IP Library Granted Patent US 8,802,233
Granted Patent B2
US 8,802,233 · App. 12/162,762 · Granted Aug 12, 2014

Meta-type wholly aromatic polyamide fiber excellent in high-temperature processability, and method for producing the same

Inventors: Kotaro Takiue (Iwakuni, JP); Hiroshi Fujita (Mihara, JP)
Assignee: Teijin Limited
D01F6/605D01F6/805D01F6/905C08G69/32D06M2101/36D04H1/42D04H1/4342D04H1/55D04H3/16D06P1/67341D06P3/24
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Quick Facts
Patent No.
US 8,802,233
App. No.
12/162,762
Granted
Aug 12, 2014
Kind
B2
Abstract

Upon producing a meta-type wholly aromatic polyamide fiber by wet spinning a polymer solution containing a meta-type wholly aromatic polyamide containing a m-phenylenediamine isophthalamide skeleton as a major component, and an amide solvent containing a salt, (1) the polymer solution is ejected into a coagulation bath containing an amide solvent and water and containing a salt at a low concentration to coagulate as a porous thread body (fibrous material), (2) which is subsequently stretched in a plastic stretching bath containing an aqueous solution of an amide solvent, (3) is rinsed with water and then subjected to a heat treatment in a saturated steam atmosphere, and (4) is then subjected to a dry heat treatment, so as to produce a novel meta-type wholly aromatic polyamide fiber that contains an extremely small amount of a solvent remaining in the fibers, contains a small amount of a volatile substance harmful in a heat treatment step at a high temperature, is capable of suppressing coloration of a fiber product, and is capable of providing a product with high performance and high quality.

Claims (22)

1. A meta-type wholly aromatic polyamide fiber excellent in high temperature processability, characterized in that an amount of a solvent remaining in the fiber is 0.8% by weight or less, a dry heat contraction rate at 300° C. is 3% or less, and a breaking strength of the fiber is 3.5 cN/dtex or more, wherein a monofilament of the fiber has a fineness of from 0.5 to 10.0 dtex, and wherein the fiber is produced by a process comprising wet spinning.

2. The meta-type wholly aromatic polyamide fiber excellent in high temperature processability as claimed in claim 1 , wherein the solvent remaining in the fiber is an amide solvent.

3. The meta-type wholly aromatic polyamide fiber excellent in high temperature processability as claimed in claim 2 , wherein the amide solvent remaining in the fiber is at least one of N-methyl-2-pyrrolidone, dimethylacetamide and dimethylformamide.

4. A method for producing a meta-type wholly aromatic polyamide fiber excellent in high temperature processability, characterized in that an amount of a solvent remaining in the fiber is 0.8% by weight or less, a dry heat contraction rate at 300° C. is 3% or less, and a breaking strength of the fiber is 3.5 cN/dtex or more,

by wet spinning a polymer solution containing a meta-type wholly aromatic polyamide comprising a m-phenylenediamine isophthalamide skeleton as a major component, and an amide solvent containing a salt, characterized in that (1) the polymer solution is ejected into a coagulation bath containing an amide solvent and water and containing a salt to coagulate as a porous fibrous material, (2) which is subsequently stretched in a plastic stretching bath containing an aqueous solution of an amide solvent, (3) is rinsed with water and then subjected to a heat treatment in saturated steam, and (4) is then subjected to a dry heat treatment.

5. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in claim 4 , wherein in the step (1), the coagulation bath has a composition in terms of weight ratio of the amide solvent of from 40 to 60% by weight and a concentration of the salt of from 0.3 to 10% by weight, and a temperature of the coagulation bath is from 20 to 70° C.

6. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in claim 4 , wherein in the step (2), the plastic stretching bath has a composition in terms of weight ratio of the amide solvent of from 20 to 70% by weight, and the fibrous material is stretched at a ratio of from 1.5 to 10 times in the plastic stretching bath at a temperature of from 20 to 70° C.

7. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in claim 4 , wherein in the step (3), the fibrous material is subjected to the heat treatment at a stretching ratio of from 0.7 to 5.0 times in saturated steam of from 0.02 to 0.50 MPa.

8. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in claim 4 , wherein in the step (4), the fibrous material is subjected to the dry heat treatment at a stretching ratio of from 0.7 to 4.0 times at a temperature of from 250 to 400° C.

9. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in claim 4 , wherein as the polymer solution subjected to wet spinning, a meta-type wholly aromatic polyamide solution is used that contains calcium chloride and water formed through neutralization of hydrogen chloride by-produced after reacting an aromatic diamine and an aromatic dicarboxylic chloride in the presence of an amide solvent.

10. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in claim 4 , wherein as the amide solvents contained in the polymer solution, the coagulation bath and the plastic stretching bath, one, or two or more selected from the group consisting of N-methyl-2-pyrrolidone, dimethyacetamide and dimethylformamide are used.

11. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in claim 4 , wherein in a method for producing a meta-type wholly aromatic polyamide fiber by wet spinning a polymer solution containing a meta-type wholly aromatic polyamide comprising a m-phenylenediamine isophthalamide skeleton as a major component, and an amide solvent including a salt, (1) the polymer solution is coagulated in a coagulation bath containing an amide solvent and water and containing a salt, where in the coagulation bath, a composition in terms of weight ratio of the amide solvent is from 40 to 60% by weight and a concentration of the salt is from 0.3 to 10% by weight, and a temperature of the coagulation bath is from 20 to 70° C., to form a porous fibrous material, (2) which is subsequently stretched at a ratio of from 1.5 to 10 times in a plastic stretching bath containing an aqueous solution of an amide solvent and having a composition in terms of weight ratio of the amide solvent of from 20 to 70% by weight and at a temperature of from 20 to 70° C., (3) is rinsed with water and then subjected to a heat treatment in saturated steam of from 0.02 to 0.50 MPa at a stretching ratio of from 0.7 to 5.0 times, and (4) is then subjected to a dry heat treatment at a stretching ratio of from 0.7 to 4.0 times at a temperature of from 250 to 400° C.

12. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in claim 5 , wherein in the step (2), the plastic stretching bath has a composition in terms of weight ratio of the amide solvent of from 20 to 70% by weight, and the fibrous material is stretched at a ratio of from 1.5 to 10 times in the plastic stretching bath at a temperature of from 20 to 70° C.

13. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in 5 , wherein in the step (3), the fibrous material is subjected to the heat treatment at a stretching ratio of from 0.7 to 5.0 times in saturated steam of from 0.02 to 0.50 MPa.

14. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in 6 , wherein in the step (3), the fibrous material is subjected to the heat treatment at a stretching ratio of from 0.7 to 5.0 times in saturated steam of from 0.02 to 0.50 MPa.

15. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in 5 , wherein in the step (4), the fibrous material is subjected to the dry heat treatment at a stretching ratio of from 0.7 to 4.0 times at a temperature of from 250 to 400° C.

16. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in 6 , wherein in the step (4), the fibrous material is subjected to the dry heat treatment at a stretching ratio of from 0.7 to 4.0 times at a temperature of from 250 to 400° C.

17. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in 7 , wherein in the step (4), the fibrous material is subjected to the dry heat treatment at a stretching ratio of from 0.7 to 4.0 times at a temperature of from 250 to 400° C.

18. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in 5 , wherein as the polymer solution subjected to wet spinning, a meta-type wholly aromatic polyamide solution is used that contains calcium chloride and water formed through neutralization of hydrogen chloride by-produced after reacting an aromatic diamine and an aromatic dicarboxylic chloride in the presence of an amide solvent.

19. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in 6 , wherein as the polymer solution subjected to wet spinning, a meta-type wholly aromatic polyamide solution is used that contains calcium chloride and water formed through neutralization of hydrogen chloride by-produced after reacting an aromatic diamine and an aromatic dicarboxylic chloride in the presence of an amide solvent.

20. The method for producing a meta-type wholly aromatic polyamide fiber as claimed in 7 , wherein as the polymer solution subjected to wet spinning, a meta-type wholly aromatic polyamide solution is used that contains calcium chloride and water formed through neutralization of hydrogen chloride by-produced after reacting an aromatic diamine and an aromatic dicarboxylic chloride in the presence of an amide solvent.

21. The meta-type wholly aromatic polyamide fiber excellent in high temperature processability as claimed in claim 1 , wherein the fiber has a hue (L*−b*) before heat treatment of 79.0-80.6 obtained in accordance with JIS Z8728.

Assignments (2)
MERGER Recorded Dec 3, 2012
From: TEIJIN TECHNO PRODUCTS LIMITED
To: TEIJIN LIMITED
Reel/Frame 029393/0416 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 30, 2008
From: TAKIUE, KOTARO; FUJITA, HIROSHI
To: TEIJIN TECHNO PRODUCTS LIMITED
Reel/Frame 021318/0201 →
Priority Claims (2)
JP 2006-022364 · Jan 31, 2006 · national
JP 2006-037905 · Feb 15, 2006 · national
Continuity (1)
Related Publication 20090054620A1 · Feb 26, 2009