IP Library Granted Patent US 11,111,607
Granted Patent B2
US 11,111,607 · App. 16/318,778 · Granted Sep 7, 2021

Process for making high-strength polylactic acid filament

Inventors: Harm Van Der Werff (Echt, NL); Bengisu Corakci (Echt, NL); Roman Stepanyan (Echt, NL)
Assignee: DSM IP ASSETS B.V.
D01F6/625D01D5/06D01D5/12C08G63/08C08J2367/04C08L67/04D10B2401/063
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Quick Facts
Patent No.
US 11,111,607
App. No.
16/318,778
Granted
Sep 7, 2021
Kind
B2
Abstract

The present invention relates to a process for making high-strength polylactic acid elongated object comprising the steps of making a solution of polylactic acid in a solvent at a concentration of 5 to 50 mass %; spinning the solution through a spinplate comprising at least 1 spinhole to form a fluid elongated object; cooling the fluid elongated object with a cooling medium to form a solvent-containing gel elongated object; removing at least partly the solvent from the gel elongated object to form a solid elongated object; and drawing the elongated object while applying a draw ratio of at least 2, to form a high strength PLA elongated object, characterized in that the cooling medium has a temperature T q of less than 0° C. The present invention also relates to gel-spun elongated objects comprising PLA with an IV in the range of 4-40 dl/g, and having a tenacity in N/tex such that Ten≥0.146*IV, as well as gel-spun elongated object having a tenacity and a filament titer in tex (t) such that Ten≥1.40*t −0.3 . The invention also relates to articles containing said gel-spun elongated objects.

Claims (48)

1. A process for making a polylactic acid (PLA) elongated object comprising the steps of:

a) making a solution of PLA having an intrinsic viscosity (IV) measured in chloroform at 25° C. of at least 4 dL/g, in a solvent, wherein the solution has a concentration cc P of 5 to 50 mass% expressed as the mass of the PLA per total mass of the solution;

b) spinning the solution through a spinplate comprising at least 1 spinhole to form a fluid elongated object;

c) optionally applying a draw ratio DR fluid to the fluid elongated object;

d) contacting the fluid elongated object with a cooling medium having a temperature T q of less than 0° C. to form a solvent-containing gel elongated object;

e) removing at least partly the solvent from the gel elongated object to form a solid elongated object; and

f) drawing the elongated object in at least one step before, during and/or after step e), while applying a draw ratio (DR solid ) of at least 2, to form a PLA elongated object.

2. The process according to claim 1 , wherein T q is less than −5° C.

3. The process according to claim 1 , wherein

T

q

=

T

0

(

c

P

50

mass

%

-

1

)

,

where

T 0 is at least 20° C.

4. The process according to claim 1 , wherein the polylactic acid has an intrinsic viscosity in a range of 5 to 15 dL/g.

5. The process according to claim 1 , wherein the polylactic acid comprises at least 90 mol% of monomeric units derived from L-lactic acid.

6. The process according to claim 1 , wherein the total draw ratio of the elongated object (DR total ) is at least 5.

7. The process according to claim 1 , wherein the PLA solution has a concentration c P of between 6 and 40 mass%.

8. The process according to claim 1 , wherein the cooling medium is a fluid.

9. The process according to claim 1 , wherein the cooling medium has limiting activity coefficient measured at a temperature of between 90-190° C. of between 1 and 2.

10. A gel-spun polylactic acid elongated object obtained by the process according to claim 1 .

11. A gel-spun polylactic acid elongated object which comprises a polylactic acid (PLA) with an IV in a the range of 5-15 dl/g, and having a tenacity (Ten) measured according to ISO 5079 in N/tex such that Ten≥f 1 * IV, wherein factor f 1 is 0.150.

12. The gel-spun polylactic acid elongated object according to claim 11 , wherein the object has an elongation at break of at least 10% = , measured according to ISO 5079.

13. The gel-spun polylactic acid elongated object according to claim 11 , wherein the elongated object is a filament, a fibre, a strap, a strip, a tape, a film or a tube.

14. The gel-spun polylactic acid elongated object according to claim 11 , wherein the factor f 1 is 0.155.

15. The gel-spun polylactic acid elongated object according to claim 11 , wherein the factor f 1 is 0.160.

16. An article containing the gel-spun polylactic acid elongated object of claim 11 , wherein the article is selected from the group consisting of yarn, rope, fishing line, fishing net, cargo nets and curtains, kite lines, tennis racket strings, canvas, non-woven fabrics, webbings, hoses, cut resistant articles, and stab resistant articles, protective gloves, sport equipment, helmets, sails, geotextiles, membranes and medical devices.

17. A gel-spun polylactic acid elongated object which comprises a polylactic acid (PLA) with an IV in a range of 5-15 dl/g, and having a tenacity in N/tex (Ten) measured according to ISO 5079 and a filament titer in tex (t) such that Ten≥f 2 * t −0.3 , wherein factor f 2 is 1.40 N.tex −0.7 .

18. The gel-spun polylactic acid elongated object according to claim 17 , wherein the factor f 2 is 1.50.

19. The gel-spun polylactic acid elongated object according to claim 17 , wherein the factor f 2 is 1.60.

20. The gel-spun polylactic acid elongated object according to claim 17 , wherein the factor f 2 is 1.70.

Assignments (3)
CHANGE OF NAME Recorded Mar 17, 2023
From: DSM PROTECTIVE MATERIALS B.V.
To: AVIENT PROTECTIVE MATERIALS B.V.
Reel/Frame 063115/0134 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 8, 2022
From: DSM IP ASSETS B.V.
To: DSM PROTECTIVE MATERIALS B.V.
Reel/Frame 061897/0987 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 1, 2019
From: VAN DER WERFF, HARM; CORAKCI, BENGISU; STEPANYAN, ROMAN
To: DSM IP ASSETS B.V.
Reel/Frame 050892/0350 →
Priority Claims (1)
EP 16180629 · Jul 21, 2016 · regional
Continuity (1)
Related Publication 20190284726A1 · Sep 19, 2019