution comprising the alpha-keratin protofibrils and the intermediate filaments in liquid crystal phase;
contacting the solution comprising the alpha-keratin protofibrils and the intermediate filaments in liquid crystal phase with a solution comprising about 20 to about 50 mg/mL of a salt, thereby yielding a two-phase solution comprising a first solution comprising alpha-keratin protofibrils and intermediate filaments in liquid crystal phase and a first portion of the salt and a second solution comprising a second portion of the salt; and
separating the first solution comprising alpha-keratin protofibrils and intermediate filaments in liquid crystal phase and the first portion of the salt from the second solution comprising the second portion of the salt,
thereby preparing the alpha-keratin solution comprising alpha-keratin protofibrils and intermediate filaments in liquid crystal phase from hair for preparation of shape-memory polymeric fibers.

2. The method of claim 1 , wherein the prepared alpha-keratin solution comprises between 25% and 50%(w/v) alpha-keratin protofibrils and intermediate filaments.

3. The method of claim 1 , wherein contacting the hair powder with the aqueous solution of a denaturing agent and a reducing agent comprises mixing the wool powder and the aqueous solution at a temperature of about 70° C. to about 100° C. for about 16 to about 48 hours.

4. The method of claim 1 , wherein the denaturing agent is LiBr and wherein the hair powder is contacted with a solution comprising about 6.25 M, about 6.5, about 6.75 M, about 7 M, about 7.25 M, about 7.5, about 7.75 M, about 8 M, about 8.25 M, about 8.5, about 8.75 M, about 8 M, about 8.25 M, about 8.5, about 8.75 M, about 9 M, about 9.25 M, about 9.5, about 9.75 M, about 10 M, about 10.25 M, about 1.5, about 10.75 M, about 11 M, about 11.25 M, about 11.5, or about 11.75 M LiBr.

5. The method of claim 1 , wherein the insoluble hair residue is removed from the hair residue suspension by filtration or ultracentrifugation.

6. The method of claim 1 , wherein the solution comprising about 20 to about 50 mg/mL of a salt comprises sodium chloride (NaCl), a phosphate salt, calcium chloride (CaCl 2 )), magnesium chloride (MgCl 2 ), a sulfate salt, or a combination of any of aforementioned.

7. The method of claim 1 , wherein the first solution comprising alpha-keratin intermediate filaments in liquid crystal phase and the first portion of the salt is separated from the second solution comprising the second portion of the salt by filtration.

8. The method of claim 2 , wherein the prepared alpha-keratin solution comprises between 40% and 50%(w/v) alpha-keratin protofibrils and intermediate filaments.

9. The method of claim 1 , wherein the hair is animal hair or human hair.

10. The method of claim 9 , wherein the hair is wool.

11. The method of claim 4 , wherein the hair powder is contacted with a solution comprising about 8 M LiBr.

12. The method of claim 1 , wherein the reducing agent is dithiothreitol (DTT).

13. The method of claim 12 , wherein the hair powder is contacted with a solution comprising about 75 mM, about 100 mM, about 125 mM, about 150 mM, 175 mM, 200 mM, about 225 mM, about 250 mM, or about 275 mM DTT.

14. The method of claim 13 , wherein the hair powder is contacted with a solution comprising about 150 mM DTT.

15. The method of claim 5 , wherein the filtration is performed at a temperature of about 70° C. to about 100° C.

16. The method of claim 1 , wherein the solution comprising about 20 to about 50 mg/mL of a salt comprises about 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 28, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, or about 49 mg/ml NaCl.

Assignees

• Harvard College

Inventors

• Cera Luca
• Parker Kevin Kit

Classifications

• D10B2401/046

  Shape recovering or form memory · CPC title

• D10B2211/02

  Wool · CPC title

• D01F4/00

  Monocomponent artificial filaments or the like of proteins; Manufacture thereof · CPC title

• D01D5/06 Primary

  Wet spinning methods {(D01D5/0046 takes precedence)} · CPC title

• B33Y80/00

  Products made by additive manufacturing · CPC title