Chitosan yarn having a crystal structure corresponding to the anhydrous allomorph and a tensile strength, after immersion in demineralized water for fifteen hours, of at least 150 MPA

Patent metadata

Field	Value
Publication number	US-9238880-B2
Application number	US-201013201489-A
Country	US
Kind code	B2
Filing date	Feb 15, 2010
Priority date	Feb 17, 2009
Publication date	Jan 19, 2016
Grant date	Jan 19, 2016

Abstract

The invention relates to a method for producing an elongate polysaccharide element, in particular a chitosan thread, comprising an operation of extruding an extrusible solution of said polysaccharide through an extrusion die and an operation of coagulating the extruded solution. The extrusible solution is a hydroalcoholic solution containing an alcohol that does not form an azeotrope with water and which has a boiling point of more than 150° C. at atmospheric pressure. The coagulation operation includes a step of evaporating the water, preferably over the alcohol, producing a gelled extruded elongate element in the form of a mainly alcoholic gel, in particular by subjecting the extruded solution to a hot air flow. At least one operation of eliminating the alcohol contained in said gel makes it possible to obtain the elongate polysaccharide element. The chitosan thread has a crystalline structure corresponding to the anhydrous allomorph and a rupture stress of at least 150 MPa after being immersed in demineralized water for fifteen hours. The apparatus (1) for the wet extrusion of polysaccharide thread ( 10 ) includes an extruder ( 2 ) with at least one extrusion die ( 3 ), an evaporation enclosure ( 4 ) placed immediately after the output ( 3 a ) of the extrusion die ( 3 ) and supplied with a hot air flow, a neutralization unit ( 5 ), a washing unit ( 6 ), a drying unit ( 8 ) and a winding unit ( 9 ).

First claim

We claim:

1. A chitosan yarn having a crystal structure corresponding to the anhydrous allomorph and a tensile strength, after immersion in demineralized water for fifteen hours, of at least 150 MPa.

2. The chitosan yarn as claimed in claim 1 , characterized in that the weight-average molar mass of the chitosan is greater than 350 000 g/mol.

3. A textile material comprising only chitosan yarns, as claimed in claim 1 or the chitosan yarns assembled with other yarns.

4. A chitosan yarn characterized in that it is made by a method comprising:
an operation of extruding an extrudable solution of a chitosan through an extrusion die and an operation of coagulating the extruded solution, characterized in that:
the extrudable solution is an aqueous-alcoholic solution containing an alcohol which does not form an azeotrope with water and which has a boiling point above 150° C. at atmospheric pressure and
the coagulating operation comprises a step of evaporating the water, in preference to the alcohol, producing a gelled extruded elongate element in the form of a mainly alcoholic gel,

and in that it comprises at least one operation of eliminating the alcohol contained in said gel in order to obtain the chitosan yarn,
the chitosan yarn having a crystal structure corresponding to the anhydrous allomorph and a tensile strength, after immersion in demineralized water for fifteen hours, of at least 150 MPa.

5. The chitosan yarn as claimed in claim 4 , characterized in that the aqueous-alcoholic solution contains from 1.5 to 3% of chitosan and a water/alcohol proportion of from 50/50 to 30/70% by weight.

6. The chitosan yarn as claimed in claim 4 characterized in that the chitosan is acetylated chitosan.

7. The chitosan yarn as claimed in claim 4 characterized in that the chitosan is acetylated chitosan, with a degree of acetylation of less than 40%.

8. The chitosan yarn as claimed in claim 4 characterized in that the alcohol is chosen from the group consisting of 1,2- and 1,3-propanediol, 1,2-, 1,3- and 1,4-butanediol and 1,2,3-propanetriol.

9. The chitosan yarn as claimed in claim 4 characterized in that the extrudable solution is obtained by dissolving chitosan in a dilute aqueous solution of acid, and in that the neutralizing bath is a solution of ammonia, of sodium hydroxide or of potassium hydroxide.

10. The chitosan yarn as claimed in claim 4 characterized in that the weight-average molar mass of the chitosan is greater than 350 000 g/mol.

11. A textile material, comprising only chitosan yarns, as claimed in claim 4 or the chitosan yarns assembled with other yarns.

12. The chitosan yarn as claimed in claim 4 characterized in that the evaporation of water is obtained by subjecting the extruded solution to an action of a hot air flow.

13. The chitosan yarn as claimed in claim 9 characterized in that the dilute aqueous solution of acid is a dilute aqueous solution of acetic acid.

Assignees

• Domard Alain
• David Laurent
• Montembault Alexandra
• Desorme Mylène
• Tetra Medical Lab
• Univ Claude Bernard Lyon
• Centre Nat Rech Scient

Inventors

• Domard Alain
• David Laurent
• Montembault Alexandra
• Desorme Mylène

Classifications

• D01D5/06

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

• D01F2/24

  from cellulose derivatives · CPC title

• D01F9/00 Primary

  Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments · CPC title

• B29C48/91

  Heating, e.g. for cross linking · CPC title

• B29C48/05

  Filamentary, e.g. strands · CPC title